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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a division of U.S. application Ser. No. 12/567,338, filed Sep. 25, 2009, now U.S. Pat. No. 8,448,922 B2, issued on May 28, 2013.
BACKGROUND OF THE INVENTION
1. Field of Invention
The present invention relates to safety brakes and, more specifically, to a safety brake device applied to theatre hoists that lift and maintain heavy loads suspended.
2. Description of Prior Art
Hoists that lift loads in a vertical direction are used in many industries for a variety of applications. For theatrical settings, athletic and entertainment arenas, overhead lifting with higher safety standards are routinely required because hoists are lifting loads directly over human beings. It is also common for portions of the staging in these theatrical settings to be lifted. Similar safety standards are required in these instances because people may be standing on the portion of the stage being lifted.
Live performances in a theater typically employ a number of curtains and backdrops to convey to the audience different settings, environments, moods, and the like. These curtains and backdrops must be changed throughout the course of a performance within a fairly short time frame without interrupting the performance. Typically this is done by raising a particular backdrop above the stage and out of sight of the audience when it is not being used. When a particular backdrop is needed, it is lowered into place on the stage.
Theatrical backdrops and curtains are typically suspended from battens, which are pipes or trusses that span the width of the stage. Battens can be 20 feet or more in length, depending on the size of the stage. As should be apparent, the weight of the battens and the items suspended from them can have substantial weight. As the weight of the load increases so does the power required to raise the load. Counterweights are employed to balance the load of the batten and its associated load. However, if the load is not closely balanced or if there is a failure in the motorized drive lifting the hoist, the system may get out of control, dropping the load or the counter-weight, causing injury or death to people nearby and/or collateral damage.
Therefore, because of the risk of hoist failure, there is a need for a safety device to prevent the uncontrolled release of heavy loads and staging that are either supported above or below human beings.
SUMMARY
The present invention comprises a combination overrunning clutch, torque disc, and friction material for preventing the uncontrolled lowering of a load. An axle connected to a motorized drive engages the overrunning running clutch. A torque disc fixedly attached to the overrunning clutch will rotate with the overrunning clutch when a load is lowered; however, resistance against rotation is generated by a set of fixed friction discs applying pressure to the sides of the torque disc. In order to lower a load, the motorized drive must overcome the friction forces applied to the side surfaces of the torque disc, thus enabling the axle to rotate.
None of the prior art devices are seen to offer the advantages of the present invention that will become apparent from the detailed description of the invention provided below.
It is an advantage of the present invention to provide a safety brake device that prevents the uncontrolled release of a suspended load.
It is a further advantage of the present invention to provide a safety brake device that provides smooth consistent resistance without producing excessive noise during operation.
It is a further advantage of the present invention to provide a safety brake device that uses a friction material that operates consistently at different temperatures and irregular use.
It is a further advantage of the present invention to provide a safety brake device that uses a friction material that is long wearing, thereby reducing the need for adjustment.
It is an advantage of the present invention to provide device of simple design and manufacture that can be fitted to current hoisting systems.
Other objects and advantages of the present invention will in part be obvious, and in part appear hereinafter.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be more fully understood and appreciated by reading the following Detailed Description in conjunction with the accompanying drawings, in which:
FIG. 1 is an exploded perspective view of a first embodiment of the present invention.
FIG. 2 is left-side elevational view of the first embodiment of FIG. 1 .
FIG. 3 is a cross-sectional view of the first embodiment along line “A-A” of FIG. 2 .
FIG. 4 is a right-side elevational view of a hub for the first embodiment of the present invention.
FIG. 5 a is an elevational view of a first embodiment of the present invention mounted on an axle and suspended from a frame.
FIG. 5 b is an elevational view of an installed first embodiment of the present invention above a stage.
FIG. 6 is a front elevational view of a second embodiment of the present invention.
FIG. 7 is a left-side elevational view of the second embodiment of FIG. 6 .
FIG. 8 is a rear elevational view of a friction disc of the second embodiment of the present invention.
FIG. 9 is a left-side elevational view of the friction disc of FIG. 8 .
FIG. 10 is an elevational view of an installed second embodiment of the present invention.
DETAILED DESCRIPTION
A first embodiment of the present invention is shown in FIGS. 1 through 4 . The first embodiment of the safety brake device comprises an overrunning clutch 12 and a disc assembly 10 . The overrunning clutch 12 may be of any suitable design known in the art, such as a ramp and roller or sprag, and includes a keyed bore enabling the inner race of the overrunning clutch to rotate with an axle installed through the keyed bore. The clutch is designed and installed such that the outer race will rotate with the inner race and axle only when a load is lowered.
The disc assembly 10 comprises a hub 22 which is installed adjacent to the overrunning clutch 12 along the axle. The hub 22 also has a bore enabling it to be installed onto the axle; however, the diameter of the bore is not keyed and is larger than the diameter of the axle, so that the hub 22 , if fixed, will not rotate with the axle. Mounted onto the hub is a torque disc 14 sandwiched between a set of friction discs 18 and backing plates 20 . A securing means is required to constantly maintain a force that presses the friction discs 18 against the sides of the torque disc 14 . In the first embodiment, the securing means comprises a nut 26 and Belleville washer 24 that is screwed onto a threaded end of the hub 22 , such that the Belleville washer is pressed against one face of a backing plate 20 . The disc assembly 10 further comprises an adaptor 16 fixed to the torque disc 14 . A first set of screws 28 are used to attach the torque disc 14 to the adaptor 16 .
A second set of screws 30 are used to attach the adaptor 16 to the outer race of the overrunning clutch 12 . The adaptor 16 and torque disc 14 are fixedly attached to the outer race of the overrunning clutch 12 , so that the three elements will rotate together when lowering a load; however, the friction discs 18 and backing plates 20 remain fixed on the hub 22 and will not rotate with the torque disc 14 , thus generating a friction forces between the torque disc 14 and friction discs 18 when a load is lowered. The disc assembly optionally includes a bearing 32 that keeps the torque disc 14 aligned with the friction discs 18 and prevent uneven wear of the friction discs.
Referring now to FIGS. 5 a and 5 b , a typical environment in which the present invention may be installed is shown. The safety brake device is mounted on the opposite end of an axle 34 from a motorized drive 38 and suspended from a frame 39 above a stage. The dashed outline in FIG. 5 b provides a cut-away view of the area above the stage where the first embodiment of the invention is typically installed. The exposed face of the hub 22 is attached to a bracket 40 which keeps the hub 22 fixed as the axle 34 rotates. A set of winch drums 36 fixed onto the axle 34 may also be present. Cables 33 wound around the winch drums 36 are attached to a batten 35 from which a load 37 , such as a curtain 37 a or theatrical scenery 37 b , is suspended. The cables 33 can also be directly attached to a load, such as a platform 37 c . When the motorized drive 38 rotates the axle 34 to lift a load, the inner race of the overrunning clutch 12 rotates with the axle 34 , but the remaining parts of the safety brake device remain fixed.
Once a load is suspended, the motorized drive 38 stops. The weight of the load will force the axle 34 to rotate in the opposite direction to lower the load; however, at this instance, the overrunning clutch 12 will lock, so that the outer race, adaptor 16 , and torque disc 14 will attempt to rotate, but will be held in place because of the friction forces between the torque disc 14 and the friction discs 18 which remain stationary with the hub 22 . If a friction disc is selected such that the friction forces are equal to the gravitational forces of the load, the motorized drive is not taxed and only a slight application of rotational force to the axle is necessary to set the load in motion.
An appropriate friction material must be selected for the friction discs 18 which has a low differential between static and dynamic coefficients of friction, such that a motorized drive is not heavily taxed when started and loads may be raised and lowered at a slow speed. It is preferred that the ratio between the static coefficient of friction and the dynamic coefficient of friction for the friction material be equal to or greater than 1.05 and less than or equal to 1.15. The friction material needs to provide smooth consistent resistance without producing any squeal, as excessive noise would be unwanted during a performance. Eliminating squeal can be achieved by saturating the friction material with a lubricant. Given the often unpredictable system usage, the friction material needs to be consistent at different temperatures and irregular use. Finally, the material needs to be long wearing reducing the need for adjustment and replacement. Any frictional material known in the art to include these characteristics, for example the frictional materials disclosed in U.S. Pat. No. 6,630,416, the disclosure of which is incorporated herein by reference, is acceptable.
Referring now to FIGS. 6 though 9 , a second embodiment of the invention is disclosed wherein the disc assembly has been replaced with a caliper and pad assembly. The second embodiment of the invention does not require the use of an adaptor as the torque disc 14 is secured directly to the overrunning clutch 12 . The friction material is now in the form of a pair of friction pads that sandwich the torque disc 14 . The friction pads are comprised of a shoe 48 to which the friction material 50 is bonded. An intermediate backing layer may be employed between the shoe 48 and the friction material 50 . The friction pad shoes 48 are attached to a caliper 44 which applies the necessary force to the sides of the torque disc 14 . Turning the knob 42 of the caliper 44 increases the distance between the ends of the caliper arms 46 . Because the caliper arms 46 are pivotally connected, the distance is decreased between the opposite ends of the caliper arms 46 to which the friction pads are attached. The knob 42 is turned and left in position to constantly maintain a force on the sides of the torque disc 14 . FIG. 10 demonstrates second embodiment of the invention installed in the same typical environment shown in FIG. 5 . The caliper 44 is braced to the frame to which the motorized drive and axle are suspended. The torque disc 14 has a bore enabling it to be installed onto the axle; however, the diameter of the bore is not keyed and is larger than the diameter of the axle, so that the torque disc 14 will only rotate with the outer race of the overrunning clutch 12 when a load is lowered. The friction forces applied by the friction pads on the caliper 44 should be equal to the gravitational forces of the load, such that the motorized drive is not taxed and only a slight application of rotational force to the axle is necessary to set the load in motion.
Thus, there has been described and illustrated herein a safety brake device that prevents the uncontrolled release of a suspended load. However, those skilled in the art will recognize that many modifications and variations besides those mentioned specifically may be made in the technique described herein without departing substantially from the spirit and scope of the present invention. For example, the safety brake device may be designed as a drum brake wherein the friction material is in the shape of a collar that applies frictional forces to the circumference of the torque disc. Accordingly, it should be clearly understood that the forms of the invention described herein are exemplary only, and are not intended as a limitation on the scope of the present invention.
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A safety brake device for a theatre hoist to prevent the uncontrolled release of a load that is suspended above or below people includes an overrunning clutch and a torque disc. The torque disc only rotates with the overrunning clutch when the load is lowered, but must overcome friction forces applied to the surface of the torque disc to do so. The friction forces are constantly applied to the torque disc by maintaining friction material in contact with the torque disc. The friction material is a non-asbestos, non-metallic composite saturated with a lubricant.
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TECHNICAL FIELD
The present invention relates generally to the control of devices attached to a network, and more particularly to a protocol facilitating the control of multiple network attached devices by a remote control device.
BACKGROUND OF THE INVENTION
Consumer electronic devices are often controlled by remote controls. Typically these remote controls or “remotes” are handheld devices having a series of buttons. Some remotes have a limited LED display and, in the case of “all in one” or “multi-remotes”, control more than one device. Devices which are traditionally controlled by such remotes include televisions, VCR's, stereo receivers, CD players and other similar devices.
The remotes control the devices by sending the device a command code that is encoded in an infrared (IR) signal. The command code causes the device to execute a particular operation. For instance, the remote may send an “off” command to the TV which causes the TV to turn off. Each device has its own unique set of commands and corresponding command codes. The remote has to be manually programmed for each device it seeks to control. For example, to program a device, a user may be instructed to enter a device code (such as 247) by pressing numbers on the keypad of the remote. For a second device, the user might be instructed instead to enter the device code of 249. The device code serves as an index into a code table which has been pre-programmed into the remote. The code table identifies the proper command codes for the associated device. A user can then use the remote to control the device whose codes the remote has identified.
This current approach has some major drawbacks. First, the approach does not readily accommodate new devices. The remote does not have access to command codes for the new devices because the pre-programmed tables of codes pre-date the new device's date of creation and are structurally fixed. Additionally, this approach requires the manual configuring of the remote by a user who may or may not perform the procedure correctly. An additional problem is that, the majority of remotes that are in use today are “line of sight” remotes that require close proximity with no obstacles between the remote and the de vice. The IR signals must have an unobstructed path from transmitter to receiver in order to be effective. Yet another problem is that the types of devices capable of being controlled by a remote are restricted for the most part to consumer electronic devices for which the remotes are programmed in advance.
SUMMARY OF THE INVENTION
The present invention addresses the difficulties of controlling new devices which have been added to a network. A network protocol, hereafter the NetCTL protocol, enables a remote control device to dynamically learn the command codes of a newly network attached device if the new device is executing the protocol. The intervention of a system administrator is not necessary since the dynamic learning process happens automatically when the new device is attached to the network. Because the protocol allows the remote control device to learn the codes dynamically, there is no need to consult previously written tables of commands which can omit the codes for newly invented devices. A user of the remote control device which has “learned” the codes (i.e. acquired the codes) for a network attached device is able to control that device regardless of the device's physical location.
In accordance with one aspect of the present invention, a method is practiced whereby the protocol enables a remote control device having a network interface to dynamically learn the command codes of a device attached to the network. The network attached devices whose commands are capable of being learned by the remote control device can take many forms such as kitchen appliances, stereo equipment, computer equipment, etc. Any network attached device that uses command codes and is equipped with the protocol can be located by the remote control device. Once the remote control device has team led the command codes, a user of the remote control device can use the remote control device to control the network attached device by sending the learned command codes to that network attached device. An example of the use of the protocol would have a user with access to a remote control device in a house's bedroom sending command codes to a stove in the kitchen and a stereo in the living room. The protocol enables the remote control device to control types of devices attached to the network which traditionally have not operated via remote control.
In accordance with another aspect of the current invention, the network environment is in a motor vehicle and a method is practiced whereby the protocol enables a remote control device having a network interface to dynamically learn the command codes of a device attached to the automobile network. The network attached devices themselves can take many forms. Any network attached-device connected to the automobile network that uses command codes and is equipped with the protocol can be located by the remote control device. Once the remote control device has “learned” the command codes, a user can use the remote control device to control the network attached device by sending command codes to that network attached device.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram showing an illustrative embodiment of the present invention;
FIG. 2 is a block diagram showing an alternative embodiment of the present invention which includes a network that is located in a car;
FIG. 3 is a block diagram depicting a remote control device used to execute the NetCTL protocol;
FIG. 4A is a block diagram illustrating the sequence of messages occurring in one aspect of the illustrated embodiment that does not use a Directory Agent of the Service Location Protocol;
FIG. 4B is a block diagram illustrating the sequence of messages occurring in an alternative aspect of the illustrated embodiment that does use a Directory Agent of the Service Location Protocol;
FIG. 5 is a block diagram showing the frame format of the header for client side messages used in the illustrated embodiment;
FIG. 6A is a flow chart of the sequence of messages in the illustrative embodiment's Hello request and response;
FIG. 6B is a block diagram showing the frame format used in the body of the Hello Request and the Hello Response of FIG. 6 ;
FIG. 7A is a flow chart of the sequence of messages in the illustrative embodiment's List Commands request and response;
FIG. 7B is a block diagram showing the frame format used in the body of the List Commands Request and the List Commands Response of FIG. 7 ;
FIG. 8A is a flow chart of the sequence of messages in the illustrative embodiment's Do Command request and response;
FIG. 8B is a block diagram showing the frame format used in the body of the Do Request and the Do Response of FIG. 8 ;
FIG. 9A is a flow chart of the sequence of messages in the illustrative embodiment's Goodbye Command request and response;
FIG. 9B is a block diagram showing the frame format used in the body of the Goodbye Request and the Goodbye Response of FIG. 9 ;
FIG. 10A is a flow chart of the sequence of messages in the illustrative embodiment's Get Image Command request and response;
FIG. 10B is a block diagram showing the frame format used in the body of the Get Image Request and the Get Image Response of FIG. 10 ;
FIG. 11A is a flow chart of the sequence of messages in the illustrative embodiment's Get Text Command request and response;
FIG. 11B is a block diagram showing the frame format used in the body of the Get Text Request and the Get Text Response of FIG. 11 ;
FIG. 12A is a flow chart of the sequence of messages in the illustrative embodiment's Get Layout Help Command request and response;
FIG. 12B is a block diagram showing the frame format used in the body of the Get Layout Help Request and the Get Layout Help Response of FIG. 12 .
DETAILED DESCRIPTION OF THE INVENTION
The illustrative embodiment of the present invention employs a protocol (i.e. the NetCTL protocol) that facilitates a remote control device locating other network attached devices. The protocol also enables the remote control device to dynamically learn command codes for network attached devices a nd then use those command codes to control the network attached devices. The set of device types that can be controlled by the remote control device is not statically fixed and is limited only by the number of devices on the network executing the protocol and hardware limitations of the remote control device.
The protocol is designed to be used in a network, such as a computer network that supports the TCP/IP protocol suite. Because protocol communications are carried over the network, there is no need for the remote control device to be in physical proximity or “line of sight” with the controlled device. In fact, the remote control device's network interface can be either a physical interface or a wireless interface. Moreover, the types of devices that may be controlled by the remote control device includes devices that are not typically controlled by an Infrared remote control device.
FIG. 1 depicts an environment suitable for practicing the illustrative embodiment of the present invention. The environment includes a network 2 to which devices 4 , 6 , 8 , 10 are interfaced. The devices include a remote control device 4 that supports the NetCTL protocol. The devices also include network attached devices 6 and 8 that do not support the NetCTL protocol (and network attached device 10 that supports the NetCTL protocol). The remote control device 4 may control all of the attached network devices 6 , 8 and 10 , even the devices 6 and 8 that do not support the protocol. It is presumed that the remote control device 4 is already aware of the network attached devices 6 and 8 but is not yet aware of network attached device 10 in the depiction of FIG. 1 .
Those skilled in the art will recognize that the components shown in FIG. 1 are intended for illustration purposes only and are in no way meant to be limiting. The present invention may be practiced on networks having different topologies and possessing different network devices. The network may be an Internet Protocol (IP) based network capable of sending and routing packets over the Internet. If the network is an IP based network, both the remote control device and any network attached devices executing the NetCTL protocol will also use the Service Location Protocol (SLP) as part of the device identification/registration process. The Service Location Protocol (SLP) is a protocol established by the Internet Engineering Task Force (NetCTL) that simplifies the discovery of network resources.
The protocol utilizes the concept of User Agents, Service Agents and Directory Agents. Applications running on a computer are represented by User Agents which understand the service and resource needs of the application. In the case of the present invention, the remote control device is represented by a User Agent. Each network device is represented by a Service Agent. Some networks have Directory Agents. The Service Agent sends out a multicast request for any Directory Agents on the network to make contact. If any Directory Agents respond, the Service Agent sends a registration unicast to each responding Directory Agent. The registration unicast includes the type of device the Service Agent is representing, the device's attributes, and the device's Uniform Resource Locator (URL) address. An attribute is a characteristic that can be used to distinguish one device from another. For example an attribute for a printer is color capability. Another attribute for the printer is its location. When a User Agent needs a particular service, it sends out a service request which includes both the type of service and attributes desired. If the network possesses a Directory Agent, the Directory Agent responds with a list of eligible devices and the devices Uniform Resource Locator (URL) address. If there is no Directory Agent on the network, the User Agent multicasts its service request on the network and the Service Agents for devices whose attributes match those requested respond directly to the User Agent.
In one embodiment of the present invention, the network is an Internet Protocol (IP) based network and the Service Location Protocol (SLP) is utilized to locate and identify available network attached devices, such as the network attached device 10 . The NetCTL protocol utilizes the SLP in one of two ways depending on the configuration of the network 2 . Upon being initially attached to the network, the Service Agent for a device executing the NetCTL protocol 10 multicasts a request for any available Directory Agents to contact the Service Agent. The Service Agent then unicasts a “registration” message to each responding Directory Agent. The registration message includes a text string identifying the name of the network attached device 10 , the device's attributes, and the URL address giving the device's location on the network 2 . The Directory Agent will subsequently forward this information to the remote control device 4 when the User Agent for the remote control device sends out a multicast request for a list of available network devices. If the network 2 does not have a Directory Agent, the User Agent for the remote control device 4 sends a multicast request out on the network directing Service Agents which represent devices which possess certain attributes to contact the User Agent. Regardless of which method is used, once the remote control device 4 receives the information for a device it wishes to contact, it can do so directly by sending messages to the device's URL address.
FIG. 2 depicts an alternative embodiment of the present invention where the remote control device 4 is used in an automobile. The environment shown in FIG. 2 includes a car network 12 to which a Seat Positioning Control Device 16 , a Climate Control Device 18 (heating and air conditioning), a CD player 20 and a Global Positioning Device 22 (used to provide mapping operations for the driver) are attached. A car stereo 24 and a cellular phone 26 are also connected to the network. The remote control device is capable of controlling all of the components 16 , 18 , 20 , 22 , 24 , and 26 by sending communications on the internal car network 12 .
The illustrative embodiment facilitates multiple network attached devices 10 being identified by the remote control device 4 . After identification of the network attached device 110 , the remote control device 4 dynamically learns the command codes of the identified network attached device through a sequence of protocol defined request and response messages. Once the remote control device 4 has received the codes for the network attached device 10 , a user of the remote control device is able to select a device from among those devices that have been identified, and issue commands to that network attached device.
FIG. 3 depicts in more detail, an example of the remote control device 4 . The remote control device 4 includes, a touch screen display surface 28 . A graphical user interface (GUI) is shown on the touch screen display surface 28 . The GUI includes numbers 1-10 (identified by reference number 30 in the figures) that may be depressed by a user to make a selection. The GUI also depicts the names 31 of the network attached devices that can be controlled by the remote control device 4 . Each network attached device name 31 appearing on the display surface 28 corresponds to a graphical user interface simulating a button 30 . For example, “Seat” corresponds with button “ 1 ”. A user selects a particular device by touching the appropriate button and a request is sent to the selected device. The remote control device 4 includes a TINI board 36 (provided by Dallas Semiconductor, Inc.) with a serial port 32 and a network interface 34 . The TINI board 36 contains a processor for executing instructions. The remote control device 4 also includes a 1 wire bus 42 and a plurality of switches 40 and ID chips 38 corresponding to the number of simulated buttons. Each “button” has 1 switch 40 and identity chip 38 assigned to it. The depression of a button closes the corresponding switch 40 which activates the identity chip 38 . The identity chip 38 sends a signal bearing its ID to the TINI 36 which then sends a NetCTL protocol request to the selected device by way of the network interface 34 .
The images depicted on the touch screen display surface 28 will vary according to the stage of communication between the electronic remote control device 4 and network attached devices. Thus after the user selects one of the network attached devices, a new screen may be shown to provide the user with appropriate choices.
A practitioner of the art will recognize that the physical composition of the remote control device 4 can take many different forms. For example the display surface can be a standard LCD display or a regular computer monitor screen rather than a touch screen and the simulated buttons may be replaced by mouse buttons or keyboard keys rather than through the use of a touch screen. Alternatively, the buttons next to the display surface which a user would manually depress. Additional embodiments of the invention are also possible. However, regardless of the form of the physical makeup of the buttons 30 on the remote control device 4 , the protocol functions identically in handling communications with the network attached devices.
When the user of the remote control device 4 selects the device that they are interested in by pressing/clicking on the button 30 associated with the name of a device on the network, button being either physical or virtual, a request for the operational command codes for that device is sent over to the network attached device 10 . The NetCTL protocol includes several formats for replies to the command request. The format that is used is dictated by the capabilities of both the remote control device 4 and the network attached device 10 . In the case of a first format, the network attached device replies to the request with the command codes for the device accompanied by a text string. A second format enables the network attached device 10 to return its command codes accompanied by a graphic image. A format enables the selected device to return its command codes accompanied by a text string and graphic image combination to the remote control device 4 .
By way of example, three allowable formats, which are described in more detail below are summarized in this chart for hypothetical responses from a selected VCR:
First Format
code
Accompanying Text String
000
“Stop”
001
“Play”
010
“Fast Forward”
011
“Reverse”
100
“Record”
101
“Pause”
Second Format
code
Accompanying graphic
000
001
010
011
100
101
=
Third Format
code
text and graphic
000
“Stop”
001
“Play”
010
“Fast Forward”
011
“Reverse”
100
“Record”
101
=
“Pause”
In the event the first format is used, the text string is shown on the touch screen display surface 28 . In the event the second format is used, the graphical image is shown on the touch screen display surface 28 . In the event the third format is used, both the text string and the graphical image are shown on the display surface 28 . If a format is requested by the remote control device 4 that the network attached device 10 cannot satisfy (i.e. a request to a network attached device to send an image graphic when the network attached device supports only text messages, or a request for a JPEG type image when the network attached device supports only GIF images), an error message is returned to the remote control device, and the remote control device subsequently requests another format that both devices can utilize. Each command ret listed on the touch screen display surface 28 is associated with one of the buttons 30 of the remote control device 4 . The user clicks on a button 30 associated with an operational command, and the command code is sent back to the network attached device. Upon receiving the command code, the network attached device 10 attempts to execute the command and returns an acknowledgment of success or an error message to the remote control device 4 .
FIG. 4A depicts the exchange of messages between a remote control device 4 and a network attached device 10 , a VCR. These two devices 4 and 10 are attached to a network which does not have a SLP Directory Agent. Since there is no Directory Agent, the multicast registration request sent out by the Service Agent for the VCR goes unanswered. With no Directory Agent, the Service Agent for the VCR 10 will listen to the network for service requests matching the services and attributes of the VCR. The User Agent for the remote control device 4 sends out a multicast request for Directory Agents. Upon getting no response, the User Agent will multicast a service request for the type of service the remote requires 45 . The Service Agent for each device matching the requested service will unicast a response 46 back to the remote control device 4 . Subsequently, the user of the remote control device 4 sees a list displayed on the display surface 28 of all of the available identified devices. In one embodiment of the present invention, the list includes the text string name that accompanied the URL of the network attached device in the registration multicast 45 . The user of the remote control device 4 selects the VCR 10 by depressing the button (physical or virtual) 30 that corresponds to the VCR 10 . The remote control device 4 sends a request 47 to the VCR 10 for the command codes of the VCR. Upon receipt of the command request, the VCR 10 sends a copy of its command codes 49 to the remote control device 4 via the network 2 . The remote control device 4 displays the available commands on its display surface 28 , and the user selects a command by depressing the associated button 30 . The selection results in a command code 51 being sent to the VCR 10 . The VCR 10 attempts to perform the command and sends either an acknowledgement or an error message 53 to the remote control device 4 . Upon receipt of the acknowledgement or error message 53 , the remote control device 4 waits for further selections by the user.
FIG. 4B depicts the sequence of messages exchanged between a network attached device 10 , a VCR, and a remote control device 4 that are utilizing the present invention on an IP based network which includes an SLP Directory Agent 58 to process SLP device registrations. The VCR 10 , sends out a registration multicast request 48 , utilizing the SLP protocol, to advertise its presence on the network. The registration multicast 45 is received by the Directory Agent 58 for the network 2 (FIG. 1 ). The Directory Agent 58 stores all of the registrations of the different network attached devices 10 as they occur. The User Agent for the remote control device 4 multicasts a request to identify available Directory Agents. The individual Directory Agents respond with identifying information. Subsequently, a user of the remote control device 4 selects an attribute descriptive of the type of devices the user wishes to control. Such an attribute may be for example, “video”. The User Agent SLP service request 61 is forwarded to a Directory Agent 58 for processing. The SLP Directory Agent 58 responds to the request 61 by sending a list of all the devices matching the attribute class 63 back to the remote control device 4 . The list matching the video attribute might be for instance “TV” and “VCR”. The text string names are accompanied by the URLs of network attached devices. The user of the remote control device 4 selects a device to control from the list of those displayed 31 , in this case the VCR 10 . A request for command codes 47 is sent to the VCR 10 . Upon receipt of the command code request 47 , the VCR 10 sends a copy of its command codes 49 to the remote control device 4 via the network 2 . The remote control device 4 displays the available commands on its display surface 28 and the user selects one by depressing a button 30 . The selection sends the selected command code 51 to the VCR 10 . The VCR 10 attempts to perform the command and then sends either an acknowledgement of successful operation performance or an error message 53 to the remote control device 4 . Upon receipt of the acknowledgement or error message 53 , the remote control device 4 waits for further selections by the user. Those skilled in the art will recognize that there can be countless sequences of different message exchanges within the scope of the present invention and the above examples are offered only for the purpose of illustration and are not meant to be a restrictive list of the possible exchanges.
The present invention dictates the form of the conversation between the remote control device 4 and the network attached devices 10 executing the protocol. The protocol works on a request-response model, where the remote control device 4 executes the client side of the protocol and initiates the requests, and the network attached device 10 executes the server side of the protocol and initiates the responses. The format of the most common exchanges is outlined and described in detail below:
Client Side of NetCTL Protocol
Server Side of NetCTL Protocol
Remote control device
Network Attached Device
Hello(Remote ID)
→
← ACK, Session Key(Key),Top
Menu Code
List Commands(Key, Menu Code)
→
← ACK, List of Command Codes
w/Text
Do Command(Key, Cmd Code)
→
← ACK, Status String, Prompt,
New Menu Code
Goodbye(Key)
→
← ACK
Utility Functions
Get Image(Key, Cmd Code, Pref
→
Type)
← ACK, type, Image Bits, GridBag
Info
Get Text(Key, Cmd Code)
→
← ACK, Text
Get Layout Help(Key, Menu Code)
→
← ACK, Grid Layout Info
The illustrative embodiment of the present invention uses a frame format for messages between the remote control device 4 and the network attached device 10 . FIG. 5 depicts the format of the message header 74 used in the illustrative embodiment for all of the remote control device's requests. The header 74 is 4 bytes in length and includes a 1 byte version code field 76 set to the version number of the protocol, a 1 byte Operation Code (opcode) field 78 set to the number representing the operation currently being performed, and a 2 byte Session ID field 80 set to the identifier number established for messages between the remote control device and the network attached device during the initial contact between the two devices. The Session ID field 80 is set to 0 if the request is the initial “Hello” request of the present invention. Those skilled in the art will recognize that the size of the fields in the frame format may be adjusted in different versions of the protocol without departing from the scope of the present invention.
Once a user of the remote control device 4 indicates a desire to control a registered network attached device 10 by depressing the appropriate button 30 , the remote control device attempts to make contact with the selected network attached device as depicted in FIG. 6 A. Contact is initiated in the illustrative embodiment by the electronic remote control 4 device sending a “Hello” request (step 84 ) to the selected network attached device 10 . The “Hello” request (step 84 ) contains an ID for the remote control device 4 so that the selected network attached device 10 can respond directly to the remote control device. The network attached device 10 sends a response (step 88 ) if available, which includes an acknowledgement, a Session Key and the top level menu code to the remote control device 4 . The session key is included in any future messages between the two devices. The Top Level Menu Code is included to allow the remote control device 4 to access the menu of command codes of the network attached device 10 .
The frame format used by the remote control device 4 and the network attached device 10 in the “Hello” request and response is depicted in FIG. 6 B. The header 90 used in the “Hello” request includes the protocol version number 92 , the “Hello” operation code as defined in the protocol 94 , and the number “0” in the Session ID field 96 since a message session with the network attached device 10 has not been established. The body of the message 98 includes the electronic remote control ID in the a two byte field 100 . The “Hello” response format includes its own header 102 which includes an Acknowledgement field 104 , the “Hello” response opcode 106 , and a session ID 108 established by the network attached device which serves as a reference number for further messages between the remote control device 4 and the network attached device 10 . The body of the response message 110 includes an acknowledgement field 112 , the Hello Response Opcode field 114 and a Top Level Menu Code field 116 . The Top Level Menu Code 116 identifies the menu holding the list of commands for the selected network attached device 10 .
FIG. 7A depicts the steps by which the remote control device 4 requests and receives the network attached device's commands and command codes. The remote control device 4 sends a List Commands request (step 120 ) to the network attached device 10 . The List Commands request (step 120 ) includes the Top Level Menu Code the remote control device 4 had previously received from the network attached device 10 . The network attached device 10 sends a response (step 124 ), which includes an acknowledgement, a list of command codes and a list of text strings representing the names of the available commands, to the remote control device 4 .
The frame format used by the illustrative embodiment in the List Commands request and response is depicted in FIG. 7 B. The List Commands request header 126 includes fields for the protocol version number 128 , the List Commands opcode 130 , and the session ID 132 assigned by the network attached device 10 in its response to the “Hello” request. The message body 134 includes the Top Level Menu code 136 of the network attached device 10 . The List Commands response header 138 includes separate fields for the protocol version 140 , the List Commands Response opcode 142 , and the Session ID 144 . The body of the List Commands response message 146 includes separate fields for the Acknowledgement 148 , the Command Count 150 indicating the number of commands being sent, and three fields for each command, the actual command 152 , the length of text string field 154 indicating the length of the following field, and the text string field 156 holding the actual name of the command. The three fields are repeated from 1 to n times, with n being the number of commands sent and equal to the number in the Command Count field 150 . The text strings representing the names of device commands are displayed on the remote control device 4 display surface 28 .
FIG. 8A depicts the steps by which the remote control device 4 of the illustrative embodiment requests the network attached device 10 perform a certain operation. The remote control device 4 sends a Do request (step 160 ) to the network attached device 10 . The Do request (step 160 ) includes the Session ID and one of the network attached device's command codes which the remote control device 4 previously received in the network attached device's List Command response 124 . The network attached device's response (step 164 ) includes an acknowledgement field and may include fields for the status of the network attached device 10 if the network attached device is configured to update its status upon request, and for a prompt message to the user if the operation requires it. The network attached device's response (step 164 ) also includes a new menu code for the network attached device 10 , which identifies the next menu to present to the user.
The frame format used by the illustrative embodiment in the Do Command request and response is depicted in FIG. 8 B. The Do Command request header 166 includes fields for the protocol version number 168 , the Do Commands Opcode 170 , and the Session ID 172 . The message body of the Do command 174 includes a command code for the network attached device 10 . The Do response header 178 includes the protocol version header 180 , the Do command response code 182 and the Session ID 184 . The message body 186 includes an acknowledgement field 188 , and a status length field 190 which indicates the length of the following status field 192 . The status field contains bits describing the condition of the network attached device 10 . The message body 186 also includes a prompt length field 194 which indicates the length of the following Prompt field 196 . Some operations require further input from the user of the remote control device 4 , and the prompt field is used to send a text message back to the user from the network attached device 10 . The Do response message format also includes a new menu code 198 which provides a different menu for the network attached device 10 . Those skilled in the art will recognize that both the status length field 190 and the prompt length field 194 may in some circumstances be set to 0 and the corresponding Status 192 and Prompt 196 fields may be empty. The Status field will be empty if the network attached device 10 does not provide updated device information to the remote control device 4 . The Prompt field 196 will be empty if the network attached device 10 is able to complete the operation requested in the Do request 160 without further information from the user of the remote electronic control device 4 .
FIG. 9A depicts the steps by which the remote control device 4 of the illustrative embodiment requests the network attached device 10 terminate the message session. The remote control device 4 sends a Goodbye request (step 202 ) to the network attached device 10 . The Goodbye request (step 202 ) includes the Session ID. The network attached device's response (step 206 ) includes an acknowledgement.
The frame format used by the illustrative embodiment in the Goodbye Command request and response is depicted in FIG. 9 B. The Goodbye Command request header 210 includes fields for the protocol version number 212 , the Goodbye Commands Opcode 214 , and the Session ID 216 . The message body of the Goodbye command 218 is empty. The Goodbye response header 220 includes the protocol version field 222 , the Goodbye Command response code field 224 and the Session ID field 226 . The message body 228 includes an acknowledgement field 230 .
The illustrative embodiment also includes utility functions that allow the remote control device 4 to obtain additional information about a device's preferred control pad layout and additional button image information. If the user of the remote control device 4 wishes to have images to display instead of text, the remote control device can query the network attached device 10 for them directly by sending the Get Image opcode. FIG. 10A depicts the steps by which the remote control device 4 requests the network attached device 10 send image data. The remote control device 4 sends a Get Image request (step 232 ) to the network attached device 10 . The Get Image request (step 232 ) includes the Session ID, the Command Code for providing the data, and a Preference Type listing the particular type of image requested (i.e.: JPEG, GIF, BMP, etc.). The network attached device's response (step 234 ) includes an acknowledgement or error message, an indication of the type of image being sent, the image bits themselves, and miscellaneous information associated with the image).
The frame format used by the illustrative embodiment in the Get Image Command request and response is depicted in FIG. 10 B. The Get Image Command request header 236 includes fields for the protocol version number 238 , the Get Image Commands Opcode 240 , and the Session ID 242 . The message body of the Get Image command 244 includes fields for a command code 246 , and a preference type 248 . The Get Image response header 250 includes fields for the protocol version header 252 , the Get Image Command response code 254 and the Session ID 256 . The message body 258 includes fields for an acknowledgement 260 , type (JPEG, GIF, BMP, etc.) 262 , image size 264 , listing the image size in bytes, image bits 266 , the image bits themselves, and a miscellaneous image information field 268 .
FIG. 11A depicts the steps by which the remote control device 4 requests the network attached device 10 send text data. The remote control device 4 sends a Get Text request (step 270 ) to the network attached device 10 . The Get Text request (step 270 ) includes the Session ID and the appropriate Command Code. The network attached device's response (step 272 ) includes an acknowledgement and the requested text.
The frame format used by the illustrative embodiment in the Get Text Command request and response is depicted in FIG. 11 B. The Get Text Command request header 274 includes fields for the protocol version number 276 , the Get Text Commands Opcode 278 , and the Session ID 280 . The message body of the Get Text command 282 includes a field for the appropriate command code 284 . The Get Text response header 286 includes fields for the protocol version header 288 , the Get Text Command response code 290 and the Session ID 292 . The message body 294 includes fields for an acknowledgement 296 , text length 298 , which indicates the length of the upcoming text field 300 , which holds the actual text bits.
FIG. 12A depicts the steps by which the remote control device 4 requests the network attached device 10 send grid layout information for the display surface 28 . The remote control device 4 sends a Get Layout Help request (step 302 ) to the network attached device 10 . The Get Layout Help request (step 304 ) includes the Session ID and the appropriate Menu Code. The network attached device's response (step 304 ) includes an acknowledgement and the grid layout information.
The frame format used by the illustrative embodiment in the Get Layout Help Command request and response is depicted in FIG. 12 B. The Get Layout Help Command request header 306 includes fields for the protocol version number 308 , the Get Layout Help Command Opcode 310 , and the Session ID 312 . The message body of the Get Layout Help command 314 includes a field for the menu code 316 for the commands for which the layout help is sought. The Get Layout Help response header 318 includes fields for the protocol version header 320 , the Get Layout Help Command response code 322 and the Session ID 324 . The message body 326 includes fields for an acknowledgement 328 , grid layout information size 330 , which indicates the length of the upcoming grid layout information field 332 , which holds the actual grid layout information. The remote control device 4 uses this information to arrange the information shown on its display surface 28 .
It will thus be seen that the invention efficiently attains the objects made apparent from the preceding description. Since certain changes may be made without departing from the scope of the present invention, it is intended that all matter contained in the above description or shown in the accompanying drawings be interpreted as illustrative and not in a literal sense. Practitioners of the art will realize that the separate requests and responses illustrated herein may have fields added or deleted from the request or response and additional requests and responses may be added from one protocol version to the next without departing from the scope of the present invention.
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The present invention addresses the difficulties of controlling new devices which have been added to a network. A network protocol, the NetCTL protocol, enables a remote control device to dynamically learn the command codes of a newly network attached device if the new device is executing the protocol. The intervention of a system administrator is not necessary since the dynamic teaming process happens automatically when the new device is attached to the network. Because the protocol allows the remote control device to learn the codes dynamically, there is no need to consult previously written tables of commands which can omit the codes for newly invented devices. A user of the remote control device which has “learned” the codes (i.e. acquired the codes) for a network attached device is able to control that device, regardless of the device's physical location, by selecting and sending the network attached device a command code to perform an operation.
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FIELD OF THE INVENTION
[0001] The invention relates to wall panel systems, and more particularly to methods of attaching wall panels to exterior surfaces.
BACKGROUND OF THE INVENTION
[0002] There are numerous problems with known aluminum wall panel attachment systems. Conventionally, such systems relied upon adhesive or caulk to “seal” the aluminum panel from the elements. However, under heat and cold and moisture, the adhesive or caulk breaks down compromising the stability of the system and giving an undesirable appearance. Even when such a seal is functional, there a tendency for undesirable effects on the aluminum panels as the interior environment can trap heat which affects the panels, creating “oil-canning” or popping in response to the pressure differential. In spite of such seals, such systems can also trap moisture in the wall cavity, which results in oxidation of parts and staining or deterioration of exterior wall surfaces.
[0003] More recently systems have been developed according to the “rainscreen principle” in which the wall cavity is vented, resulting in a temperature and pressure equalized system with adequate moisture drainage. However, such systems can be difficult to install, relying on many components to be milled or adapted on-site, and requiring excessive labour cost and specialty materials. No suitable system has been developed which applies the rainscreen principle, while providing cost-effective simple installation.
SUMMARY OF THE INVENTION
[0004] A dry joint aluminum wall panel attachment system is provided. The system comprises
[0005] a bracket assembly fastened to the exterior wall;
[0006] an attachment clip fastened to the bracket assembly by a fastener, the attachment clip having a central fastening surface fastened to the bracket assembly and at least one wing member extending outwardly from the central fastening surface;
[0007] a wall panel having an exterior flat surface and at least two side surfaces bent generally perpendicularly to the exterior flat surface and defining a hollow interior portion;
[0008] a panel perimeter strip fastened to one side surface of the wall panel, the perimeter strip comprising:
a generally C shaped body member sitting inside a corner of the wall panel and extending along an inside portion of the side surface, and a receiving member integrally attached to the body member that extends beyond the side surface of the wall panel and provides a slot adapted to engage and interlock the wing member of the attachment clip, thus connecting the wall panel to the attachment clip and thereby to the wall;
[0011] an infill strip dimensioned to fit in the slot of the panel perimeter strip proximate to the attachment clip so as to cover the fastener;
[0012] wherein the system is held together non-adhesively and wherein the wall panels are ventilated to permit ingress and egress of air and moisture to provide a pressure-balanced and moisture-drained interior environment.
[0013] Preferably, the attachment clip (here aluminum) comprises two wing members, each adapted to engage a panel perimeter strip of an adjacent wall panel.
[0014] Preferably, the bracket assembly (here steel) comprises two back-to-back L angle brackets fastened to each other to form a generally Z shaped assembly, a first end of which is for attachment to the wall and a second end of which is for fastening to the attachment clip (such as a threaded fastener).
[0015] The wall panels comprise an aluminum composite material, which is preferably routed and bent to form the exterior and side surfaces. The panel perimeter strip (here aluminum) may be pre-assembled to the wall panel before installation to the wall. Preferably the panel perimeter strip is fastened to the wall panel by rivet. This rivet may contribute to the ventilation of the panel system.
[0016] The infill strip (here aluminum composite) may be engaged with the slot of the panel perimeter strip prior to installing an adjacent wall panel. Alternatively, the infill strip may be introduced to the slots of two adjacent panel perimeter strips after two adjacent wall panels have been installed.
[0017] Preferably, the system further comprises an isolation tape which is applied between the attachment clip and the bracket assembly.
[0018] The system may further comprise a panel stiffener component placed inside the hollow interior portion of the wall panel to reinforce the exterior surface of the panel and prevent deforming or popping of the wall panel.
BRIEF DESCRIPTION OF THE FIGURES
[0019] So that the manner in which the above recited features of the present invention can be better understood, certain drawings are appended hereto. It is to be noted, however, that the appended drawings illustrate only selected embodiments of the inventions and are therefore not to be considered limiting of scope, for the inventions may admit to other equally effective embodiments and applications.
[0020] FIG. 1 shows a simplified cut-through view of the dry joint aluminum wall panel attachment system, according to the preferred embodiment.
[0021] FIG. 2 shows a panel perimeter strip used in the attachment system.
[0022] FIG. 3 shows an attachment clip used in the attachment system.
[0023] FIG. 4 shows a cut-through view of a panel stiffener optionally used in the attachment system.
[0024] FIG. 5 shows a cut-through view of the aluminum composite material (ACM) used in the panels.
[0025] FIGS. 6, 7 , 8 show progressive steps in the formation of an ACM panel for use in the present system.
[0026] FIG. 9 shows a cut-through view of an infill strip used in the attachment system.
[0027] FIG. 10 shows a detailed view of the preferred placement of the infill strip in the attachment system.
[0028] FIG. 11 shows a simplified elevational view of the sub-framing used before mounting the ACM panels in the present system.
[0029] FIG. 12 shows a detailed view of the complete attachment system with sub-framing.
[0030] FIGS. 13, 14 , 15 show progressive steps in the installation of panels in the present system (first method).
[0031] FIG. 16 shows a view of the installation of lengths of infill strip in the present system (second method).
[0032] FIG. 17 shows a view of a finished wall paneled exterior.
[0033] FIG. 18 shows a cut-through view of an alternative panel perimeter strip.
[0034] FIGS. 19-20 show cut-through views of two versions of an alternative panel stiffener.
DETAILED DESCRIPTION
[0035] The present panel attachment system 10 uses an extruded aluminum attachment system for fastening fabricated panels to all building surfaces. The system's strength is further enhanced by the use of an extruded perimeter frame design.
[0036] The system 10 is designed to the standard of the rainscreen principle. Simply, it is designed so that the wall cavity is vented, resulting in a pressure equalized system as seen in FIG. 1 . Controlled moisture drainage within the system, coupled with this equalized pressure, contributes to effective, maintenance free construction.
[0037] The extrusion process begins with an aluminum billet, the material from which the profiles are extruded. The billet must be softened by heat prior to extrusion process. The heated billet is placed into the extrusion press, a powerful hydraulic device wherein a ram pushes a dummy block that forces the softened metal through a precision opening, known as a die, to produce the required shapes. The extruded shape may have a mill or anodized finish.
[0038] The system includes a panel perimeter strip 14 ( FIG. 2 ), which is attached to the ACM panel 32 using counter sunk rivets 36 . The panel perimeter strip is designed to fit together with the attachment clip 16 ( FIG. 3 ). The custom designed extrusion allows for maximum attachment area without foregoing structural integrity.
[0039] The attachment clip 16 ( FIG. 3 ) is used on site to attach the panel perimeter strip 14 to the building as illustrated in FIG. 12 . The clip 16 is designed so as to interlock with the panel perimeter strip 14 while holding the infill strip 38 ( FIG. 10 ) securely in place.
[0040] The system optionally includes a panel stiffener 18 component ( FIG. 4 ), which may be used on large sized panels. The stiffener 18 is used to prevent the popping or “oil canning” of the panel. As the panel heats up, the panel expands and makes a popping sound. The stiffener 18 reinforces the panel to reduce this effect.
[0041] The panel stiffener 18 may comprise a hollow tube, as shown in FIG. 4 . An internally reinforced panel stiffener 18 A, 18 B may alternatively be used for greater stability (see FIGS. 19, 20 ). Where panel stiffeners are used, the panel perimeter strip may be adapted to better locate and secure the stiffener component. A panel perimeter strip 14 A having profile as shown in FIG. 18 may be advantageous for this purpose. The extended interior lip of the panel perimeter strip operates to secure the panel stiffener component.
[0042] Panel stiffeners may be provided in different sizes depending on the wind pressures to which the panel will be exposed. A larger width panel stiffener 18 B may be advantageous where there are greater wind loads on the panel system or if less deflection on the panel is desired. It will be appreciated that the construction of the panels also provides a basic level of rigidity and stiffeners are not necessarily required.
[0043] As shown in FIG. 5 , the aluminum composite material 20 (ACM) consists of a core of low density polyethylene 24 sandwiched between two sheets of aluminum 22 (each approximately 0.5 mm thick). The finish face of the aluminum is coated with a polyvinylidene fluoride coating. The inner aluminum layer is typically coated with chrome or polyester coatings. The standard thickness of the panel is 5/32″ (4 mm) but thickness may range from ⅛″ (3 mm) to ¼″ (6 mm), depending on customer preference or structural requirements.
[0044] A finished ACM panel 32 may be fabricated from a flat sheet of ACM 26 using different types of router and cutting bits 28 ( FIG. 6 ). After the sheet of ACM has been cut and routed, it is then bent along the router lines to form the finished panel 32 ( FIG. 7 ). The newly shaped panel 32 is then assembled with the panel perimeter strip 14 using a panel rivet 36 to complete the finished panel ( FIG. 8 ). A standard panel rivet for this application is 3/16″ diameter.
[0045] There are various methods to accomplish the routing and cutting process:
[0046] Method 1
[0047] Handheld router (not shown): A handheld router is used more often when reworking a panel to a different size. This method requires the simplest tool set up, but is the most labour-intensive method of fabrication due to the lengthy time for setup and layout of each different panel.
[0048] Method 2
[0049] Vertical table saw (not shown): A vertical table saw can also be used, both to cut and rout the panels. Custom “V” routing blades can be purchased to rout the panels. Panel design is limited using the vertical table saw in itself. Using it in combination with the hand held router has its advantages, but it is still a costly way to manufacture panels.
[0050] Method 3
[0051] CNC-Machine (not shown): The computer numerically controlled (CNC) machine is a complete and concise way to manufacture panels. Once the panel has been designed by a CAD operator it is then sent directly to the machine. This machine has been found to be very useful and economical for manufacturing panels. This is the applicants' preferred method for cutting and routing panels.
[0052] The infill strip ( FIG. 9 ) is typically cut to a width of approximately 1¼″ (32 mm) for a ½″ (13 mm) joint. The infill strip replaces the conventional caulk joint, giving the panel system a clean, maintenance free appearance. The infill strip also is used to hide the fasteners 36 for the attachment clip ( FIG. 10 ).
[0053] As shown in FIG. 11 , to install the panel system, sub framing is first constructed using two back-to-back galvanized steel “L” angles 40 ( FIG. 12 ); the two “L” angles allow the installer to level the substrate in all 3 axes before installation of panels. The sub framing is typically installed horizontally at each horizontal joint as shown in FIG. 11 . The method of installation of the framing at its correct installation measurements starts at the bottom of the substrate wall and moves up, making sure that each row is level to the previous row installed.
[0054] A layer of isolation tape 42 may be applied to the back of aluminum attachment clips 16 ( FIG. 3 ) to prevent direct contact between the galvanized steel sub framing and the aluminum attachment clip and thus prevent galvanic action (electrolytic decay of the aluminum) over time. Preferably, stainless steel self-drilling screws are used to fasten aluminum attachment clips to steel sub framing 40 . After determining a logical order of installation, each panel is to be plumbed and leveled to ensure a tight and concise fit form panel to panel.
[0055] Infill strip is preferably shipped in long lengths and are to be cut to fit on site. The strips may have a protective plastic coating, which is then removed from the face of the infill strips before installing them. These infill strips can be installed one or two ways:
[0056] First, as shown in FIGS. 13-15 , the infill strips may be slipped in before the adjacent panel is installed when the edge of the joint is not accessible, or when the infill strip has a curve or bend in it. The infill strip 38 is fitted into the space between the panel 32 return and the attachment clips 14 as illustrated in FIG. 13 and FIG. 14 . Then an adjacent panel 32 ′ is installed so that the infill strip 38 and attachment clip 16 engage into the slots in the panel edge at the perimeter strip 14 ′ ( FIG. 15 ).
[0057] As an alternative method of installation, the installer can slide the infill strip 38 in from the end ( FIG. 16 ), which allows for a simplified installation of the panels. The infill strips are not installed until an area is complete. This means that panels can be adjusted for straightness and position even after adjacent panels have been installed. The difficulty with this method is that the end of the joint will not always be accessible (i.e. wall or window frame) and the infill strip 38 may have a tendency to catch on the attachment clips as it is being slid into the joint. To aid in the sliding of the strip, a tool may be used to pull the leading edge over the clips (not shown).
[0058] The finish faces of the panels may have a protective film 50 to protect against minor abrasions that may occur during handling and installation. The protective film may be peeled back from the returns of the panels before installing. To keep the panels clean and free of construction debris, generally the protective plastic film 50 is only removed from the faces of the panels once the landscaping has been completed, as seen in FIG. 17 .
[0059] The foregoing description illustrates only certain preferred embodiments of the invention. The invention is not limited to the foregoing examples. That is, persons skilled in the art will appreciate and understand that modifications and variations are, or will be, possible to utilize and carry out the teachings of the invention described herein. Accordingly, all suitable modifications, variations and equivalents may be resorted to, and such modifications, variations and equivalents are intended to fall within the scope of the invention as described and within the scope of the claims.
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The invention provides a dry joint wall panel attachment system, applying the rainscreen principle. Interlocking components are used to attach aluminum wall panels to an exterior wall.
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BACKGROUND OF THE INVENTION
The present invention relates to a heating element comprising an electrical resistance strip which is arranged in a predetermined pattern, for example, a meander-like pattern between sheets or layers of insulation material, the width of the insulation material sheets being wider than the resistance strip arrangement.
One problem which arises in connection with installation of such heating elements is that the element may be torn at the edges or at nail holes. Under certain conditions the element can be torn so that the resistance strip pattern is disturbed or broken, which is detrimental to the heating element.
SUMMARY OF THE INVENTION
The object of the present invention is to provide a heating element wherein an electrical resistance strip arrangement is laminated to at least one insulation sheet and reinforcing material is laminated to the insulation sheet rendering its less sensitive to tearing.
BRIEF DESCRIPTION OF THE DRAWING
The above-mentioned and other features and objects of the present invention will become more apparent by reference to the following description taken in conjunction with the accompanying drawing in which:
FIG. 1 illustrates a heating element according to the present invention, with one insulation sheet removed,
FIG. 2 illustrates a double heating element of the type shown in FIG. 1,
FIG. 3 illustrates a cross-section of an enlarged portion of the element shown in FIG. 1, taken at line III, and includes both insulation sheets,
FIG. 4 illustrates an enlargement of part of a heating element having an open mask type reinforcement, and
FIGS. 5 and 6 show a cross-section of the element shown in FIG. 4, taken at lines V and VI, respectively.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 illustrates a heating element 1 having an electrical resistance strip 2 arranged in a meander-shaped pattern, the electrical terminations being shown at 3 and 4. The resistance strip is laminated to at least one sheet of insulation material 5, the width of which is greater than that of the resistance strip arrangement. The free insulation areas outside the resistance strip arrangement are usually used for nailing or otherwise mounting the element to a wall, a ceiling or the like. In order to reinforce the insulation side areas there are, in accordance with the invention, provided sheets, tapes, fabric strips or the like of a reinforcement material 6. In a preferred embodiment the reinforcement is of the slightly stretchable textile web type so as to obtain the best possible bonding between the insulation sheet and the reinforcement. The requirement of the reinforcement is that it shall withstand at least the tearing forces of 10 Newtons for 10 seconds in any direction.
FIG. 2 illustrates the principle of the present invention applied to a so-called double heating element. As shown, this element consists of two resistance strip arrangements 10, 11 which may be connected in series or parallel, depending on the installation required. In this case there is also provided a reinforcement strip or the like 12 in the "side" area between the two resistance strip arrangements 10, 11, in addition to the outer reinforcements 13.
FIG. 3 illustrates a cross-section of the element shown in FIG. 1, taken at line III. The resistance strip 2 is laminated between two insulation sheets 5, and the reinforcements 6 are shown also to be laminated between the insulation sheets 5. In some cases there may be used only one insulation sheet to which the resistance strip 2 and reinforcement 6 are laminated. The reinforcements 6 which are placed in the "nailing" area of the heating element, should preferably have a thickness which is greater than that of the resistance strip in order to prevent the resistance strip from being subjected to unauthorized pressure during installation. When nailing the element onto a wall or ceiling the reinforcements will take up all or most of the pressure which would otherwise have undesirable effect on the resistance strip.
FIG. 4 schematically illustrates a side area section where the insulation sheets may be of the transparent type, and the reinforcement, which is of the slightly stretchable open mask textile web type, may be of a colored material. In this way mounting is facilitated since the mounting area will be clearly denoted.
Cross-sections of the side area shown in FIG. 4 are shown in FIGS. 5 and 6 indicating that the two insulation sheets 5 meet in the spaces between the horizontal and vertical threads 20, 21 of the reinforcement, so as to obtain the best possible bonding between the insulation sheets and the reinforcement.
While I have described above the principles of my invention in connection with specific apparatus it is to be clearly understood that this description is made only by way of example and not as a limitation to the scope of my invention as set forth in the objects thereof and in the accompanying claims.
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Electrical resistance strip heating element, the insulated side areas of which are mechanically reinforced in order to render the strip less sensitive to tearing. The reinforcement may be of a slightly stretchable open mask type textile web.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation application which claims the benefit of U.S. patent application Ser. No. 12/262,391, which was filed on Oct. 31, 2008, which claims the benefit of priority from U.S. Provisional Patent Application Ser. No. 61/001,176, which was filed Oct. 31, 2007.
FIELD OF THE INVENTION
[0002] The present invention relates to oil pumps, and in particular, a high-performance external involute gear-style oil pump that eliminates or greatly reduces cavitation in the oil pump, thereby increasing the efficiency and performance of the oil pump.
BACKGROUND OF THE INVENTION
[0003] Cavitation is an undesirable condition that often occurs in external involute gear-style oil pumps that are commonly used on internal combustion engines. Cavitation occurs when the static pressure at any point in the fluid flow of the fluid being pumped becomes less than the fluid's vapor pressure, thereby creating vapor bubbles in the inlet fluid stream. When this situation arises in an oil pump, vapor bubbles in the inlet oil stream reach the high-pressure side or outlet side of the oil pump and implode, thereby causing noise, vibration, and damage to any surface of the oil pump in which the imploding bubbles touch. The effects of cavitation can range from a loss of oil pump efficiency, a reduction in the oil pumps' output, or more serious effects, such as noise, vibration, and damage to the oil pump's components.
[0004] The onset of cavitation is determined by the oil pump's speed, capacity, and inlet design. In addition, external involute gear-style oil pumps tend to cavitate at relatively low operating speeds as compared to other pump designs. Cavitation has caused lubrication issues with many high-performance engines, since many of those engines utilize an external involute gear-style oil pump. Because of this condition, many high-performance engines utilize a dry sump oiling system; however, such dry sump oiling systems are more expensive and complex, thereby increasing the cost and maintenance of such systems.
SUMMARY OF THE INVENTION
[0005] The present invention provides a high-performance oil pump for pumping engine oil in an internal combustion engine in order to reduce or eliminate cavitation of the oil in the oil pump. The present invention provides a housing having an inlet for receiving oil and an outlet for discharging oil. At least two gears are rotatably and matingly disposed within a pumping chamber of the housing for pumping oil from the inlet to the outlet. An inlet passageway extends from the inlet to the inlet side of the pumping chamber, and an outlet passageway extends from an outlet side of the pumping chamber to the outlet. A pressure regulating circuit disposed within the housing redirects oil from the outlet side of the pumping chamber to the inlet passageway when the pressure differential between the outlet side of the pumping chamber and the inlet side of the pumping chamber exceeds a predetermined level in order to reduce or eliminate cavitation of oil in the oil pump.
[0006] The pressure regulation circuit of the present invention provides a pressure relief valve having a spool valve structure disposed within the bore of the housing. A redirect outlet passageway communicates with the outlet side of the pumping chamber and the pressure relief valve. A redirect inlet passageway communicates with the pressure relief valve and the inlet passageway. The pressure relief valve is moveable between a normally closed position, wherein oil is prevented from passing from the redirect outlet passageway to the redirect inlet passageway, and an open position, wherein oil is allowed to pass from the redirect outlet passageway to the redirect inlet passageway. The relief valve is biased in the closed position and moves from the closed position to the open position when the pressure differential between the redirect outlet passageway and the redirect inlet passageway exceeds a predetermined level.
[0007] The inlet of the housing provides an opening that is communicatable with a supply of oil, and the opening of the inlet has a larger diameter than the inlet passageway. A strainer is removably connected to and extends across the inlet for filtering oil and minimizing a pressure drop of oil prior to entering the inlet passageway. The inlet passageway has a longitudinal axis that extends directly from the inlet to the inlet side of the pumping chamber.
[0008] A venting passageway extends from the inlet to the bore in the housing for receiving the relief valve in order to maintain atmospheric pressure on both sides of the relief valve.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] Various other uses of the present invention will become more apparent by referring to the following detailed descriptions and drawings, and which:
[0010] FIG. 1 is an exploded view of the high-performance oil pump of the present invention;
[0011] FIG. 2 is a sectional view of the high-performance oil pump of the present invention;
[0012] FIG. 3 is a top plan view of the oil pump cover of the high-performance oil pump of the present invention;
[0013] FIG. 4 is a top plan view of the oil pump body of the high-performance oil pump of the present invention;
[0014] FIG. 5 is a sectional view of the oil pump cover of the high-performance oil pump of the present invention;
[0015] FIG. 6 is a sectional view of the high-performance oil pump of the present invention;
[0016] FIG. 7 is a top plan view of the high-performance oil pump of the present invention;
[0017] FIG. 8 is an isometric view of the oil pump cover of the high-performance oil pump of the present invention; and
[0018] FIG. 9 is an isometric view of the oil pump of the high-performance oil pump of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0019] Referring to the drawings, the present invention will now be described in detail with reference to the disclosed embodiments.
[0020] FIGS. 1-10 illustrate a high-performance oil pump 10 of the present invention for reducing or eliminating cavitation of oil in the oil pump 10 . The oil pump 10 provides a housing 12 having an oil pump body 14 and an oil pump cover 16 . The oil pump cover 16 has an inlet 18 formed therein for receiving oil (not shown) from an oil supply reservoir (not shown), such as an oil pan from an internal combustion engine (not shown). The inlet 18 is in communication with a hollow pumping chamber 20 formed in the oil pump body 14 of the housing 12 . An outlet 22 is also formed in the oil pump body 14 and is in communication with the pumping chamber 20 . A pair of gears 24 , 26 are rotatably disposed within the pumping chamber 20 of the oil pump body 14 and are driven by the engine. The gears 24 , 26 pump oil from the inlet 18 to the outlet 22 of the housing 12 , and the outlet 22 of the housing 12 is connected to and communicates with an engine block of the engine so as to provide oil to the engine block. A pressure regulation circuit 28 disposed within the housing 12 balances oil flow pressure between the inlet 18 and the outlet 22 by redirecting a portion of the oil from the outlet 22 to the inlet 18 of the oil pump 10 when the oil flow pressure differential between the outlet 22 and the inlet 18 reaches a predetermined level. By allowing oil to flow from the outlet 22 to the inlet 18 , especially under high speed engine conditions, an appropriate amount of oil is supplied to the inlet 18 , thereby ensuring a proper supply of oil to the pumping chamber 20 and reducing or avoiding cavitation of the oil in the oil pump 10 . By reducing or eliminating cavitation, the efficiency and performance of the oil pump 10 is increased.
[0021] In order to provide the housing 12 of the present invention with the appropriate structural strength and weight, the oil pump body 14 and the oil pump cover 16 of the housing 12 may be fabricated from billet 6061-T6 aluminum, which is hard-coated and anodized for durability. Although the noted aluminum is an ideal material for the housing 12 of the oil pump 10 , it should be noted that the present invention is not limited to such material, but rather, various other materials having similar strength and weight properties can be utilized.
[0022] The oil pump cover 16 has a substantially cylindrical configuration with the inlet 18 formed at an open end 30 of the oil pump cover 16 . The initial opening 32 of the inlet 18 extends across almost the entire width of the end 30 of the oil pump cover 16 . The initial opening 32 of the inlet 18 is relatively large and sized accordingly in order to reduce flow restriction of the oil. A steel mesh strainer 34 is seated within an annular recess 36 in the inlet 18 of the oil pump cover 16 , and a removable retaining ring 38 is also seated in an annular recess 40 in the inlet 18 of the oil pump cover 16 so as to secure the strainer 34 in the oil pump cover 16 . Since an oil filter (not shown) is typically downstream from the oil pump 10 , the oil being supplied from the oil pan to the oil pump 10 is not filtered. Thus, the strainer 34 filters any contaminates in the oil and prevents such contaminates from entering the oil pump 10 of the present invention while minimizing the amount of pressure drop across the strainer 34 . The retaining ring 38 can be easily removed from the oil pump cover 16 , thereby allowing regular maintenance to be performed on the strainer 34 . For example, the strainer 34 can be removed, cleaned, and replaced in the oil pump cover 16 . Since the strainer 34 can provide restriction of the oil flow into the inlet 18 , the initial opening 32 of the inlet 18 from the oil pump cover 16 is relatively large, as previously mentioned, to ensure for the proper flow of oil into the inlet 18 .
[0023] For oil to be pumped from the oil supply to the pumping chamber 20 , the inlet 18 in the oil pump cover 16 provides an inlet passageway 42 extending from and in communication with the initial opening 32 of the inlet 18 of the oil pump cover 16 . Although the inlet passageway 42 is smaller in diameter than the initial inlet opening 32 , the inlet passageway 42 is still larger than most conventional designs in order to reduce flow restriction of the oil. The length of the inlet passageway 42 is also designed to be as short a distance as possible to the pumping chamber 20 in order to reduce the restriction of flow to the incoming oil. Again, the initial opening 32 is larger than the inlet passageway 42 to ensure that there is no flow resistance caused by the strainer 34 . The inlet passageway 42 has a longitudinal axis that is laterally offset from the longitudinal axis of the oil pump cover 16 , and the inlet passageway 42 extends substantially straight through the oil pump cover 16 to communicate with an inlet side 43 of the hollow pumping chamber 20 provided in the oil pump body 14 . Thus, the inlet 18 provides communication between the oil supply and the pumping chamber 20 of the housing 12 .
[0024] In order to pump oil from the oil supply through the inlet 18 and out through the outlet 22 , the oil pump cover 16 has a substantially rectangular stepped configuration, wherein a substantially flat mating surface 44 on the oil pump cover 16 abuts a substantially flat mating surface 46 on the oil pump body 14 . Four apertures 48 extend through the mating surface 44 of the oil pump cover 16 and are correspondingly aligned with four threaded apertures 50 in the mating surface 44 of the oil pump body 14 . Four conventional threaded fasteners 51 extend through the apertures 48 and thread into apertures 50 to secure the oil pump cover 16 to the oil pump body 14 .
[0025] The gears 24 , 26 of the oil pump 10 are disposed within the hollow pumping chamber 20 of the oil pump body 14 wherein the pumping chamber 20 is open to the mating surfaces 44 , 46 of the oil pump body 14 and the oil pump cover 16 . The pair of gears 24 , 26 are external involute gears that are substantially similar and are designed to mesh together in a complementary manner. The first gear 24 has a throughbore extending along its longitudinal axis for receiving an idler shaft 52 wherein the first gear 24 is press fit onto the idler shaft 52 . The idler shaft 52 has one of its ends 54 received within a blind bore 56 provided in the mating surface 44 of the oil pump cover 16 . A small trough 55 provided on the mating surface 44 of the oil pump cover 16 directs oil from the pumping chamber 20 to the blind bore 56 to lubricate the end 54 of the idler shaft 52 . The other end 58 of the idler shaft 52 extends through a throughbore 60 in the oil pump body 14 . The throughbore 60 has a stepped-diameter to secure the idler shaft 52 in the housing 12 . The first gear 24 is then free to rotate with the idler shaft 52 within the pumping chamber 20 of the oil pump body 14 .
[0026] The second gear 26 also has a throughbore extending along the longitudinal axis of the second gear 26 . A drive shaft 62 is inserted through the throughbore of the second gear 26 wherein the second gear 26 is press-fit to the drive shaft 62 . One end 64 is seated within a blind bore 66 extending from the mating surface 44 of the oil pump cover 16 . A small trough 57 is provided on the mating surface 44 of the oil pump cover 16 to direct oil from the pumping chamber 20 to the blind bore 66 to lubricate the end 64 of the drive shaft 62 . A throughbore 68 extending through the oil pump body 14 receives the drive shaft 62 . A free end 70 of the drive shaft 62 extends outward beyond the oil pump body 14 and is coupled to a portion of the engine, such as a crankshaft or a camshaft. The second gear 26 is disposed within the pumping chamber 20 of the oil pump body 14 and rotates with the drive shaft 62 . The first and second gears 24 , 26 are situated such that when the second gear 26 is driven by the drive shaft 62 , the second gear 26 rotates in a meshing and complementary fashion with the first gear 24 . Since the drive shaft 62 is connected to the camshaft or crankshaft of the engine, the speed at which the gears 24 , 26 rotate is in direct relation to the speed of the engine.
[0027] To pump the oil from the inlet 18 through to the outlet 22 , an outlet passageway 72 extends from an outlet side 73 of the pumping chamber 20 of the oil pump body 14 to an outlet opening 78 which extends to an outside landing 74 on the oil pump body 14 . The outlet opening 78 is larger in diameter than the outlet passageway 72 and is relatively large and sized accordingly in order to reduce the restriction of oil flow. A through-hole 76 extending from the opposite side of the oil pump body 14 extends into the outlet opening 78 of the oil pump body 14 . The through-hole 76 allows for a fastener (not shown) to extend up through the through-hole 76 , thereby connecting the landing 74 of the oil pump body 14 directly to the engine block of an engine. This allows the oil pump 10 of the present invention to pump the oil from the inlet 18 to the outlet 22 and into the engine block of the engine.
[0028] In order to regulate and balance oil flow pressure between the outlet 22 and the inlet 18 of the oil pump, the pressure regulation circuit 28 provides a relief valve 80 slidably disposed within the oil pump cover 16 . The relief valve 80 is movable between a normally closed position, wherein oil is prohibited from flowing from the outlet 22 to the inlet 18 , and an open position, wherein oil is allowed to flow from the outlet 22 to the inlet 18 to ensure a proper supply of oil to the pumping chamber 20 , thereby reducing or avoiding cavitation of the oil in the oil pump 10 . The relief valve 80 is disposed within the oil pump cover 16 in a blind bore 82 extending through an integral boss 84 formed on the outside of the oil pump cover 16 . The relief valve 80 provides a spool valve 86 slidably disposed within the blind bore 82 for movement between the closed position and the open position. The spool valve 86 has a larger diameter portion 88 , which is slightly smaller than the diameter of the blind bore 82 , and a smaller diameter portion 90 that is integral with and extends from the larger diameter portion 88 of the spool valve 86 . The smaller diameter portion 90 of the spool valve 86 may abut the end of the blind bore 82 in order to prohibit further movement of the spool valve 86 at that end of the bore 82 . The larger diameter portion 88 of the spool valve 86 has a blind bore 92 extending from the end of the spool valve 86 . A helical compression spring 94 is inserted into the bore 92 of the spool valve 86 , wherein a portion of the helical compression spring 94 extends outward from the spool valve 86 and is housed within the blind bore 82 in the oil pump cover 16 . A plug 96 is threaded into corresponding threads provided in the opening of the blind bore 82 in the boss 84 of the oil pump cover 16 . The plug 96 secures the spool valve 86 and the gears 24 within the blind bore 82 in the oil pump cover 16 and acts as an abutment to one end of the compression spring 94 .
[0029] In order for the relief valve 80 to redirect oil from the outlet 22 to the inlet 18 when the flow pressure differential between the outlet 22 and the inlet 18 reaches a predetermined level, a redirected outlet passageway 98 is formed on the mating surface 44 of the oil pump cover 16 and is in communication with the outlet side 73 of the pumping chamber 20 . This redirected outlet passageway 98 extends from the pumping chamber 20 to the end of the blind bore 82 in the oil pump cover 16 that houses the relief valve 80 . This provides communication between the outlet 22 and the blind bore 82 housing the relief valve 80 . Thus, the outlet pressure of the oil is constantly in communication with the relief valve 80 , and when the outlet pressure becomes great enough to overcome the force of the compression spring 94 on the spool valve 86 , the spool valve 86 will begin to move against the force of the compression spring 94 . The compression spring 94 has a predetermined spring force that corresponds to a desired outlet pressure wherein oil from the outlet 22 is redirected to the inlet 18 .
[0030] When the outlet pressure becomes too great, the spool valve 86 moves to the open position, and oil is allowed to flow from the outlet 22 to the inlet 18 of the oil pump 10 . To redirect such flow of oil, a redirected inlet passageway 95 is provided by a pair of blind bores 100 that extends between the inlet passageway 42 and the blind bore 82 that houses the relief valve 80 . The blind bores 100 have longitudinal axes that are substantially perpendicular to the longitudinal axis of the inlet passageway 42 . Thus, the redirected inlet passageway 95 provides communication from the blind bore 82 housing the relief valve 80 to the inlet passageway 42 . At the end of the pair of blind bores 100 that extends outward from the oil pump cover 16 , a plug 101 is threaded into the oil pump cover 16 to maintain the oil within the oil pump 10 . Thus, when the outlet pressure becomes too great and the spool valve 86 moves to the open position, the oil from the redirected outlet passageway 98 travels into the blind bore 82 housing the relief valve 80 and into the redirected inlet passageway, which allow for oil to travel back to the inlet passageway 42 . This supply of oil is added to the normal supply of oil in the inlet 18 , thereby providing an additional supply of oil to the gears 24 , 26 within the pumping chamber 20 of the housing 12 . This additional supply of oil ensures a sufficient supply of oil so as to reduce or eliminate the onset of cavitation within the oil pump 10 . The redirected outlet passageway and the redirected inlet passageway are substantially straight and direct so as to reduce the length and turns within the redirected passageways. This assists in avoiding any flow restriction of the oil.
[0031] It should also be noted that a small venting passageway 102 extends from the inlet 18 to the backside of the spool valve 86 . This allows atmospheric pressure to be provided on the backside of the spool valve 86 so that the spool valve 86 can move freely between the open and closed positions, thereby avoiding vacuum within the blind bore housing the spool valve 86 .
[0032] In operation, the initial opening 32 of the inlet 18 of the oil pump 10 of the present invention may be located within an oil pan of an engine, and the outlet 22 of the oil pump 10 may be connected to the engine block of an engine. Once the engine begins operating, the drive shaft 62 of the oil pump 10 is driven by the crankshaft or camshaft of the engine. The drive shaft 62 drives the second gear 26 , which, in turn, drives the first gear 24 . As the gears 24 , 26 rotate, the un-meshing of the gears 24 , 26 create a local drop in pressure, which draws the oil into the inlet 18 of the oil pump 10 from the oil pan. The incoming oil flows into the pumping chamber 20 due to the un-meshing of the gears 24 , 26 . As the oil pump 10 speed increases with the engine speed, so does the speed of the gears 24 , 26 , and, as a result, the fill time of the oil into the pumping chamber 20 is reduced to the point at which the incoming oil does not have enough time to fill the pumping chamber 20 . This is when cavitation may start to occur.
[0033] In order to reduce or eliminate the onset of cavitation, the outlet pressure of the oil begins to reach a level wherein the spool valve 86 begins to move from the first or closed position, wherein oil is prohibited from flowing from the outlet 22 to the inlet 18 , to the second or open position, wherein a portion of the oil from the outlet 22 is allowed to flow to the inlet 18 . As the outlet pressure forces the spool valve 86 against the compression spring 94 , the spool valve 86 continues to move toward the open position until the larger diameter portion 88 of the spool valve 86 moves beyond the pair of blind bores 100 provided in the oil pump cover 16 . When this occurs, the spool valve 86 is in the open position, and a portion of the oil travels from the outlet side 73 of the pumping chamber 20 , through the redirect outlet passageway 98 , through the redirect inlet passageway 95 , through the inlet passageway 42 , and into the inlet side 43 of the pumping chamber 20 . This provides a sufficient amount of oil to the pumping chamber 20 so that the oil pump 10 does not begin to cavitate.
[0034] Once the oil pressure at the outlet 22 is reduced, such as by the slowing of the engine, the outlet pressure delivered to the spool valve 86 begins to drop. When this occurs, the compression spring 94 forces the spool valve 86 back toward the closed position, thereby closing the redirect inlet passageway to the inlet passageway 42 . This prohibits the flow of oil from the outlet 22 to the inlet 18 , as there is now a sufficient supply of oil to the pumping chamber 20 .
[0035] It should be noted that various engine configurations may require various oil pump 10 configurations of the present invention. For instance, the oil inlet 18 and strainer 34 may have to be a further distance laterally to communicate with the oil pan. In addition, height limitations may require a reduction in the number or a rerouting of the oil flow passageways. Lastly, various engine sizes may require various size oil pumps 10 of the present invention.
[0036] While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiments, but to the contrary, it is intended to cover various modifications or equivalent arrangements included within the spirit and scope of the appended claims. The scope is to be accorded the broadest interpretation so as to encompass all such modifications and equivalent structures as is permitted under the law.
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A high-performance oil pump for pumping oil in an internal combustion engine that eliminates or greatly reduces cavitation in the oil pump, thereby increasing the efficiency and performance of the oil pump. The present invention provides a housing having an inlet for receiving a supply of oil and an outlet for discharging the oil. At least two gears rotatably and matingly are disposed within the housing for pumping the oil from the inlet to the outlet. A pressure regulation circuit is disposed within the housing for balancing oil flow pressure between the inlet and the outlet by redirecting a portion of the oil from the outlet to the inlet when said oil flow pressure reaches a predetermined level at the outlet in order to reduce or eliminate cavitation of oil in the oil pump.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims priority to European Patent Application No. 13 173 019.4, filed Jun. 20, 2013, which is incorporated herein by reference in its entirety.
TECHNICAL HELD
[0002] The technical field relates to window technology. In particular, the technical field relates to aircraft window technology for an aircraft fuselage. More particularly, the technical field relates to a window element, a window system and a vehicle, in particular in aircraft, having a window shade.
BACKGROUND
[0003] Known window elements, in particular for aircraft applications, regularly comprise a transparent pressure proof window pane through which a passenger seated adjacent to the window may look through the same to get information about the surroundings of the aircraft. Regularly, such a window further comprises a window shade, embodied as a manually operated shade element, e.g. a plastic pull down/push up shade. In other words, the passenger is required to manually darken the window by pulling it down or remove the shade by pushing it up. In certain situations, e.g. emergency situations or while takeoff and landing, regulations require the window shades to be fully opened. During the flight however, the passenger may choose whether he/she wants to have an open window or whether to close the shade.
[0004] FIG. 1 shows two exemplary embodiments of aircraft windows. Each aircraft window 2 comprises a viewing area, i.e. an area where the passenger may look through to obtain information from the outside of the aircraft. The viewing area may be covered by a shade element 4 , and comprises a handle 6 for manually moving up and down the shade element 4 . In case the shade element 4 is moved completely downward, the window element/viewing area is darkened while when the shade element 4 is moved completely upwards, the viewing area is substantially free.
[0005] Establishing that all shades are open may be a cumbersome task for aircraft personnel during takeoff and landing while manually moving a plastic shade may lack a certain degree of convenience for the passenger.
[0006] In addition, other objects, desirable features and characteristics will become apparent from the subsequent summary and detailed description, and the appended claims, taken in conjunction with the accompanying drawings and this background.
SUMMARY
[0007] One of various aspects of the present disclosure may be seen in providing a novel window shade, a window element with such a window shade as well as a window system.
[0008] One of various aspects of the present disclosure is to replace the previously known manual pull down shade by a window shade element, that is an at least partially electrically darkable element. The window shade element may be moved at least between a first position and a second position, with the window shade element covering a first portion of the viewing area in the first position and a second portion of the viewing area in a second position. The first and second positions or the first and second portions are unequal.
[0009] According to one embodiment of the present disclosure, a window system having at least one window element according to the present disclosure is provided, wherein the window shade element is manually movable between the first position and the second position and wherein the window shade element and/or the electrically darkable element is controllable by a locally provided control element and also remotely controllable, in one example, centrally controllable.
[0010] According to one embodiment of the present disclosure, a vehicle, for example, an aircraft comprising at least one of the window system and the window element according to the present disclosure is provided.
[0011] The window shade element of the present disclosure may be comparable to the formally known manually movable plastic window shade in that it may be moved up and down to be either in front of the viewing area of the window element or at least partially removed from the viewing area of the window element. The window shade element may either be itself an electrically darkable element or it may be at least (partially) comprise an electrically darkable element. By using the electrically darkable element, the viewing area of the window element may be embodied at least having two different viewing modes, one viewing mode in which the electrically darkable element is substantially transparent or at least translucent, while in a further viewing mode the electrically darkable element is substantially non-transparent or darkened. Accordingly, the shade functionality in that the viewing area may be either presented to the passenger inside the aircraft or may be darkened so that the passenger may not see through the viewing area/window to the outside of the aircraft may be provided by either operating the electrically darkable element to be in a transparent or a non-transparent mode or by manually moving the window shade element. The electrically darkable element may be embodied as an element, which only requires energy when switching its state, i.e. when switching between transparent and non-transparent or when assuming a different level of translucency or opacity. Such an operation may be comparable to e.g. e-ink display of an e-book reader, which also requires energy only when switching pages but not when maintaining a certain depiction of a page.
[0012] According to one embodiment of the present disclosure, the window shade element itself may still be provided with the functionality of manually moving the shade element, so that it may be possible to remove the electrically darkable element itself from the viewing area, e.g. by moving the shade element upwards so that it resides in the fuselage of the aircraft and thus the passenger is having an unobstructed view of the viewing area through the pressure proof window pane of an aircraft window. Thus, the first position of the window shade element may thus be seen as the position in which it is substantially fully covering the viewing area while the second position may be considered to be the position in which the window shade element is substantially completely removed from the viewing area. As with previously known plastic shade elements, the window shade element may take up any arbitrary position between the first position and the second position, i.e. any position the window shade element may be moved to manually by pulling down or pushing up the shade element. In other words, the window element may be darkened by arranging the window shade element in the viewing area, while electrically darking the electrically darkable element. A non-darkened mode of the window element may be provided by either manually removing the window shade element and/or by operating the electrically darkable element in a transparent, non-darkened mode.
[0013] According to one embodiment of the present disclosure, the window shade element and/or the electrically darkable element may be embodied as a darkable glass, e.g. by employing micro-mirror arrays, an electrochromic element, a suspended particle device or a similar technology, in particular a technology that may switch between a darkened and a non-darkened state in a fast manner, in particular substantially instantaneously.
[0014] According to one embodiment of the present disclosure, the window shade element may be further provided with a photoelectric element, in particular a photovoltaic element, adapted to generate energy which can be employed for at least partially operating the electrically darkable element and/or the window shade element. In one example, the generated energy is employed for operating the electrically darkable element so that no further energy is required for its operation. In other words, the window element may be seen as being energy self-sufficient in that energy required for operation of the window element is generated by the photoelectric element of the same window element. The photoelectric element may be provided separately at the window element or it may be provided such that the electrically darkable element and the photoelectric element together constitute the window shade element. E.g., the photoelectric element may be a transparent or translucent element attached to an area of the electrically darkable element, thereby providing energy without influencing the ability to employ the electrically darkable element in one of a darkened and a transparent mode. The photoelectric element may partially be arranged in the viewing area, thus be only partially arranged on the window shade element and/or the electrically darkable element, while the photoelectric element may not be completely transparent, so long as at least some transparency remains so that a passenger may look through the window element, i.e. through the electrically darkable element, in an undarkened state, and the photoelectric element, and still sees the outside surroundings of the aircraft, it may be sufficient for the window element for providing its window functionality.
[0015] According to one embodiment of the present disclosure, a control element may be provided, arranged in the vicinity of the window element, i.e. arranged locally for operation by e.g. a passenger seated next to the window in a specific row in an aircraft. The control element may be incorporated in a specific seat, may be incorporated in more than one seat per row, e.g. all seats in a specific row associated with a respective window element or may be arranged at the window element itself, in the rim area or cover area of the aircraft fuselage. The control element may even be incorporated into/provided on the window shade element itself so that a user or passenger may control the electrically darkable element, in particular the opacity or transparency/translucency of the electrically darkable element. In other words, the control element may provide a switching functionality between either (completely) transparent and (completely) non-transparent, may provide specific levels of transparency in between or may even provide a substantially continuous controlling of transparency of the electrical darkable element by e.g. a slider functionality. The control element may thus control the electrically darkable element to be either transparent, non-transparent or to a certain degree translucent between transparent and non-transparent. The control element may e.g. be a capacitive control element or a comparable touch capable control element, which is affixed to the surface of the window shade element and/or the electrically darkable element. Thereby, a user of the window element may employ the control element attached to the window element itself, in particular to the window shade element or the electrically darkable element, e.g. by sliding a finger or the like on a specific surface of the control element, for setting a desired state of the electrically darkable element between and including completely transparent and completely non-transparent.
[0016] According to one embodiment of the present disclosure, the window element further comprises an energy storage element for storing energy for operating the electrically darkable element, in particular together with the control element, especially in a ease when insufficient energy may be generated by the photoelectric element to cover a certain current need of the electrically darkable element. The energy storage element may be a capacitive element, e.g. a capacitor arranged in the vicinity of the window element, in particular attached to the window shade element or the electrically darkable element. Also, the window shade element and/or the electrically darkable element may comprise the energy storage element. Thus, a discrete energy storage element may be provided or the window shade element and/or the electrically darkable element may comprise a further (functional) layer providing the energy storage capability. In the latter case, providing the energy storage element to be also transparent or at least translucent may be preferable. Also the photoelectric element may be provided as an additional layer of/on the window shade element and/or the electrically darkable element.
[0017] According to one embodiment of the present disclosure, the light employed for generating energy by the photoelectric element may be received from a first side and/or from a second side of the window element. The first side may e.g. be the interior side of the aircraft cabin while the second side may be the outside of the aircraft, thereby receiving light through the viewing area/the window pane. In case the electrically darkable element is not fully non-transparent, light may be received from either side, while, in case the electrically darkable element is substantially completely darkened, light may only be received from the side opposite of the electrically darkable element. Also, a photoelectric element may be arranged at both sides, e.g by providing two layers, of the electrically darkable element and thus may receive light from the first side and from the second side independently.
[0018] According to one embodiment of the present disclosure, the window shade element may be movable between the first position and the second position by a manual operation, in one example, directly engaging the window shade element and/or may be movable by an actuator element engaging the window shade element. In other words, the window shade element may e.g. be provided with a handle and may be operated as a previously known (plastic) window shade in that it may be moved up and down by a passenger or aircraft personnel. Thus, even in an emergency situation or in case of a malfunction of the window element, the window element, in particular in its darkened state, may be removed by manually moving the window shade element. Further, an actuator element may be arranged in the vicinity of a particular window element, which may move the window shade element, e.g. electrically or pneumatically. Energy for the actuator element may be provided by the energy storage element or externally from a further energy source, e.g. within the aircraft. Also, by the actuator element, the window shade element may be operated remotely, e.g. centrally from within the aircraft cabin, e.g. by aircraft personnel. In other words, either the electrically controllable element and/or the window shade element may be operated remotely, in one example, centrally from within the aircraft cabin. For example, in case of an emergency, a flight attendant could set ail electrically darkable elements of a specific aircraft to a non-darkened state and/or may remotely operate the actuator element to remove the window shade element from the viewing area by moving the window shade element by the actuator element. In case the energy storage element provides sufficient energy for operating either the electrically darkable element and/or the actuator element, only a control connection to a specific window element may be required. In case also energy is to be provided to the window element, said energy could be provided via the same control connection or via a further, separate dedicated energy connection.
[0019] According to one embodiment of the present disclosure, the electrically darkable element may be adapted to be selectively darkable, in one example, so that visual information may be visualized or presented on the electrically darkable element, e.g. to passengers of the aircraft seated adjacent to the window element in a specific seat row. By employing a certain technology for the electrically darkable element, it may e.g. comprise a specific pixel structure for providing the darkening. However, such a pixel structure may also be controlled such that individual pixels are darkened or non-darkened thereby allowing the presentation of text, pictures or other kinds of information, thereby enhancing the flight experience of the passengers. Also, information may be depicted by controlling the electrically darkable element such that information depicted is depicted by slightly reducing the non-transparency of certain pixels of the electrically darkable element, thereby e.g. employing the outside light surrounding the aircraft as a form of background illumination. Thus, it may not be required to steer certain areas or pixels of the electrically darkable element to be completely transparent but it may be sufficient to only partly reduce non-transparency. Thus, highlighted information, illuminated by light outside of the cabin, could be presented vs. a substantial darkened, non-transparent background.
[0020] According to one embodiment of the present disclosure, the window element further comprises a guiding element for accommodating the window shade element and for guiding the window shade element when being moved. In one example, a dedicated rail system or the like, comparable to a guiding element used for guiding a known window shade, may be employed. Subsequently, it may be preferred that the window element is embodied as an integral element comprising the electrically darkable element and at least one of the photoelectric element, the control element and the energy storage element. E.g., the window shade element may be provided as a shade shaped structure having a suitable width and length while featuring a comparably small thickness, with the electrically darkable element, the photoelectric element, the control element and/or the energy storage clement being embodied as individual layers of a suitable material attached to one another. E.g., the electrically darkable element and the photoelectric element may be attached to one another, e.g. glued to one another, while the energy storage element is provided by an energy storing functionality between the electrically darkable element and the photoelectric element, e.g. using a capacitive effect, thereby being capable of storing energy, while the control element, e.g. embodied as a (capacitive) touch control element is also attached to the electrically darkable element or the photoelectric element and provides its functionality through a surface contact area directly to the electronic structure of the electrically darkable element, the photoelectric element and/or in particular the energy storage element.
[0021] According to one embodiment of the present disclosure, the window clement further comprises a sensor element for detecting a fight level, in particular an ambient light level within the aircraft cabin and/or an exterior light level, external of the aircraft. The information obtained by the sensor element may thus be employed for controlling, in particular automatically controlling, the electrically darkable element. For example, in case a high level of light is outside of the cabin, e.g. when flying in sunlight or over a desert, the electrically darkable element could be darkened to a certain degree, to hinder a specific percentage of external light entering the cabin. Also, the operation or mode of the electrically darkable element could be controlled by a specific difference of light within and outside of the cabin. For example, in case of a completely darkened cabin during a night flight, it may not be required that the electrically darkable element is darkened. Also, e.g. at the end of the night, while the aircraft cabin still is substantially light-free or at least has a reduced light level, the electrically darkable element could be progressively darkened while the outside light level is rising, e.g. during sunrise. The same functionality may be provided, in reverse, during sunset.
[0022] According to one embodiment of the present disclosure, the window element may be embodied as an aircraft window element, in particular a window element for the passenger cabin.
[0023] According to one embodiment of the present disclosure, a window system with at least one window element according to the present disclosure is provided, whereby the window shade element is manually movable between the first position and the second position, wherein the window shade element and/or the electrically darkable element is controllable by a locally provided control element and wherein the window shade element and/or the electrically darkable element is remotely controllable, in one example, centrally controllable, e.g. from within the aircraft cabin by a flight attendant.
[0024] According to one embodiment of the present disclosure, a vehicle, in particular an aircraft, comprising one of a window system and/or a window element according to the present disclosure is provided.
[0025] Thus, the window element and in particular the window shade element may be embodied using a dust cover comparable to a previously known manual pull down shade, however constituting of the electrically darkable element, a photoelectric element or solar cell together with capacitive sensing. Such an embodiment would allow to reduce weight, would be dimmable with low maintenance requirements and in particular without wires, brackets and external power supply, in particular in case the window element comprises the energy storage element as well as a locally arranged control element, e.g. a switch or a touch control element in the window element itself. Such a system results in single item robustness. Sunlight from outside the cabin or light from within the cabin may thus provide the energy required for darkening or coloring, thereby removing the need for a dedicated power supply. The window element may feature external dimensions comparable to a common window element. Thus, the window element according to the present disclosure may be incorporated into existing aircraft cabin structures without redesign, while providing the same or comparable structural support as a common window element, since in particular only the shade itself of a previously known window is substituted by the window shade element of the present disclosure. Also, the window element of the present disclosure ma be the window shade element.
[0026] A person skilled in the art can gather other characteristics and advantages of the disclosure from the following description of exemplary embodiments that refers to the attached drawings, wherein the described exemplary embodiments should not be interpreted in a restrictive sense.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] The various embodiments will hereinafter be described in conjunction with the following drawing figures, wherein like numerals denote like elements, and wherein:
[0028] FIG. 1 shows two exemplary embodiments of aircraft windows;
[0029] FIG. 2 shows a cross-sectional view of an exemplary embodiment of the window element according to the present disclosure;
[0030] FIG. 3 shows an exemplary embodiment of a window element according to the present disclosure in operation; and
[0031] FIG. 4 shows an exemplary embodiment of a window system according to the present disclosure.
DETAILED DESCRIPTION
[0032] The following detailed description is merely exemplary in nature and is not intended to limit the present disclosure or the application and uses of the present disclosure. Furthermore, there is no intention to be bound by any theory presented in the preceding background or the following detailed description.
[0033] Now referring to FIG. 2 , an exemplary embodiment of the window element according to the present disclosure is depicted.
[0034] FIG. 2 shows a cross-sectional view of an aircraft fuselage with a window element. Window element 2 is situated in fuselage 28 with the inside of the aircraft 26 a depicted on the left side and the outside of the aircraft 26 b depicted on the right side of fuselage 28 and window element 2 . An outer window pane 24 is arranged at the window element 2 . It is also conceivable, that window element 2 and outer window pane 24 constitute an integral element that can be inserted into fuselage 28 and which also provides structural support for the aircraft/fuselage 28 . Window element 2 comprises window shade element 4 . Window shade element 4 is exemplarily embodied comprising a layered structure with an electrically darkable element 8 , a photoelectric element 10 , a control element 12 as well as a cover element 11 , e.g. a dust cover. Dust cover 11 however is not mandatory but may be provided to protect the window shade element 4 e.g. when a passenger rests against the window. An energy storage element 14 is provided, exemplarily incorporated into the window shade element 4 at its bottom as a separate element, e.g. a capacitive element. However, an additional layer, comparable to layers 11 , 8 and 10 , may be provided to provide the functionality of an energy storage element 14 . Control element 12 is only arranged at a specific location on the window shade element 4 , however my also be provided, alternatively, or additionally, in the fuselage section adjacent to the window element 2 , as depicted by element 12 ′. Exemplarily, control connection 16 is provided, which however is not mandatory, in particular in case the window element 2 is a standalone, self-sufficient window element as previously described, for controlling e.g. the electrically darkable element 8 and possibly a further actuator, not depicted in FIG. 2 , for moving the window shade element 4 , e.g. with regard to FIG. 2 to the upper part of fuselage 28 . Elements required for allowing the moving of the window shade element 4 are not depicted in FIG. 2 . It is also conceivable to provide window element 2 with a non-movable window shade element, which then however does not provide the emergency functionality of removing the window shade element manually. However, further applications are conceivable, where the emergency functionality may not be required. In case the window shade element 4 is not movable, the window shade element may comprise at least the elements of the electrically darkable element, the photoelectric element and possibly one of the dust cover element 11 , the control element 12 and the energy storage element 14 . A control connection 16 can also be provided to a non-movable window shade element 4 .
[0035] Photoelectric element 10 , e.g. a solar cell, is provided, which may receive light 18 , either from inside the cabin 18 a or from outside the cabin 18 b through the viewing area 21 . All elements of the window shade element 4 are generally transparent or at least translucent so that light from outside of the cabin 18 b may penetrate and enter the aircraft, while a passenger situated on the inside 26 a of the cabin may grasp the surroundings 26 b of the aircraft through viewing area 21 . Since the electrically darkable element 8 may be darkened, light 18 b could be prevented from entering the cabin, while a passenger seated inside the cabin could be hindered from seeing to the outside 26 b of the aircraft.
[0036] Sensor 36 is provided to Obtain information about a specific current light situation at the window element. Sensor 36 may be embodied such that it may differentiate between the light 18 a coming from within the cabin 26 a and the light 18 b coming from outside of the cabin 26 b and could thus automatically steer the electrically darkable element 8 according to the current light condition.
[0037] Now referring to FIG. 3 , an exemplary embodiment of a window element according to the present disclosure in operation is depicted.
[0038] FIG. 3 is an exemplary depiction of a window element according to the present disclosure seen by a passenger sitting adjacent to the window element. On the left side of axis 33 , the window shade element 4 is almost fully closed while the electrically darkable element 8 is in its darkened state. Thus, a passenger may not look to the outside 26 b of the aircraft. On the right side of axis 33 , a substantially transparent or at least translucent electrically darkable element 8 is depicted so that a passenger may look to the outside 26 b of the aircraft. Exemplarily, a building 35 , a church, is depicted in FIG. 3 . Thus, the passenger may look through the window shade element 4 and see the surroundings of the aircraft, thereby seeing the church. Information 34 is provided by the electrically darkable element 8 in the form of text and explains that the church 35 is called “St. Christopher”. Additional information 34 about the church or the surroundings in general could be provided by the electrically darkable element 8 .
[0039] Window shade element 4 is movable 20 , in FIG. 3 exemplarily upwards and downwards e.g. by a passenger employing handle 6 . A control element 12 a is provided on the surface of the window shade element 4 , e.g. a capacitive or touch-sensitive control element, while a further control element 12 b is depicted at a position, which is locally in the vicinity of window element 2 , however arranged at the aircraft fuselage 28 . In FIG. 3 , the first position, i.e. the fully closed position of the window shade element 4 is depicted by arrow 22 a while the fully opened position or second position is depicted by arrow 22 b. Regardless of a specific position 22 a, 22 b or any position in between said two positions, the window element may be darkened by using the electrically darkable element S. In case the window shade element 4 is in the second position 22 b, then the viewing area 21 and thus the outside 26 b of the cabin is always visible from within the aircraft cabin 26 a, thus allowing to quickly remove any shading of window element 2 , e.g. in an emergency situation or in case of a malfunction.
[0040] Now referring to FIG. 4 , an exemplary embodiment of a window system according to the present disclosure is depicted.
[0041] FIG. 4 shows a window system exemplarily comprising three rind& elements 2 a,b,c according to the present disclosure. Each window element 2 a,b,c is arranged adjacent to a seat row 37 a, 37 b, 37 c. Exemplarily only depicted with regard to seat row 37 b, apart from the functionality of window clement 2 as described with regard to either FIG. 2 and/or FIG. 3 , a control element 12 c is provided at the seat, e.g. incorporated into the arm rest of the aircraft seat. However, not only the passenger sitting next to the window element 2 may be provided with control element 12 c, but also one, more or all further seats of a specific seat row 37 may be provided with a control element 12 c ′, 2 c ″ for controlling window element 2 , in one example, the electrically darkable element 8 of said window element 2 .
[0042] Window element 2 in FIG. 4 however is not only locally controllable by either control element 12 , 12 a, 12 b or 12 c but may also be controlled by a remotely arranged control element 12 d via control connection 16 . An operator or flight attendant 32 may employ remote control element 12 d, in one example, as a centrally arranged control element for operating all window elements 2 /electrically darkable elements 8 at the same time. Control connection 16 could also provide energy to window elements 2 in case a window element 2 has no local energy storage element 14 or in case said local energy storage element 14 is depleted. Also, by using control connection 16 , the local energy storage elements 14 of multiple window elements 2 could act together as a common energy storage element 14 , i.e. energy source, thereby possibly sharing the stored energy of the energy storage elements 14 amongst the window elements 2 . It is conceivable to group window elements 2 with regard to a combined or common energy storage element 14 , so that e.g. only a sub-group of window elements 2 of an aircraft share their respective local energy storage elements 14 . With regard to FIG. 4 , e.g. window element 2 a,b,c could share their respective local energy storage element 14 amongst each other with further window elements 2 , not depicted in FIG. 4 , not sharing.
[0043] While at least one exemplary embodiment has been presented in the foregoing detailed description, it should be appreciated that a vast number of variations exist. It should also be appreciated that the exemplary embodiment or exemplary embodiments are only examples, and are not intended to limit the scope, applicability, or configuration of the present disclosure in any way. Rather, the foregoing detailed description will provide those skilled in the art with a convenient road map for implementing an exemplary embodiment, it being understood that various changes may be made in the function and arrangement of elements described in an exemplary embodiment without departing from the scope of the present disclosure as set forth in the appended claims and their legal equivalents.
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A window element having a window shade is provided. The window element has a viewing area, comprising a window shade element. The window shade element includes an electrically darkable element, and the window shade element is movable between a first position and a second position. In the first position, the window shade element is covering a first portion of the viewing area, and in the second position, the window shade element is covering a second portion of the viewing area. The first portion and the second portion are unequal.
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The .txt file entitled “Dec-13-2013-Substitute_ST25.txt” submitted herewith, created Dec. 13, 2013 and having a size of 4811 bytes, is incorporated herein by reference and sets forth the Sequence Listing.
RELATED APPLICATIONS
This application is a 371 of PCT/SE2007/051080 filed Dec. 21, 2007 and claims priority under 35 U.S.C. 119 of U.S. Application Ser. No. 60/876,958 filed Dec. 22, 2006.
FIELD OF THE INVENTION
The present invention relates to the field of allergy. More specifically, the invention relates to the identification of novel allergens from mammals and to diagnosis and treatment of allergy towards mammals.
BACKGROUND
Dog dander is a common cause of indoor allergy with symptoms including rhinitis, conjunctivitis, bronchial inflammation and asthma. Dog allergens can be detected not only in houses where dogs are kept as pets but also in other places such as schools and day care centres where dogs are not present on a regular basis (1).
Allergy to dog is accompanied and dependent of sensitization to proteins released from dog hairs and dander. In cases of suspected allergy to dog, the clinical investigation includes assessment of sensitization by skin prick or specific IgE antibody measurement using extract of dog hair and/or dander. A laboratory immunoassay for specific IgE, such as a Phadia ImmunoCAP, can detect most cases of sensitization to dog using natural dog dander extract due to favourable assay conditions and a large solid phase available for allergen attachment.
Dog hair and dander extracts contain a complexity of allergenic and non-allergenic proteins (2, 3). Three dog allergens have so far been identified and studied in detail: Can f 1, Can f 2 and Can f 3. Can f 1, a member of the lipocalin protein family, with reported molecular weight of 21-25 kD, was first purified by de Groot et al. (4) and later cloned and expressed as a recombinant protein (5). Can f 2 belongs to the same protein family but is a protein distinct from Can f 1 (4, 5). Can f 3, dog serum albumin, is a relatively conserved protein demonstrating extensive cross-reactivity to other mammalian albumins (6).
Of the known dog allergens, Can f 1 is the most important, binding IgE antibodies from approximately half of dog allergic subjects (7). About 20% of dog allergic subjects display IgE binding to Can f 2 but most of these are also sensitized to Can f 1. Although 30-40% of adult dog allergic individuals may show IgE binding to Can f 3 (2, 8), the specific clinical relevance of mammalian serum albumins is uncertain.
It has been known for a long time that major allergens relevant to allergy to rodents, such as mice and rats, are present in the animals' urine and these have been isolated and extensively characterized (9-13). IgE antibody binding activity has also been reported to exist in urine of other animals, including cats and dogs (14), but no allergen has been purified from urine of these animals and characterized at a molecular level.
SUMMARY OF THE INVENTION
As stated above, a laboratory immunoassay for specific IgE can detect most cases of sensitization to dog using natural dog dander extract due to favourable assay conditions and a large solid phase available for allergen attachment. However, in a miniaturized or non-laboratory immunoassay, such as an allergen microarray or a doctor's office test, the combination of less favourable assay conditions, lower capacity for antibody-binding allergen reagent and natural allergen extract of limited potency, has been found to cause insufficient diagnostic sensitivity. A similar situation may exist also for immunoassays for specific IgE to other animal epithelia. Thus, there is a need in some cases to use pure allergenic proteins to achieve sufficient sensitivity in diagnostic tests for specific IgE.
Furthermore, a significant proportion of dog allergic individuals also do not react to any of the known identified dog allergens and this was recently demonstrated in a Finnish population (7).
The above led the present inventors to look for additional, not yet identified, dog allergens. Such novel allergens may be useful not only as reagents for increased sensitivity in routine diagnostic tests, but also as a complement to known dog allergens in different types of component-resolved diagnostic applications (15, 16). Pure allergenic proteins, or fragments and variants thereof with improved non-anaphylactic properties, may also be used in component-resolved immunotherapy (16-20).
A new major allergen has thus been purified from dog urine and identified as prostatic kallikrein. It is in all aspects distinct from previously known dog allergens. Further, a similar or identical and immunologically equivalent allergen has been found to exist in dog dander extract. Kallikrein represents an important addition to the panel of known dog allergens and will be useful in the diagnosis of dog allergy. It is also anticipated that homologous proteins from other mammals, such as cat, horse and rodents, including rat and mouse, will have similar allergenic properties and diagnostic utility.
Prostatic kallikrein was found to exist not only in urine but also in the fur of dander of dogs. However, the fact that protein specifically expressed in prostate tissue would be restricted to male individuals, suggests that female dogs would lack this allergen. Preliminary results in our laboratory indeed support this notion and, if corroborated by results from more extensive studies, the implication would be that dog allergic individuals sensitized exclusively to prostatic kallikrein may tolerate female dogs.
In a recently published report, it was demonstrated that vaginal hypersensitivity reaction to ejaculate was associated with IgE sensitization to human prostate-specific antigen, PSA, present in seminal plasma (21). As canine and human prostatic kallikrein and human prostate-specific antigen have partial sequence similarity, it is possible that sensitization to canine prostate-specific kallikrein confers an elevated risk of developing such allergic reactions. It can also be envisaged that IgE-mediated immune reactions to prostate-specific kallikrein may play a role in certain cases of infertility in humans.
In one aspect the invention relates to the use of kallikrein in diagnosis of Type I allergy and the use of kallikrein for the manufacture of a composition for diagnosis of Type I allergy.
In a further aspect the invention relates to an allergen composition “spiked” with kallikrein. Such an allergen composition may be an allergen extract or a mixture of purified or recombinant allergen components having no or a low kallikrein content, wherein the kallikrein is added in order to bind IgE from patients whose IgE would not bind or bind poorly to the other allergen components in the composition. This aspect of the invention also relates to a method for producing such a composition, which method comprises the step of adding kallikrein to an allergen composition, such as an allergen extract (optionally spiked with other components) or a mixture of purified native or recombinant allergen components.
In yet a further aspect the invention relates to an in vitro diagnostic method for diagnosing a Type I allergy in a patient, wherein a body fluid sample such as a blood or serum sample from the patient is brought into contact with kallikrein or a composition according to the previous aspect, and it is detected whether or not the patient sample contain IgE antibodies that bind specifically to kallikrein. Such a diagnostic method may be carried out in any manner known in the art. The kallikrein may e.g. be immobilized on a solid support, such as in a conventional laboratory immunoassay, in a microarray or in a lateral flow assay.
In a further aspect the invention relates to a diagnostic kit for performing the method according to the previous aspect, which kit includes kallikrein.
In the above mentioned aspects, the wildtype kallikrein molecule may be replaced with fragments or variants of kallikrein, natural or man-made, sharing epitopes for antibodies with wildtype kallikrein, as defined below.
The invention further relates to a method of treatment of Type I allergy comprising administering to a patient in need of such treatment a kallikrein or a modified kallikrein, as explained below. This aspect of the invention also relates to the use of kallikrein in such immunotherapy, including e.g. component-resolved immunotherapy (16). In one embodiment of this aspect, the kallikrein may be used in its natural form or in a recombinant form displaying biochemical and immunological properties similar to those of the natural molecule. In another embodiment, kallikrein may be used in a modified form, generated chemically or genetically, in order to abrogate or attenuate its IgE antibody binding capacity, while preferably being capable of eliciting an IgG response in a treated individual. Examples of modifications include, but are not limited to, fragmentation, truncation or tandemerization of the molecule, deletion of internal segment(s), substitution of amino acid residue(s), domain rearrangement, or disruption at least in part of the tertiary structure by disruption of disulfide bridges or it's binding to another macromolecular structure, or by removal of the protein's ability to bind calcium ions or other low molecular weight compounds. In yet another embodiment of this aspect, the individual 10 kDa and/or the 18 kDa subunits of kallikrein, which display reduced IgE binding activity as compared to the intact molecule, are used as modified kallikrein.
In all of the above mentioned aspects of the invention, the kallikrein can be derived from any mammal producing kallikrein capable of inducing an allergic response in a patient. The kallikrein may be purified from its natural source, such as from urine, saliva or other body fluids, or from tissue, such as hair or dander, of the mammal in question. It may also be produced by recombinant DNA technology or chemically synthesized by methods known to a person skilled in the art.
The invention also relates to canine prostatic kallikrein for use in diagnosis and therapy, such as diagnosis and therapy of Type I allergy to dog.
The invention also relates to a method for purification of kallikrein from mammalian urine, comprising the steps
filtering the mammalian urine; buffer exchange with a buffer suitable for hydrophobic interaction chromatography; filtering of the buffer exchanged urine sample; applying the buffer exchanged urine sample to a hydrophobic interaction chromatography column; and collecting the flow-through fraction comprising kallikrein.
The mammalian urine may be canine urine.
DEFINITIONS
Kallikreins are proteolytic enzymes from the serine endopeptidase family found in normal blood and urine. In the IUBMB enzyme nomenclature system, plasma kallikrein has been assigned number EC 3.4.21.34 and tissue kallikrein number EC 3.4.21.35. Urinary kallikrein from dog is a 28 kDa heterodimeric protein comprising two subunits of approximately 10±2 and 18±2 kDa, respectively, for the purposes of this invention referred to as the 10 and 18 kDa subunits, respectively. It has an amino acid sequence according to SEQ ID NO: 1, GenBank Accession no: P09582, and homologous proteins have been described in a wide range of mammalian species, including, horse, cow, pig, mouse, rat and primates (e.g. Accession no AAQ23713-4 (horse), NP — 001008416 (cow), P00752 (pig), P00755-6 and P15947 (mouse), P36373 and P00758 (rat), Q28773 (baboon), XP — 001174026 (chimpanzee), Q07276 (macaque), P20151, Q07276 and AAM11874 (human).
Variants and fragments of a kallikrein should be construed as meaning proteins or peptides with a length of at least 10 amino acids, more preferably at least 50, even more preferably at least 75 or 100 amino acid residues, and a sequence identity to said kallikrein of at least 50%, preferably over 60%, 70%, 80%, 90% or 95%.
A modified kallikrein should in the context of the present invention be construed as meaning a kallikrein that has been chemically or genetically modified to change its immunological properties, e.g. as exemplified above in relation to the immunotherapy aspect of the invention.
Variants and fragments of kallikrein sharing epitopes for antibodies with wildtype kallikrein should be construed as being those fragments and variants whose binding of IgE antibodies from a serum sample from a representative kallikrein sensitized patient can be significantly inhibited by kallikrein. Such an inhibition assay may e.g. be performed according to the protocol disclosed in Example 8.
A hypoallergenic modified kallikrein or variant or fragment of kallikrein should be construed as being a modified kallikrein or variant or fragment of kallikrein that is not capable of binding kallikrein reactive IgE antibodies from a serum sample of a representative kallikrein sensitized patient, as determined e.g. by the protocol according to Example 3 or which displays no or significantly reduced biological allergen activity, as determined by a cellular activation assay such as the basophil histamine release assay (22, 23).
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 shows the fractionation of dog urinary proteins by size exclusion chromatography. Fractions comprising each of the three peaks indicated in the figure (labeled 1-3) were pooled as indicated for analysis of IgE binding activity.
FIG. 2 shows the purification of an IgE binding protein from peak 2 of FIG. 1 by reversed phase chromatography. The peak containing the protein selected for further investigation is indicated by an arrow.
FIG. 3 is an SDS-PAGE analysis of reduced (red) and non-reduced (ox) samples of the IgE binding protein purified from dog urine by size exclusion and reversed phase chromatography. Lane M contains molecular weight marker proteins.
FIG. 4 shows the effect of kallikrein as a fluid-phase inhibitor on specific IgE binding to immobilized dog dander extract.
FIG. 5 a - b is an assessment by immunoblot analysis of IgE antibody reactivity to dog dander extract in 37 dog allergic subjects' sera. Prior to incubation with the membrane strips, serum samples were diluted as indicated. Lane M contains molecular weight marker proteins.
FIG. 6 shows a comparison of the immunoblot signal intensity of a 28 kDa band, corrected for serum dilution, and the level of kallikrein-specific IgE, as determined by experimental ImmunoCAP analysis. The ImmunoCAP and immunoblot detection limits applied are indicated by hatched lines. Immunoblot signal intensity is expressed in arbitrary units (AU).
FIG. 7 shows specific immunoblot inhibition of the 28 kDa protein band by purified dog urinary kallikrein. Lane M contains molecular weight marker proteins.
FIG. 8 shows the first step of purification of kallikrein from dog dander, by size exclusion chromatography. Six fractions (labeled 1-6) indicated in the figure were analysed for IgE binding activity.
FIG. 9 shows the second step of purification of kallikrein from dog dander, by reversed phase chromatography. Top fractions of three peaks indicated in the figure (labeled 1-3) were analysed for IgE antibody binding activity.
FIG. 10 shows a comparative immunoblot analysis specific IgE antibody binding to dog dander extract, purified urinary kallikrein and partially purified kallikrein from dog dander. Two kallikrein-reactive sera (no. 6 and 8) and one kallikrein non-reactive serum (no. 11) were used. Both reduced and non-reduced forms of the allergen preparations were analysed, as indicated in the legend. Lane M contains molecular weight marker proteins.
FIG. 11 shows SDS Page analysis of purified recombinant dog urinary kallikrein.
FIG. 12 shows analytical gelfiltration analysis of purified recombinant dog urinary kallikrein.
FIG. 13 shows a comparison of specific IgE antibody binding activity of natural and recombinant dog urinary kallikrein.
DETAILED DESCRIPTION OF THE INVENTION
The examples below illustrate the present invention with the isolation and use of kallikrein from dog. The examples are only illustrative and should not be considered as limiting the invention, which is defined by the scope of the appended claims.
Example 1
Detection and Isolation of an IgE Binding Protein from Dog Urine
In order to investigate whether dog urine may contain allergens relevant to dog allergy in humans, the following experiments were performed. Urine was collected from a 7 year old male crossbreed between Siberian Husky and Vorsteh. After filtration through a 0.45 μm mixed cellulose ester filter, 10 mL of urine was applied to a Superdex 75 size exclusion chromatography (SEC) column (XK26/100, V t =505 mL, GE Healthcare Biosciences, Uppsala, Sweden) equilibrated with 20 mM MOPS pH 7.6, 0.5 M NaCl (MBS) and elution was performed with the same buffer at a flow rate of 2 mL/min. Fractions from three peaks were pooled as indicated in the chromatogram shown in FIG. 1 and analysed for allergen activity. The protein content of each fraction was immobilized on ImmunoCAP (Phadia, Uppsala, Sweden) solid phase and its IgE antibody binding activity tested using eight sera from dog dander sensitized individuals. Most of these sera were selected as having high IgE binding to dog dander extract but relatively low binding to rCan f 1, rCan f 2 and nCan f 3. Of the three peaks tested, peak 2 was found to contain by far the highest level of IgE binding activity (Table 1). Sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE) using the NuPAGE MES buffer system (10% NuPAGE gel, Invitrogen, Carlsbad, Calif., USA) of a reduced sample of peak 2 revealed two dominant protein bands, with apparent molecular weights of approximately 10 and 18 kDa, respectively (not shown).
Further protein purification from the pool corresponding to peak 2 was performed using a Source 15 reversed phase chromatography (RPC) column (ST4.6/100, V t =1.66 mL, GE Healthcare Biosciences). After addition of trifluoro acetic acid (TFA) to a final concentration of 0.065%, the pool was applied to the column, followed by washing with 9 column volumes of 0.065% TFA in water. Elution was performed with a 0-45% linear gradient of acetonitrile in water containing 0.05% TFA, resulting in one distinctive but somewhat asymmetrical peak ( FIG. 2 , peak indicated by an arrow). SDS-PAGE of reduced samples of fractions containing this peak revealed the presence of both the 10 and 18 kDa bands, seemingly unseparable ( FIG. 3 ). The fractions covering the entire peak were therefore pooled as indicated by horizontal bars in FIG. 2 . SDS-PAGE of a non-reduced sample of this pool revealed an additional band of 28 kD and a slight shift in mobility of the 10 kDa and 18 kDa bands ( FIG. 3 ). A faint protein band of approximately 55 kDa can also be seen in the non-reduced state, which may be a dimer of the 28 kDa protein. The occurrence of the 28 kDa band in the non-reduced state suggested that this protein may be made up of the 10 and 18 kDa polypeptides, joined together by one or more cystein bridge(s). The fact that linear mass spectromemetric analysis (data not shown) later showed dissociation of the 28 kDa component upon reduction and alkylation added further evidence to this notion.
Example 2
Identification of the IgE Binding Protein from Dog Urine as Prostate Kallikrein
Mass spectrometry and N-terminal sequencing was used to determine the identity of the IgE binding protein isolated from dog urine.
Peptide Mass Fingerprint Analysis by MALDI-TOF
For in-solution digestion of the RPC purified urinary protein, reduction and alkylation was performed by sequentialy adding to the sample DTT and iodoacetamide at approximately 45- and 100-fold molar excess, respectively. Trypsin digestion was then performed overnight at 37° C., using porcine trypsin (Trypsin Gold, mass spectrometry grade, Promega, Madison, Wis., USA). Samples containing digested peptides were spotted onto the MALDI target plate and α-cyano matrix in 50% acetonitrile, 10 mM NH 4 [H 2 PO 4 ], 0.1% TFA, was added. Following evaporation of the solvent, peptide mass fingerprinting (PMF) was performed in a Bruker Daltonics Autoflex 2 instrument (Bruker Daltonics, Bremen, Germany). To identify proteins matching PMF results obtained, the MSDB database was searched using a Mascot server (Matrixscience, London, UK). Post source decay (PSD) analysis was performed on selected peptides. External calibration was performed using a peptide calibration standard (Bruker Daltonics).
In-gel digestion analysis of the individual protein bands from SDS-PAGE was performed essentially according to Shevchenko (24). In summary, the 10, 18 and 28 kDa bands described in Example 1 above were excised from a Coomassie brilliant blue stained SDS-PAGE gel. The gel pieces were sequentially washed with 50 mM ammonium bicarbonate containing 50% acetonitrile followed by shrinking in pure acetonitrile. After rehydration of the gel piece with 50 mM ammonium bicarbonate, acetonitrile was added to 50% and following a second acetonitrile wash step, the gel pieces were dried in a vacuum centrifuge. eduction and alkylation was performed in sequence using 45 mM DTT and 100 mM iodoacetamide in 50 mM ammonium bicarbonate. After repeated washes with 50% acetonitrile in 50 mM ammonium bicarbonate and a final 100% acetonitrile wash, the gel particles were again dried down in a vacuum centrifuge. Trypsin digestion was performed overnight at 37° C. using porcine trypsin as described above. The digested sample was then sonicated and peptides extracted from the gel particles in 50% acetonitrile containing 0.1% TFA. Sample preparation and peptide mass fingerprinting was performed as described above.
The PMF analysis of the in-solution digested urinary protein resulted in a highly significant match (p<0.05) to prostatic kallikrein from dog (Accession no P09582). PSD analysis of two peptides, m/z=1224.6 and m/z=1632.8, which were also present in the in-gel digestion analysis of the 18 kDa band, gave significant database matches to the amino acid sequences FMLCAGVLEGK (SEQ ID NO: 2) and SHDLMLLHLEEPAK (SEQ ID NO: 3), corresponding to residues 194-204 and 117-130, respectively, of the same protein database entry.
Corroborating results were obtained from analysis of the in-gel digested protein bands as PMF of the 28 kDa band also yielded a highly significant database match (p<0.05) to kallikrein from dog (P09582) (SEQ ID NO: 1). Further evidence to the identity of the isolated urinary protein came from the analysis of in-gel digested samples of the 10 kDa band, PSD analysis of peptide m/z=1004.6 gave a highly significant (p<0.05) database match with the amino acid sequence SFIHPLYK (SEQ ID NO: 4), corresponding to residues 95-102 of P09582 (SEQ ID NO: 1).
N-Terminal Amino Acid Sequencing
For N-terminal sequencing, the reduced 10 kDa and 18 kDa protein bands were excised separately from a SDS-PAGE gel and extracted in 6 M guanidinium-HCl, 20 mM Tris pH 8.0, 0.5 M NaCl, using a plastic rod for homogenization. N-terminal sequence analysis of the extracted 10 kDa and 18 kDa bands, performed using a Hewlett-Packard G1000A instrument (Hewlett-Packard, Palo Alto, Calif.), yielded the amino acid sequences IIGGREXLKN (SEQ ID NO: 5) and AVIRPGEDRS (SEQ ID NO: 6), respectively, which were found to match residues 25-34 and 108-117 in the dog prostatic kallikrein precursor sequence of Accession no P09582 (SEQ ID NO: 1).
Taken together, the results described in this example demonstrate that the major constituent of the purified dog urinary protein, corresponding to the 10 and 18 kDa bands in reducing SDS-PAGE analysis, is identical to prostatic kallikrein from dog. Further, the observations suggest that the 10 and 18 kDa polypeptides are formed by posttranslational cleavage of a primary gene product and are held together by disulfide bridges to form the 28 kDa protein seen under non-reducing conditions, similar to what has previously been described for human kallikrein (25).
Prostatic kallikrein is also known as arginine esterase and carries that designation in database entries describing identical or nearly identical amino acid sequences, including NP — 001003284, CAA68720 and AAA30831. Further, we note that another variant of kallikrein, expressed in renal, pancreatic and salivary gland tissues, has been identified in dog (Accession No CAA53210) and shares 68% amino acid identity with prostatic kallikrein.
Example 3
Assessment of IgE Binding Activity of Kallikrein, rCan f 1, rCan f 2 and nCan f 3
In vitro IgE binding activity of the purified recombinant and natural dog allergens were examined using ImmunoCAP® (Phadia, Uppsala, Sweden), an immunoassay system used for specific IgE antibody measurement in clinical diagnosis of atopic allergy. Recombinant Can f 1 and Can f 2 (5) were cloned and expressed in E. coli essentially as described (26). Dog albumin was purified from serum using anion exchange chromatography and Blue Sepharose affinity chromatography, essentially as described (27). Experimental ImmunoCAP tests were prepared and used for serum analysis as described (26).
Sera from 37 dog allergic patients from Sweden (n=9), Spain (n=23) and North America (n=4) were used in the study. All patients had a positive skin prick test for dog dander extract and a doctors' diagnosis of dog allergy with symptoms of asthma, rhinoconjunctivitis and/or urticaria. All of the sera had a positive specific IgE test (ImmunoCAP) to dog dander extract.
The levels of specific IgE to dog dander extract, rCan f 1, rCan f 2, nCan f 3 and purified kallikrein are shown in Table 2 and a summary of the results is shown in Table 3. Of the tested sera, 29 showed IgE reactivity to kallikrein and 18 to rCan f 1. Both rCan f 2 and nCan f 3 appeared as minor allergens among the subjects studied, binding IgE from only 8 and 6 of 37, respectively. Fourteen of the 37 sera (38%) reacted only to kallikrein. On average among the kallikrein-reactive sera, the level of IgE binding to kallikrein amounted to 64% of the IgE binding to dog dander. The corresponding relative levels of IgE binding to rCan f 1, rCan f 2 and nCan f 3 were 45%, 25% and 47%, respectively, among sera specifically reactive to those allergens. Only two of the 37 sera tested lacked IgE reactivity to all of the four dog allergens. The IgE binding to kallikrein showed no correlation to any of the other dog allergens, demonstrating that the immune response to kallikrein is an independent variable and not a result of cross reactivity to Can f 1, Can f 2 or Can f 3.
The results obtained clearly demonstrated that prostatic kallikrein from dog is a major and unique allergen among the dog allergic subjects studied here. By both prevalence and magnitude of IgE binding, kallikrein was found to be the most important dog allergen so far described and among the subjects studied, over one third reacted to kallikrein but none of the other allergens tested.
Example 4
Demonstration of Kallikrein-Specific IgE Antibody Binding Activity in Dog Dander Extract
An IgE inhibition experiment was performed to examine whether dog dander contains epitopes capable of binding kallikrein-reactive IgE antibodies. Serum samples from three dog sensitized subjects (A-C) with IgE reactivity to kallikrein were first incubated for 2 h at room temperature with purified kallikrein at a final concentration of 100 μg/mL and, in parallel as negative controls, with serum diluent or the non-allergenic maltose binding protein (MBP) of E. coli . All samples were then analysed in duplicate for IgE binding to ImmunoCAP tests carrying immobilized dog dander extract to study whether preincubation with kallikrein specifically would prevent IgE binding to dander protein attached to the solid phase. As a control for specificity of kallikrein as inhibitor, a serum from a subject (D) sensitized to Can f 1 and Can f 2, but not to kallikrein, was included alongside the other sera in the experiment.
The results of the inhibition experiment are shown in FIG. 4 . Kallikrein purified from dog urine was found to completely inhibit the IgE binding to dog dander of two (A and B) of the three kallikrein-reactive sera and partly the binding of the third serum (C), which was known to be reactive also to other dog allergens. The negative control protein, MBP, showed no significant inhibitory effect as compared to serum diluent. In addition, no inhibition by kallikrein was observed on IgE binding of the Can f 1- and Can f 2-reactive serum (D).
The results demonstrated that epitope structures capable of binding kallikrein-reactive IgE antibodies are present in dog dander and, hence, are not confined to urine.
Example 5
Assessment of IgE Binding to a Kallikrein-Like 28 kDa Protein from Dog Dander Extract Using Immunoblot Analysis
With the aim to identify a protein present in dog dander to which the observed kallikrein-like allergen activity may be attributed, 37 sera with known levels of kallikrein-reactive IgE were used in an immunoblot experiment. Immunoblot analysis was performed on non-reduced dog dander extract separated by SDS-PAGE (12.5% Excel 2-D gel, GE Healthcare Biosciences) and electroblotted onto nitrocellulose membrane (Hybond ECL, GE Healthcare Biosciences). Protein blots were blocked for 1 h at room temperature using blocking buffer (50 mM phosphate pH 7.4, 0.1% (v/v) Tween-20, 0.9% (w/v) NaCl, 0.3% w/v) Dextran T10) and then incubated overnight with each patient's serum, diluted 1.5- to 20-fold in blocking buffer. The dilution factor for each serum is indicated in brackets at the top of its corresponding membrane strip in FIG. 5 . After washing in blocking buffer with 0.5% (v/v) Tween-20, the membrane was incubated 4 hrs at room temperature with an 125 I-labelled anti-human IgE antibody in blocking buffer and bound IgE was then radiographically detected using a storage phosphor screen and a Variable Mode Imager, Typhoon 9410 (GE Healthcare Biosciences).
The results of the experiment are shown in FIG. 5 a - b . Of the 37 sera used, 30 showed IgE binding to a 28 kDa protein while 21 showed IgE binding to a 23 kDa band, corresponding to Can f 1 and/or possibly Can f 2. Immunoblotting signal intensities were quantified using the Phoretix 1D software (Nonlinear Dynamics Ltd, Newcastle upon Tyne, UK). The level of IgE reactivity in each serum to individual bands was calculated by multiplying the signal intensity with the serum dilution factor. FIG. 6 shows a comparison of the level of IgE binding to the 28 kDa band in immunoblot analysis and the kallikrein ImmunoCAP measurements described in Example 3 above, revealing a close correlation.
In order to directly examine the relationship between urinary kallikrein and the 28 kDa band in dog dander, an immunoblot inhibition experiment was performed. A serum mono-reactive to the 28 kDa band was preincubated 2 hrs at room temperature with either purified urinary kallikrein or rCan f 1, both at a final concentration of 100 μg/mL, or with serum diluent. Membrane strips carrying immunoblottted non-reduced dog dander extract were then subjected to the preincubated serum samples and IgE binding was analysed as described above. The experiment revealed that IgE binding to the 28 kDa band in dog dander was completely abolished by serum preincubation with kallikrein whereas it remained unaffected by preincubation with both rCan f 1 and buffer alone ( FIG. 7 ).
Taken together, the results described in this example demonstrated the presence in dog dander extract of a protein displaying close electrophoretic and immunological similarity to urinary kallikrein.
Example 6
Partial Purification and Identification of Kallikrein in Dog Dander
The kallikrein-like protein from dog dander was purified by SECand RPC for biochemical identification. Three grams of dog dander (Allergon, Välinge, Sweden) was extracted in a 100 mL of MBS by end-over-end rotation for 3 hrs at room temperature. After centrifugation at 20,000×g and concentration using an Amicon filter (PM-10, Millipore, Billerica, Mass., USA), the extract was applied to an XK50/100 Superdex 75 column (GE Healthcare Biosciences) and eluted using MBS ( FIG. 8 ). Fractions from six peaks (indicated 1-6 in FIG. 8 ) were pooled and analysed for allergen activity. The protein content of each fraction was immobilized on ImmunoCAP (Phadia, Uppsala, Sweden) solid phase and its IgE antibody binding activity tested using eight sera from dog dander sensitized individuals, as indicated in Table 4. Most of these sera were selected as having high IgE binding to dog dander extract but relatively low binding to either of rCan f 1, rCan f 2 and nCan f 3. From Table 4 it is evident that peak 3 from the SEC separation contained the highest level of IgE binding activity of the six peaks tested. This pool was selected for further purification.
After adding TFA to a final concentration of 0.065%, the pool was applied to a ST4.6/100 Source 15 RPC column (GE Healthcare Biosciences) and elution was performed using a linear, 0-54% gradient of acetonitril in water containing 0.05% TFA ( FIG. 8 ). Analysis of allergen reactivity of the three peaks indicated in FIG. 9 was performed using five sera, selected by the criteria described above, The results of the analysis (Table 5) clearly showed that peak 1 contained the highest level of IgE antibody binding. Reducing SDS-PAGE analysis of this peak revealed the presence of 10 kDa, 18 kDa and 23 kDa protein bands (not shown).
The three band present in peak 1 were excised from the gel and subjected to in-gel digestion and mass spectrometric analysis as described in Example 2 above. While the 23 kDa band was identified as Can f 1, both the 10 kDa and 18 kDa bands were identified as dog prostatic kallikrein (Accession no P09582) after PSD analysis of selected peptides m/z=1004.52 and m/z=1632.98, respectively.
Further, the two 10 kDa and 18 kDa bands were eluted from excised gel bands and subjected to N-terminal amino acid sequencing. The resulting sequences, xIGGRExLKN (SEQ ID NO: 7) and AVXRPGEDRX (SEQ ID NO: 8), where “x” represents unresolved residues, matched residues 25-34 and 108-117 of the canine prostatic kallikrein precursor sequence, Accession no P09582 (SEQ ID NO: 1).
The results described in this example demonstrated that a protein with a primary structure identical or closely related to prostatic kallikrein is present in dog dander.
Example 7
Similar IgE Antibody Reactivity to Kallikrein from Dog Dander and Urine
To compare the IgE antibody binding activity of kallikrein from dog urine and dander, two kallikrein-reactive sera (sera no 6 and 8 from Table 2) and one kallikrein non-reactive serum (no 11) were used in immunoblot analysis of non-reduced samples of dog dander extract, purified urinary kallikrein and partially purified kallikrein from dog dander ( FIG. 10 ). The two kallikrein-reactive sera displayed IgE binding to a 28 kDa band in all three preparations, indicating that IgE binding at 28 kDa in dog dander extract is due to kallikrein. In addition, it was evident that the dominant reactivity to the 28 kDa band in purified urinary kallikrein coincided with the Coomassie stained protein bands of the same preparation. IgE binding to a band of about 55 kDa in the non-reduced kallikrein preparations is consistent with the notion in Example 1 above, of a putative dimer of kallikrein. The serum that was kallikrein non-reactive according to ImmunoCAP showed no IgE binding to the 28 kDa band in any of the three allergen preparations analysed.
The immunoblotting reactivity to reduced kallikrein-containing samples was considerably weaker than to non-reduced samples. Only the purified urinary kallikrein preparation, which had a higher kallikrein concentration than the other preparations analysed, gave rise to detectable IgE binding to the 18 kDa band formed upon reduction.
The observation that the immune reactivity to purified urinary kallikrein in immunoblot analysis was directed against the major protein band at 28 kDa served to support the validity of the experimental kallikrein ImmunoCAP test, in that its IgE binding was not caused a contaminant of the protein preparation used. The results further show that at least some IgE binding epitopes on kallikrein are sensitive to reduction of the molecule, as indicated by the weaker antibody binding to the 10 kDa and 18 kDa subunits, as compared to the 28 kDa unreduced molecule.
Example 8
Assessment of IgE-Binding Properties of a Modified Kallikrein or a Variant or Fragment of Kallikrein (Analyte)
The analyte is immobilized to a solid support, such as ImmunoCAP (Phadia, Uppsala, Sweden). Serum samples from at least three representative human patients sensitized to the relevant species and showing IgE reactivity to kallikrein from that species are incubated for 3 h at room temperature with kallikrein at a final concentration of 100 μg/mL and, in parallel as negative controls, with buffer alone and the non-allergenic maltose binding protein (MBP) of E. coli . The samples are then analysed for IgE binding to ImmunoCAP (Phadia, Uppsala, Sweden) tests carrying immobilized analyte to study whether preincubation with kallikrein specifically inhibits or significantly lowers IgE binding.
Example 9
Purification of Kallikrein from Dog Urine by Hydrophobic Interaction Chromatography (HIC)
A pooled sample of dog urine was filtered through a 5 μm and a 0.45 μm filter under nitrogen pressure. All chromatographic operations were performed with an ÄKTA Explorer 100 Air system (GE Healthcare Biosciences, Uppsala, Sweden). Four aliquots of 120 ml filtered dog urine was buffer exchanged using a Sephadex G-25 column (GE Healthcare Biosciences, Uppsala, Sweden) (column volume 461 ml), with cleaning of the column after each run. Buffer used: 50 mM Na-phosphate, 1 M (NH 4 ) 2 SO 4 , 0.02% NaN 3 , pH=7. The sample (about 505 ml) was then filtered through a 0.45 μm filter and applied to the HIC column (HiPrep Phenyl FF (high sub), 20 ml, GE Healthcare Biosciences, Uppsala, Sweden). Buffers used for HIC separation were: A) 50 mM Na-phosphate, 1 M (NH 4 ) 2 SO 4 , 0.02% NaN 3 , pH=7, and B) 50 mM Na-phosphate, 0.02% NaN 3 , pH=7. The flow through fraction (containing kallikrein) was collected in 10 ml fractions (Frac 950) at a flow rate of 5 ml/min and the flow through fractions were then pooled. The adsorbed material was eluted in a step gradient using 100% buffer B.
The fractions were analyzed using a BCA (bicinchoninic acid) assay, as well as SDS-PAGE (non reduced samples, silver staining). SDS-PAGE under non-reducing conditions revealed that kallikrein was found in the flow-through fractions which thus were pooled for further processing.
Two aliquots of about 125 ml and one aliquot of about 87 ml of the pooled HIC flow through fractions were buffer exchanged with a Sephadex G-25 SF column (GE Healthcare Biosciences, Uppsala, Sweden) to a buffer with the composition 20 mM Na-phosphate, 0.02% NaN 3 , pH=8. The kallikrein-pool (456 ml) was then concentrated on an Amicon cell (350 ml, Millipore filter, PBCC, cutoff 5000 kDa, diameter 76 mm) to a volume of about 43 ml. Using BCA assay, the protein concentration in the final pool was determined to be 0.9 mg/ml (in 43 ml=totally 38.7 mg) The sample applied to the HIC-column contained 101 mg protein which yielded a recovery of 38% of kallikrein after the HIC purification.
The purity of the kallikrein preparation was assessed by analytical gel filtration on a Superdex 75 HR 10/30 column in an ÄKTA purifier XT10 system. For this experiment the sample volume was 100 μl and the buffer was 10 mM Na-phosphate, 150 mM NaCl, 0.02% NaN 3 , pH=7.4.
Example 10
Identification and Characterization of Kallikrein from Dog Urine by the Use of Electrophoresis and Mass Spectrometry
Using electrophoresis the following samples were compared on the same gel, applying colloidal coomassie brilliant blue (CBB) staining:
1. A standard molecular weight marker
2. Dog urine
3. HIC-eluted material (reduced)
4. HIC flow-through fraction (reduced)
5. HIC flow-through fraction (non-reduced)
6. HIC-eluted material (non-reduced)
For samples 2, 3 and 6, a large number of proteins were detected. However, in sample 4 (reduced HIC flow-through fraction), only two main bands could be seen. These two bands were later, by the use of MALDI-TOF(-TOF) analysis (see below), found to correspond to two different variants of the kallikrein protein (as a result of proteolysis at R107, due to arginin-esterase activity). In sample 5 (non-reduced HIC flow-through fraction), seven distinct bands were detected and all bands were found to correspond to different variants of the kallikrein protein by the use of MALDI-TOF(-TOF) analysis (see below). Kallikrein comprises 12 cystein-residues, therefore the formation of different variants is possible under non-reducing conditions due to formation of cystein-cystein bridges. Thus, the formation of for example dimers, trimers etc is likely to happen under non-reducing conditions.
SDS-PAGE Conditions, Trypsin Digestion and MALDI-TOF-TOF Analysis:
Diluted samples were prepared using a SDS-PAGE cleanup kit according to the procedure recommended in the manual from the supplier (GE Healthcare, Uppsala, Sweden). The gels were run in a MES buffer at 200 V for 35 minutes. Reduced and non-reduced samples were run in separate aggregates. Staining was done overnight with colloidal CBB (de-staining was later done using water immersion for about 5 hours). Samples were manually picked from the gel using a pipette tip, and treated according to a standard protocol (using ethanol instead of acetonitrile), incubated with 12.5 ng/μl trypsin over night at 37 degrees Celsius. 0.5 μl of the digested samples was applied on the target plate for the MALDI system and mixed with 0.5 μl MALDI matrix solution (saturated solution of HCCA in 50% acetonitril, 0.1% TFA). All samples were analyzed, using a MALDI-TOF-TOF (Bruker Daltonics, Bremen, Germany) mass spectrometer. To identify proteins matching PMF results obtained, the MSDB database was searched using a Mascot server (Matrixscience, London, UK). MS-MS analysis was performed on selected peptides. External calibration was performed using a peptide calibration standard (Bruker Daltonics). Database searches were run using the following search criteria:
Taxonomy: mammalia
Mass tolerance: 100 ppm
Allowing for oxidized methionines and 1 missed cleavage.
Kallikrein sequence from the database:
(SEQ ID NO: 1) MWFLALCLAMSLGWTGAEPHFQPRIIGGRECLKNSQPWQVAVYHNGEFAC GGVLVNPEWVLTAAH CANSNCEVWLGR HNLSESEDEGQLVQVRK SFIHPL YKTKVPRAVIRPGEDRSHDLMLLHLEEPAK ITKAVRVMDLPKKEPPLGST CYVSGWGSTDPETIFHPGSLQCVDLKLLSNNQCAKVYTQKVTK FMLCAGV LEGK KDTCKGDSGGPLICDGELVGITSWGATPCGKPQMPSLYTR VMPHLM WIKDTMK ANT
(Peptide sequences identified by MALDI-TOF (/TOF) MS (/MS) in bold italic.)
Example 11
Cloning, Purification and Assessment of the IgE Binding Activity of Recombinant Dog Kallikrein Expressed in Pichia pastoris
In order to verify the identification and importance of urinary kallikrein as a dog allergen, the protein was produced as a recombinant allergen using Pichia pastoris as expression host, purified and analysed for IgE antibody binding activity.
Preparation of Synthetic Gene Construct Encoding Dog Urinary Kallikrein
A synthetic dog urinary kallikrein gene was designed by back-translating into nucleotide sequence the part of the reported amino acid sequence of dog prostatic arginine esterase (urinary kallikrein, Acc. No. P09582) corresponding to the mature protein. The nucleotide sequence was designed for optimal codon usage and synonymously adjusted to minimize secondary structures and eliminate or add restriction enzyme sites as desired. Oligonucleotides corresponding to the final coding sequence were obtained and assembled, and the full-length synthetic gene amplified by PCR and cloned into the XhoI and SalI sites of vector pPICZ A (Invitrogen, Carlsbad, Calif., USA), adding a C-terminal hexahistidine tag to enable protein purification by immobilised metal ion affinity chromatography (IMAC). The plasmid DNA construct was linearized by Sac I digestion and transformed into P. pastoris strain X-33 for homologous recombination into the chromosomal AOX1 locus.
Expression and Purification of Recombinant Dog Kallikrein-2
The recombinant protein was produced in Pichia pastoris strain X-33 (Invitrogen) using a 7 L bioreactor (Belach Bioteknik, Solna, Sweden). A rich broth medium (20 g/L peptone, 10 g/L yeast extract, 3.4 g/L yeast nitrogen base, 10 g/L ammonium sulfate, 0.4 mg/L biotin and 0.1 M potassium phosphate) was used and the cultivation carried out at 30° C. Expression was induced and maintained by feeding methanol to the culture to a steady-state concentration of 0.1% (v/v). After 70 hrs of fermentation, the culture was harvested by centrifugation at 10 000 g for 10 min at +4° C. and the supernatant recovered for protein purification.
The supernatant was conditioned for purification by adding imidazole to 5 mM and NaCl to 0.15 M and adjusting the pH to 7.2 using Tris base (s) before applying it to a Streamline 25 chelating column (GE Healthcare Biosciences), charged with NiSO 4 according to the manufacturer's recommendation. After loading, the column was washed in separate steps with 20 mM and 60 mM imidazole and the recombinant protein was then eluted with 500 mM imidazole, all in a buffer composed of 20 mM Tris-HCl pH 8.0 and 0.15 M NaCl.
Further purification of the recombinant protein was performed using cation exchange chromatography. IMAC fractions containing recombinant kallikrein were identified by SDS-PAGE, pooled and diluted with 2 volumes of 20 mM MES pH 6.0. After adjusting pH to 6.0, the diluted pool was applied to an XK26/100 SP Sepharose FF column (GE Healthcare Biosciences). The column was then washed with 2 column volumes of 0.15 M NaCl in 20 mM MES pH 6.0 and the recombinant protein eluted with 0.30 M NaCl in the same buffer. The protein concentration was determined from absorbance at 280 nm, using a calculated extinction coefficient of 1.46 per mg/mL.
Although the synthetic kallikrein gene construct was designed to direct the production of a single polypeptide chain, the protein purified from the culture medium was found to have undergone a partial cleavage into 18 kDa and 12 kDa chains ( FIG. 11 ), similar to the processing of natural urinary kallikrein. Indeed, N-terminal sequencing revealed that the recombinant kallikrein had been cleaved at the same position as the natural molecule (data not shown).
To assess the aggregation state and integrity of the recombinant protein under physiological conditions, a sample of the preparation was subjected to analytical size exclusion chromatography. As shown in FIG. 12 , the chromatogram was dominated by a single symmetrical peak, corresponding to a molecular weight of 34 kDa as defined by the LMW Calibration Kit (GE Healthcare Biosciences). The analysis demonstrated that the recombinant protein, despite its partial processing, was held together in solution and existed in a homogeneous, most likely monomeric, aggregation state.
IgE Binding Activity of Recombinant Kallikrein
The immunological activity of the recombinant kallikrein produced was assessed in comparison to the natural protein purified from dog urine. The two proteins were immobilised separately on ImmunoCAP® solid phase and their in vitro IgE binding capacity was examined using the 37 serum samples from dog allergic subjects described in Example 3 above.
As can be seen in FIG. 13 , the two datasets showed a very strong correlation (r=0.9988), demonstrating that the recombinant kallikrein produced closely resembled natural urinary kallikrein with respect to IgE antibody binding. Drawing from the complete absence of any other dog-derived protein in the recombinant protein preparation, it can be further noted that the results eliminate any possible doubt as to the identity of the active component of the natural kallikrein preparations described in the previous examples.
TABLE 1
Specific IgE binding activity of three size
exclusion chromatography peaks of dog urine
Peak no
Serum
1
2
3
A
0.72
75.87
neg
B
0.62
0.59
neg
C
1.32
14.71
0.35
D
1.32
14.47
neg
E
1.08
7.98
neg
F
0.81
6.38
neg
G
0.48
2.35
neg
H
0.54
1.83
neg
The protein content of pooled fractions of each peak was immobilized on ImmunoCAP solid phase for analysis of IgE binding activity, using serum samples from 8 dog allergic subjects. Values given are kU A /L of specific IgE.
TABLE 2
Specific IgE analysis of sera from 37 dog allergic subjects
Serum
dog dander
rCan f 1
rCan f 2
nCan f 3
kallikrein
1
44.5
32.14
neg
neg
0.73
2
27.1
9.60
4.36
neg
7.48
3
2.66
1.21
0.60
0.67
neg
4
1.89
neg
neg
neg
0.74
5
3.86
1.38
neg
neg
1.60
6
>100
neg
neg
neg
>100
7
5.92
neg
neg
neg
5.88
8
16
neg
neg
neg
24.98
9
5.2
neg
neg
neg
neg
10
3.14
1.92
neg
neg
0.89
11
2.9
0.84
neg
neg
neg
12
4.5
1.30
neg
neg
1.53
13
1.9
neg
neg
neg
1.61
14
4.31
neg
neg
neg
2.83
15
2.75
neg
neg
neg
2.68
16
1.64
neg
neg
neg
1.50
17
>100
11.04
2.21
28.20
0.72
18
2.2
neg
neg
neg
1.48
19
4.38
1.78
1.19
neg
0.49
20
3.19
neg
neg
neg
1.88
21
9.86
neg
neg
nog
11.17
22
3.43
1.19
neg
neg
neg
23
1.58
3.75
neg
neg
neg
24
2.27
neg
neg
neg
neg
25
1.57
neg
0.80
neg
neg
26
10.8
neg
neg
19.09
7.46
27
4.6
neg
neg
neg
3.95
28
34.8
neg
neg
1.45
25.32
29
2.39
1.06
neg
neg
1.56
30
8.85
neg
neg
neg
8.26
31
21.5
5.83
neg
8.76
1.34
32
3.17
neg
neg
neg
2.71
33
57.5
12.25
neg
neg
81.53
34
8.07
2.32
neg
neg
neg
35
22.1
4.04
6.06
1.97
7.28
36
3.85
0.44
1.22
neg
0.66
37
7.41
1.78
1.36
neg
5.00
Specific IgE was determined using ImmunoCAP tests carrying immobilized dog dander extract, rCan f 1, rCan f 2, nCan f 3 and dog urinary kailikrein. Values given are kU A /L of specific IgE. Values below a cut-off of 0.35 kU A /L are assigned as negative.
TABLE 3
Prevalence of specific IgE reactivity among 37 dog allergic subjects
No. of test results
dog dander
rCan f 1
rCan f 2
nCan f 3
kallikrein
in total
37
37
37
37
37
negative
0
19
29
31
8
>0.35 kU A /L
37
18
8
6
29
of specific IgE
>0.35 kU A /L
22
7
2
3
12
of specific IgE
The data comprise a summary of the results shown in Table 2
TABLE 4
Specific IgE binding activity of six size exclusion
chromatography peaks of dog dander extract
Peak no.
Serum
1
2
3
4
5
6
a
1.10
1.50
4.11
0.70
0.63
0.61
b
1.34
1.66
5.61
0.70
neg
neg
c
1.40
1.70
2.51
1.71
1.43
1.31
d
0.89
1.06
2.29
0.47
0.37
0.36
The protein content of top fractions of each peak was immobilized on ImmunoCAP solid phase for analysis of IgE binding activity, using serum samples from 4 dog allergic subjects. Values given are kU A /L of specific IgE.
TABLE 5
Specific IgE
binding activity of three reversed phase
chromatography peaks of dog dander extract
Peak no
Serum
1
2
3
a
15.82
neg
neg
b
14.00
0.75
0.42
d
4.77
0.60
0.42
e
1.45
0.80
0.53
f
neg
0.94
1.04
The protein content of top fractions of each peak was immobilized on ImnunoCAP solid phase for analysis of IgE binding activity, using serum samples from 5 dog allergic subjects. Values given are kU A /L of specific IgE.
REFERENCES
1. Custovic A, Green R, Taggart S C O, Smith A, Pickering C A C, Chapman M D et al. Domestic allergens in public places II: dog (Can f 1) and cockroach (Bla g 2) allergens in dust and mite, cat, dog and cockroach allergens in the air in public buildings. Clinical & Experimental Allergy 1996; 26:1246-1252.
2. Spitzauer S, Schweiger C, Anrather J, Ebner C, Scheiner O, Kraft D et al. Characterisation of dog allergens by means of immunoblotting. International Archives of Allergy and Immunology 1993; 100:60-67.
3. Spitzauer S. Allergy to mammalian proteins: At the borderline between foreign and self? [Review]. International Archives of Allergy and Immunology 1999; 120:259-269.
4. de Groot H, Goei K G H, van Swieten P, Aalberse R C. Affinity purification of a major and a minor allergen from dog extract: serologic activity of affinity-purified Can f I and of Can f I-depleted extract. Journal of Allergy and Clinical Immunology 1991; 87:1056-1065.
5. Konieczny A, Morgenstern J P, Bizinkauskas C B, Lilley C H, Brauer A W, Bond J F et al. The major dog allergens, Can f 1 and Can f 2, are salivary lipocalin proteins: cloning and immunological characterization of the recombinant forms. Immunology 1997; 92:577-586.
6. Boutin Y, Hebert H, Vrancken E R, Mourad W. Allergenicity and cross-reactivity of cat and dog allergenic extracts. Clinical Allergy 1988; 18:287-293.
7. Saarelainen S, Taivainen A, Rytkonen-Nissinen M, Auriola S, Immonen A, Mantyjarvi R et al. Assessment of recombinant dog allergens Can f 1 and Can f 2 for the diagnosis of dog allergy. Clinical & Experimental Allergy 2004; 34:1576-1582.
8. Cabanas R, Lopez-Serrano M C, Carreira J, Ventas P, Polo F, Caballero M T et al. Importance of albumin in cross-reactivity among cat, dog and horse allergens. Journal of Investigational Allergology & Clinical Immunology 2000; 10:71-77.
9. Bayard C, Holmquist L, Vesterberg O. Purification and identification of allergenic alpha (2u)-globulin species of rat urine. Biochim Biophys Acta 1996; 1290:129-134.
10. Ohman J L. Allergy in man caused by exposure to mammals. J Am Vet Med Assoc 1978; 172:1403-1406.
11. Schumacher M J. Characterization of allergens from urine and pelts of laboratory mice. Mol Immunol 1980; 17:1087-1095.
12. Siraganian R P, Sandberg A L. Characterization of mouse allergens. Journal of Allergy and Clinical Immunology 1979; 63:435-442.
13. Taylor A N, Longbottom J L, Pepys J. Respiratory allergy to urine proteins of rats and mice. Lancet 1977; 2:847-849.
14. Hoffman D R. Dog and cat allergens: urinary proteins or dander proteins? Annals of Allergy 1980; 45:205-206.
15. Hiller R, Laffer S, Harwanegg C, Huber M, Schmidt W M, Twardosz A et al. Microarrayed allergen molecules: diagnostic gatekeepers for allergy treatment. FASEB Journal 2002; 16:414-416.
16. Valenta R, Lidholm J, Niederberger V, Hayek B, Kraft D, Gronlund H. The recombinant allergen-based concept of component-resolved diagnostics and immunotherapy (CRD and CRIT). Clinical & Experimental Allergy 1999; 29:896-904.
17. Cromwell O, Fiebig H, Suck R, Kahlert H, Nandy A, Kettner J et al. Strategies for recombinant allergen vaccines and fruitful results from first clinical studies. Immunol Allergy Clin North Am 2006; 26:261-281, vii.
18. Gafvelin G, Thunberg S, Kronqvist M, Gronlund H, Gronneberg R, Troye-Blomberg M et al. Cytokine and antibody responses in birch-pollen-allergic patients treated with genetically modified derivatives of the major birch pollen allergen Bet v 1. International Archives of Allergy and Immunology 2005; 138:59-66.
19. Jutel M, Jaeger L, Suck R, Meyer H, Fiebig H, Cromwell O. Allergen-specific immunotherapy with recombinant grass pollen allergens. Journal of Allergy and Clinical Immunology 2005; 116:608-613.
20. Mahler V, Vrtala S, Kuss O, Diepgen T L, Suck R, Cromwell O et al. Vaccines for birch pollen allergy based on genetically engineered hypoallergenic derivatives of the major birch pollen allergen, Bet v 1. Clinical & Experimental Allergy 2004; 34:115-122.
21. Weidinger S, Mayerhofer A, Raemsch R, Ring J, Kohn F M. Prostate-specific antigen as allergen in human seminal plasma allergy. Journal of Allergy and Clinical Immunology 2006; 117:213-215.
22. Demoly P, Lebel B, Arnoux B. Allergen-induced mediator release tests. Allergy 2003; 58:553-558.
23. Ebo D G, Hagendorens M M, Bridts C H, Schuerwegh A J, De Clerck L S, Stevens W J. In vitro allergy diagnosis: should we follow the flow?[Review]. Clinical & Experimental Allergy 2004; 34:332-339.
24. Shevchenko A, Wilm M, Vorm O, Mann M. Mass spectrometric sequencing of proteins silver-stained polyacrylamide gels. Anal Biochem 1996; 68:850-858.
25. Frenette G, Deperthes D, Tremblay R R, Lazure C, Dube J Y. Purification of enzymatically active kallikrein hK2 from human seminal plasma. Biochim Biophys Acta 1997; 1334:109-115.
26. Marknell DeWitt Å, Niederberger V, Lehtonen P, Spitzauer S, Sperr W R, Valent P et al. Molecular and immunological characterization of a novel timothy grass ( Phleum pratense ) pollen allergen, Phl p 11. Clinical 85 Experimental Allergy 2002; 32:1329-1340.
27. van Eijk H M, Rooyakkers D R, van Acker B A, Soeters P B, Deutz N E. Automated isolation of high-purity plasma albumin for isotope ratio measurements. J Chromatogr B Biomed Sci App 1999; 731:199-205.
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Prostatic kallikrein for the manufacture of a diagnostic or pharmaceutical composition for diagnosis/treatment of type 1 allergy, especially allergy to dogs.
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FIELD OF THE INVENTION
[0001] The present invention relates to improving the continuity of a catalyst comprising a phosphinimine ligand and a hetero atom ligand, preferably bulky, and the reaction thereof in a dispersed phase (i.e. gas phase, fluidized bed or stirred bed or slurry phase) olefin polymerization. There are a number of factors which impact on reactor continuity in a dispersed phase polymerization. A decrease in catalyst productivity or activity is reflected by a decrease in ethylene uptake over time but may also result in a lower kinetic profile and potentially a lower potential for fouling.
BACKGROUND OF THE INVENTION
[0002] Single site catalysts for the polymerization of alpha olefins were introduced in the mid 1980's. These catalysts are more active than the prior Ziegler Natta catalysts, which may lead to issues of polymer agglomeration. Additionally, static may contribute to the problem. As a result reactor continuity (e.g. fouling and also catalyst life time) may be a problem.
[0003] The kinetic profile of many single site catalysts starts off with a very high activity over a relatively short period of time, typically about the first five minutes of the reaction, the profile then goes through an inflection point and decreases rapidly for about the next five minutes and thereafter there is period of relative slower decline in the kinetic profile. This may be measured by the ethylene uptake, typically in standard liters of ethylene per minute in the reactor.
[0004] U.S. Pat. No. 6,147,172 issued Nov. 14, 2000 to Brown et al. assigned to NOVA Chemicals International S.A. discloses a catalyst comprising a phosphinimine ligand and a boron heterocyclic ligand, typically bulky. The patent teaches the catalyst may be supported (Col. 21, part C) but does not suggest any treatment of the support as set out in the present disclosure.
[0005] Canadian Patent Application 2,716,772 filed Oct. 6, 2010 discloses a process to improve the dispersed phase reactor continuity of catalyst having a phosphinimine ligand by supporting the catalyst on a silica support treated with Zr(SO 4 ) 2-4 H 2 O. The support is also treated with MAO. This patent application fails to disclose or suggest the type of catalyst of the present disclosure.
[0006] U.S. Pat. No. 6,734,266 issued May 11, 2004 to Gao et al., assigned to NOVA Chemicals (International) S.A. teaches sulfating the surface of porous inorganic support with an acid, amide or simple salt such as an alkali or alkaline earth metal sulphate. The resulting treated support may be calcined. Aluminoxane and a single site catalyst are subsequently deposited on the support. The resulting catalyst shows improved activity. However, the patent fails to teach or suggest depositing zirconium sulphate on a metal oxide support.
[0007] U.S. Pat. No. 7,001,962 issued Feb. 21, 2006 to Gao et al., assigned to NOVA Chemicals (International) S.A. teaches treating a porous inorganic support with a zirconium compound including zirconium sulphate and an acid such as a fluorophosphoric acid, sulphonic acid, phosphoric acid and sulphuric acid. The support is dried and may be heated under air at 200° C. and under nitrogen up to 600° C. Subsequently, a trialkyl aluminum compound (e.g. triethyl aluminum) or an alkoxy aluminum alkyl compound (e.g. diethyl aluminum ethoxide) and a single site catalyst are deposited on the support. The specification teaches away from using aluminoxane compounds. The activity of these supports is typically lower than the activity of the catalyst of U.S. Pat. No. 6,734,266 (compare Table 5 of U.S. Pat. No. 7,001,962 with Table 2 of U.S. Pat. No. 6,734,266). The present invention eliminates the required acid reagent that reacts with the zirconium compound.
[0008] U.S. Pat. No. 7,273,912 issued Sep. 25, 2007 to Jacobsen et al., assigned to Innovene Europe Limited, teaches a catalyst which is supported on a porous inorganic support which has been treated with a sulphate such as ammonium sulphate or an iron, copper, zinc, nickel or cobalt sulphate. The support may be calcined in an inert atmosphere at 200 to 850° C. The support is then activated with an ionic activator and then contacted with a single site catalyst. The patent fails to teach aluminoxane compounds and zirconium sulphate.
[0009] U.S. Pat. No. 7,005,400 issued Feb. 28, 2006 to Takahashi assigned to Polychem Corporation teaches a combined activator support comprising a metal oxide support and a surface coating of a group 2, 3, 4, 13 and 14 oxide or hydroxide different from the carrier. The support is intended to activate the carrier without the conventional “activators”. However, in the examples the supported catalyst is used in combination with triethyl aluminum. The triethyl aluminum does not appear to be deposited on the support. Additionally, the patent does not teach phosphinimine catalysts.
[0010] U.S. Pat. No. 7,442,750 issued Oct. 28, 2008 to Jacobsen et al., assigned to Innovene Europe Limited teaches treating an inorganic metal oxide support typically with a transition metal salt, preferably a sulphate, of iron, copper, cobalt, nickel, and zinc. Then a single site catalyst, preferably a constrained geometry single site catalyst and an activator are deposited on the support. The activator is preferably a borate but may be an aluminoxane compound. The disclosure appears to be directed at reducing static in the reactor bed and product in the absence of a conventional antistatic agent such as STADIS®.
[0011] U.S. Pat. No. 6,653,416 issued Nov. 25, 2003 to McDaniel at al., assigned to Phillips Petroleum Company, discloses a fluoride silica—zirconia or titania porous support for a metallocene catalyst activated with an aluminum compound selected from the group consisting of alkyl aluminums, alkyl aluminum halides and alkyl aluminum alkoxides. Comparative examples 10 and 11 show the penetration of zirconium into silica to form a silica-zirconia support. However, the examples (Table 1) show the resulting catalyst has a lower activity than those when the supports were treated with fluoride.
[0012] None of the above art suggests treating the support with an antistatic agent.
[0013] The use of a salt of a carboxylic acids, especially aluminum stearate, as an antifouling additive to olefin polymerization catalyst compositions is disclosed in U.S. Pat. Nos. 6,271,325 (McConville et al., to Univation) and 6,281,306 (Oskam et al., to Univation).
[0014] The preparation of supported catalysts using an amine antistatic agent, such as the fatty amine sold under the trademark KEMANINE® AS-990, is disclosed in U.S. Pat. Nos. 6,140,432 (Agapiou et al.; to Exxon) and 6,117,955 (Agapiou et al.; to Exxon).
[0015] Antistatic agents are commonly added to aviation fuels to prevent the buildup of static charges when the fuels are pumped at high flow rates. The use of these antistatic agents in olefin polymerizations is also known. For example, an aviation fuel antistatic agent sold under the trademark STADIS composition (which contains a “polysulfone” copolymer, a polymeric polyamine and an oil soluble sulfonic acid) was originally disclosed for use as an antistatic agent in olefin polymerizations in U.S. Pat. No. 4,182,810 (Wilcox, to Phillips Petroleum). The examples of the Wilcox '810 patent illustrate the addition of the “polysulfone” antistatic agent to the isobutane diluent in a commercial slurry polymerization process. This is somewhat different from the teachings of the earlier referenced patents—in the sense that the carboxylic acid salts or amine antistatics of the other patents were added to the catalyst, instead of being added to a process stream.
[0016] The use of “polysulfone” antistatic composition in olefin polymerizations is also subsequently disclosed in:
[0017] 1) chromium catalyzed gas phase olefin polymerizations, in U.S. Pat. No. 6,639,028 (Heslop et al.; assigned to BP Chemicals Ltd.);
[0018] 2) Ziegler Natta catalyzed gas phase olefin polymerizations, in U.S. Pat. No. 6,646,074 (Herzog et al.; assigned to BP Chemicals Ltd.); and
[0019] 3) metallocene catalyzed olefin polymerizations, in U.S. Pat. No. 6,562,924 (Benazouzz et al.; assigned to BP Chemicals Ltd.).
[0020] The Benazouzz et al. patent does teach the addition of STADIS antistatic agent to the polymerization catalyst in small amounts (about 150 ppm by weight). However, in each of the Heslop et al. '028, Herzog et al. '074 and Benazouzz et al. '924 patents listed above, it is expressly taught that it is preferred to add the STADIS antistatic directly to the polymerization zone (i.e. as opposed to being an admixture with the catalyst).
[0021] None of the above art discusses the kinetic profile of the catalyst system. One of the difficulties with high activity (“hot”) catalyst is that they tend to have a very high initial reactivity (ethylene consumption) that goes through an inflection point and rapidly decreases over about the first 10 minutes of reaction and then decreases at a much lower rate over the next 50 minutes together with fluctuations in reactor temperature. It is desirable to have a high activity catalyst (e.g. more than about 1,300 grams of polymer per gram of supported catalyst normalized to 200 psig (1,379 kPa) ethylene partial pressure and 90° C. in the presence of 1-hexene comonomer) having a kinetic profile for a plot of ethylene consumption in standard liters of ethylene per minute against time in minutes, corrected for the volume of ethylene in the reactor prior to the commencement of the reaction, in a 2 liter reactor over a period of time from 0 to 60 minutes is such that the ratio of the maximum peak height over the first 10 minutes to the average ethylene consumption from 10 to 60 minutes taken at not less than 40, preferably greater than 60 most preferably from 120 to 300 data points, is less than 7, preferably less than 6, most preferably less than 5.5.
[0022] The present invention seeks to provide a catalyst having a kinetic profile as described above, optionally having reduced static and its use in the dispersed phase polymerization of olefins.
SUMMARY OF THE INVENTION
[0023] In one embodiment the present invention provides a catalyst system having an activity greater than 1,300 g of polymer per gram of supported catalyst per hour normalized to 1,379 kPag (200 psig) of ethylene partial pressure and a temperature of 90° C. in the presence of 1-hexene comonomer and a kinetic profile for a plot of ethylene consumption in standard liters of ethylene per minute against time in minutes, at a reaction pressure of 1,379 kPag (200 psig) and 90° C., corrected for the volume of ethylene in the reactor prior to the commencement of the reaction, in a 2 liter reactor over a period of time from 0 to 60 minutes is such that the ratio of the maximum peak height over the first 10 minutes to the average ethylene consumption from 10 to 60 minutes taken at not less than 40 data points, is less than 6, comprising:
[0024] (i) a porous inorganic oxide support having an average particle size from 10 to 150 microns, a surface area greater than 100 m 2 /g, and a pore volume greater than 0.3 ml/g impregnated with
[0025] (ii) at least a 1 weight % based on the weight of said inorganic oxide support of Zr(SO 4 ) 2-4 H 2 O;
[0026] (iii) from 10 to 60 weight % of an aluminum activator based on the weight of said inorganic oxide support of said activator having the formula:
[0000] R 12 2 AlO(R 12 AlO) q AlR 12 2
[0000] wherein each R 12 is independently selected from the group consisting of C 1-20 hydrocarbyl radicals and q is from 3 to 50; and
[0027] (iv) from 0.1 to 30 weight % of a catalyst of the formula:
[0000]
[0000] wherein M is a group 4 metal having an atomic weight less than 179; Pl is a phosphinimine ligand of the formula
[0000]
[0000] wherein each R 21 is independently selected from the group consisting of a hydrogen atom; a halogen atom; C 1-10 hydrocarbyl radicals which are unsubstituted by or further substituted by a halogen atom; H is a heteroligand characterized by (a) containing a heteroatom selected from N, S, B, O, P or Si, and (b) being bonded to M through a sigma or pi bond with the proviso that H is not a phosphinimine ligand as defined above or a ketamide ligand as defined below; L is an activatable ligand; n is 1, 2 or 3 depending upon the valence of M with the proviso that L is not a cyclopentadienyl, indenyl or fluorenyl ligand.
[0028] In a further embodiment the present invention provides the above catalyst further comprising from 50 to 250 ppm based on the weight of the supported catalyst of an antistatic comprising:
[0029] (i) from 3 to 48 parts by weight of one or more polysulfones comprising:
(a) 50 mole % of sulphur dioxide; (b) 40 to 50 mole % of a C 6-20 an alpha olefin; and (c) from 0 to 10 mole % of a compound of the formula ACH═CHB
[0033] where A is selected from the group consisting of a carboxyl radical and a C 1-15 carboxy alkyl radical and B is a hydrogen atom or a carboxyl radical provided if A and B are carboxyl radicals A and B may form an anhydride;
[0034] (ii) from 3 to 48 parts by weight of one or more polymeric polyamides of the formula:
[0000] R 20 N[(CH 2 CHOHCH 2 NR 21 ) a —(CH 2 CHOHCH 2 NR 21 —R 22 —NH) b —(CH 2 CHOHCH 2 NR 23 ) c H x ]H 2-x
[0000] wherein R 21 is an aliphatic hydrocarbyl group of 8 to 24 carbon atoms; R 22 is an alkylene group of 2 to 6 carbon atoms; R 23 is the group R 22 —HNR 21 ; R 20 is R 21 or an N-aliphatic hydrocarbyl alkylene group having the formula R 21 NHR 22 ; a, b and c are integers from 0 to 20 and x is 1 or 2; with the proviso that when R 20 is R 21 then a is greater than 2 and b=c=0, and when R 20 is R 21 NHR 22 then a is 0 and the sum of b+c is an integer from 2 to 20; and
[0035] (iii) from 3 to 48 parts by weight of C 10-20 alkyl or arylalkyl sulphonic acid.
[0036] In a further embodiment the present invention provides a process of making a catalyst system having an activity greater than 1,300 g of polymer per gram of supported catalyst per hour normalized to 1,379 kPag (200 psig) of ethylene partial pressure and a temperature of 90° C. in the presence of 1-hexene comonomer and a kinetic profile for a plot of ethylene consumption in standard liters of ethylene per minute against time in minutes, at a reaction pressure of 1,379 kPag (200 psig) and 90° C., corrected for the volume of ethylene in the reactor prior to the commencement of the reaction, in a 2 liter reactor over a period of time from 0 to 60 minutes is such that the ratio of the maximum peak height over the first 10 minutes to the average ethylene consumption from 10 to 60 minutes taken at not less than 40 data points, is less than 6.0, comprising:
[0037] (i) impregnating a porous inorganic support having an average particle size from 10 to 150 microns, a surface area greater than 100 m 2 /g, and a pore volume greater than 0.3 ml/g with
[0038] (ii) at least a 1 weight % aqueous solution of Zr(SO 4 ) 2-4 H 2 O, to provide not less than 1 weight % based on the weight of the support of said salt;
[0039] (iii) recovering the impregnated support;
[0040] (iv) calcining said impregnated support in one or more steps at a temperature from 300° C. to 600° C. for a time from 2 to 20 hours in an inert atmosphere;
[0041] (v) and either
(a) contacting said calcined support with a hydrocarbyl solution of an aluminum activator compound of the formula: R 12 2 AlO(R 12 AlO) q AlR 12 2 wherein each R 12 is independently selected from the group consisting of C 1-20 hydrocarbyl radicals and q is from 3 to 50 to provide from 10 to 60 weight % of said aluminum compound based on the weight of said calcined support; optionally, separating said activated support from said hydrocarbyl solution and contacting said activated support with a hydrocarbyl solution containing a single site catalyst as set out below to provide from 0.1 to 30 wt % of said single site catalyst; or (b) contacting said support with a hydrocarbyl solution containing an aluminum activator compound of the formula:
[0000] R 12 2 AlO(R 12 AlO) q AlR 12 2 wherein each R 12 is independently selected from the group consisting of C 1-20 hydrocarbyl radicals and q is from 3 to 50 and a catalyst of the formula:
[0000]
wherein M is a group 4 metal having an atomic weight less than 179; Pl is a phosphinimine ligand of the formula:
[0000]
wherein each R 21 is independently selected from the group consisting of a hydrogen atom; a halogen atom; C 1-10 hydrocarbyl radicals which are unsubstituted by or further substituted by a halogen atom; H is a heteroligand characterized by (a) containing a heteroatom selected from N, S, B, O or P; and (b) being bonded to M through a sigma or pi bond with the proviso that H is not a phosphinimine ligand as defined above or a ketamide ligand as defined below; L is an activatable ligand; n is 1, 2 or 3 depending upon the valence of M with the proviso that L is not a cyclopentadienyl, indenyl or fluorenyl ligand to provide from 10 to 60 weight % of said aluminum compound based on the weight of said calcined support and form 0.1 to 30 wt % of said singles site catalyst based on the weight of said support; and
[0044] (vi) recovering and drying the catalyst.
[0045] In a further embodiment the present invention provides the above process further comprising contacting said catalyst with from 15,000 to 120,000 ppm based on the weight of the supported catalyst of an antistatic comprising:
[0046] (i) from 3 to 48 parts by weight of one or more polysulfones comprising:
(a) 50 mole % of sulphur dioxide; (b) 40 to 50 mole % of a C 6-20 an alpha olefin; and (c) from 0 to 10 mole % of a compound of the formula ACH═CHB where A is selected from the group consisting of a carboxyl radical and a C 1-15 , carboxy alkyl radical; and B is a hydrogen atom or a carboxyl radical provided if A and B are carboxyl radicals A and B may form an anhydride;
[0050] (ii) from 3 to 48 parts by weight of one or more polymeric polyamides of the formula:
[0000] RN[(CH 2 CHOHCH 2 NR 1 ) a —(CH 2 CHOHCH 2 NR 1 —R 2 —NH) b —(CH 2 CHOHCH 2 NR 3 ) c H x ]H 2-x
[0000] wherein R 1 is an aliphatic hydrocarbyl group of 8 to 24 carbon atoms; R 2 is an alkylene group of 2 to 6 carbon atoms; R 3 is the group-R 2 —HNR 1 ; R is R 1 or an N-aliphatic hydrocarbyl alkylene group having the formula R 1 NHR 2 ; a, b and c are integers from 0 to 20 and x is 1 or 2; with the proviso that when R is R 1 then a is greater than 2 and b=c=0, and when R is R 1 NHR 2 then a is 0 and the sum of b+c is an integer from 2 to 20; and
[0051] (iii) from 3 to 48 parts by weight of C 10-20 alkyl or arylalkyl sulphonic acid and optionally from 0 to 150 parts by weight of a solvent or diluent.
[0052] In a further embodiment the present invention provides a dispersed phase olefin polymerization process having improved reactor continuity conducted in the presence of the above catalyst further comprising an antistatic agent.
[0053] In a further embodiment the present invention provides a disperse phase polymerization process comprising contacting one or more C 2-8 alpha olefins with a catalyst system which does not contain an antistatic agent, and feeding to the reactor from 10 to 80 ppm based on the weight of the polymer produced of an antistatic comprising:
[0054] (i) from 3 to 48 parts by weight of one or more polysulfones comprising:
(a) 50 mole % of sulphur dioxide; (b) 40 to 50 mole % of a C 6-20 an alpha olefin; and (c) from 0 to 10 mole % of a compound of the formula ACH═CHB where A is selected from the group consisting of a carboxyl radical and a C 1-15 carboxy alkyl radical and B is a hydrogen atom or a carboxyl radical provided if A and B are carboxyl radicals A and B may form an anhydride;
[0058] (ii) from 3 to 48 parts by weight of one or more polymeric polyamides of the formula:
[0000] R 20 N[(CH 2 CHOHCH 2 NR 21 ) a —(CH 2 CHOHCH 2 NR 21 —R 22 —NH) b —(CH 2 CHOHCH 2 NR 23 ) c H x ]H 2-x
[0000] wherein R 21 is an aliphatic hydrocarbyl group of 8 to 24 carbon atoms; R 22 is an alkylene group of 2 to 6 carbon atoms; R 23 is the group R 22 —HNR 21 ; R 20 is R 21 or an N-aliphatic hydrocarbyl alkylene group having the formula R 21 NHR 22 ; a, b and c are integers from 0 to 20 and x is 1 or 2; with the proviso that when R 20 is R 21 then a is greater than 2 and b=c=0, and when R 20 is R 21 NHR 22 then a is 0 and the sum of b+c is an integer from 2 to 20; and
[0059] (iii) from 3 to 48 parts by weight of C 10-20 alkyl or arylalkyl sulphonic acid.
BRIEF DESCRIPTION OF THE DRAWING
[0060] FIG. 1 is the kinetic profile of the catalysts run in example 1.
DETAILED DESCRIPTION
[0061] As used in this specification dispersed phase polymerization means a polymerization in which the polymer is dispersed in a fluid polymerization medium. The fluid may be liquid in which case the polymerization would be a slurry phase polymerization or the fluid could be gaseous in which case the polymerization would be a gas phase polymerization, either fluidized bed or stirred bed.
[0062] As used in this specification kinetic profile means a plot of ethylene consumption in standard liters of ethylene per minute against time in minutes, corrected for the volume of ethylene in the reactor prior to the commencement of the reaction, in a 2 liter reactor over a period of time from 0 to 60 minutes.
[0063] As used in this specification gram of supported catalyst means a gram of the catalyst system and activator on the support treated with Zr(SO 4 ) 2 .4H 2 O.
[0064] As used in this specification ketamide ligand means a ligand of the formula:
[0000]
[0000] wherein Sub 1 and Sub 2 are independently selected from the group consisting of C 1-20 hydrocarbyl radicals which are unsubstituted or may be substituted by up to 4 hetero atoms selected from the group consisting of N, O, and S or up to three C 1-9 straight chain, branched, cyclic or aromatic radicals which may be unsubstituted or substituted by a C 1-6 alkyl radical or Sub 1 and Sub 2 taken together may form a saturated or unsaturated ring which may be substituted by up to 4 hetero atoms selected from the group consisting of N, O, and S and which ring may be further substituted by up to three C 1-9 straight chain, branched, cyclic or aromatic radicals which may be unsubstituted or substituted by one or more C 1-6 alkyl radicals.
The Support
[0065] The support for the catalysts of the present invention is an inorganic oxide, preferably silica oxide, having a pendant reactive moiety. The reactive moiety may be a siloxyl radical but more typically is a hydroxyl radical. The support should have an average particle size from about 10 to 150 microns, preferably from about 20 to 100 microns. The support should have a large surface area typically greater than about 100 m 2 /g, preferably greater than about 250 m 2 /g, most preferably from 300 m 2 /g to 1,000 m 2 /g. The support will be porous and will have a pore volume from about 0.3 to 5.0 ml/g, typically from 0.5 to 3.0 ml/g.
[0066] Silica suitable for use as a support in the present invention is amorphous. For example, some commercially available silicas are marketed under the trademark of Sylopol® 958, 955 and 2408 by Davison Catalysts a Division of W. R. Grace and Company and ES70 and ES70W by PQ Corporation Silica.
Treatment of the Support
[0067] The support is treated with an aqueous solution of Zr(SO 4 ) 2 .4H 2 O. The support need not be dried or calcined as it is contacted with an aqueous solution.
[0068] Generally a 2 to 50, typically a 5 to 15, preferably an 8 to 12, most preferably a 9 to 11 weight % aqueous solution of Zr(SO 4 ) 2 .4H 2 O is used to treat the support. The support is contacted with the solution of Zr(SO 4 ) 2 .4H 2 O at a temperature from 10° C. to 50° C., preferably from 20 to 30° C., for a time of not less than 30 minutes, typically from 1 to 10 hours, preferably from 1 to 4 hours, until the support is thoroughly impregnated with the solution.
[0069] The impregnated support is then recovered typically by drying at an elevated temperature from 100° C. to 150° C., preferably from 120° C. to 140° C., most preferably from 130° C. to 140° C., for about 8 to 12 hours (e.g. overnight). Other recovery methods would be apparent to those skilled in the art.
[0070] The dried impregnated support is then calcined. It is important that the support be calcined prior to the initial reaction with an aluminum activator, catalyst or both. Generally, the support may be heated at a temperature of at least 200° C. for up to 24 hours, typically at a temperature from 500° C. to 675° C., preferably from 550° C. to 600° C. for about 2 to 20, preferably 4 to 10 hours. The resulting support will be free of adsorbed water and should have a surface hydroxyl content from about 0.1 to 5 mmol/g of support, preferably from 0.5 to 3 mmol/g of support.
[0071] The amount of the hydroxyl groups in a support may be determined according to the method disclosed by J. B. Peri and A. L. Hensley, Jr., in J. Phys. Chem., 72 (8), 2926, 1968, the entire contents of which are incorporated herein by reference.
[0072] The Zr(SO 4 ) 2 is substantially unchanged by calcining under the conditions noted above. At higher temperatures the Zr(SO 4 ) 2 starts to be converted to ZrO.
[0073] The resulting dried and calcined support is then contacted sequentially with the activator and the catalyst in an inert hydrocarbon diluent.
The Activator
[0074] The activator is an aluminoxane compound of the formula R 12 2 AlO(R 12 AlO) q AlR 12 2 wherein each R 12 is independently selected from the group consisting of C 1-20 hydrocarbyl radicals and q is from 3 to 50. In the aluminum activator preferably R 12 is a C 1-4 alkyl radical, preferably a methyl radical and q is from 10 to 40. Optionally, a hindered phenol may be used in conjunction with the aluminoxane to provide a molar ratio of Al:hindered phenol from 2:1 to 5:1 if the hindered phenol is present. Generally the molar ratio of Al:hindered phenol, if it is present, is from 3.25:1 to 4.50:1. Preferably the phenol is substituted in the 2, 4 and 6 position by a C 2-6 alkyl radical. Desirably the hindered phenol is 2,6-di-tert-butyl-4-ethyl-phenol.
[0075] The aluminum compounds (aluminoxanes and optionally hindered phenol) are typically used as activators in substantial molar excess compared to the total amount of metal in the catalysts (e.g. group 4 transition metal in the phosphinimine catalyst). Aluminum: total metal (in the catalyst) molar ratios may range from 10:1 to 10, 000:1, preferably 10:1 to 500:1, most preferably from 50:1 to 150:1, especially from 90:1 to 120:1.
[0076] Typically the loading of the aluminoxane compound may range from 10 up to 60 weight % preferably from 15 to 50 weight %, most preferably from 20 to 40 weight % based on the weight of the calcined support impregnated with metal salt.
[0077] The aluminoxane is added to the support in the form of a hydrocarbyl solution, typically at a 5 to 30 weight % solution, preferably an 8 to 12 weight % solution, most preferably a 9 to 10 weight % solution. Suitable hydrocarbon solvents include C 5-12 hydrocarbons which may be unsubstituted or substituted by C 1-4 alkyl group such as pentane, hexane, heptane, octane, cyclohexane, methylcyclohexane, toluene, or hydrogenated naphtha. An additional solvent is Isopar™ E (C 8-12 aliphatic solvent, Exxon Chemical Co.).
[0078] The treated support may optionally be filtered and/or dried under an inert atmosphere (e.g. N 2 ) and optionally at reduced pressure, preferably at temperatures from room temperature up to about 80° C.
[0079] The optionally dried support with activator is then contacted with the catalyst again in a hydrocarbyl solution of catalyst.
[0080] In an alternate embodiment the support could be treated with a combined solution of activator and catalyst. However care needs to be taken with this approach as prolonged contact (e.g. more than about 15 minutes) of the activator with the catalyst may result in degradation of one or both components.
The Catalyst
[0081] The catalytic component of the catalyst system is a catalyst comprising a phosphinimine ligand and a hetero ligand, preferably bulky, of the formula:
[0000]
[0000] wherein M is a group 4 metal having an atomic weight less than 179; Pl is a phosphinimine ligand of the formula:
[0000]
[0000] wherein each R 21 is independently selected from the group consisting of a hydrogen atom; a halogen atom; C 1-10 hydrocarbyl radicals which are unsubstituted by or further substituted by a halogen atom; H is a heteroligand characterized by (a) containing a heteroatom selected from N, S, B, O, P or Si; and (b) being bonded to M through a sigma or pi bond with the proviso that H is not a phosphinimine ligand as defined above or a ketamide ligand as defined above; L is an activatable ligand; n is 1, 2 or 3 depending upon the valence of M with the proviso that L is not a cyclopentadienyl, indenyl or fluorenyl ligand.
[0082] The preferred metals (M) are from Group 4 (especially titanium, hafnium or zirconium) with titanium being most preferred (e.g. with an atomic weight less than 179).
[0083] The phosphinimine ligand is defined by the formula:
[0000]
[0000] wherein each R 15 is independently selected from the group consisting of a C 1-8 , preferably C 1-6 hydrocarbyl radicals which are unsubstituted by or further substituted by a halogen atom. Most preferably the phosphinimine ligand is tris t-butyl phosphinimine.
[0084] In the catalyst preferably L is selected from the group consisting of a hydrogen atom; a halogen atom, a C 1-10 hydrocarbyl radical. Most preferably L is selected from the group consisting of a hydrogen atom, a chlorine atom and a C 1-4 alkyl radical.
[0085] H is a heteroligand containing a heteroatom selected from N, S, B, O, P or Si. Some such heteroligands include silicon containing heteroligands, amido ligands, alkoxy ligands, boron heterocyclic ligands and phosphole ligands. Preferred heteroligand are boron containing heteroligands.
Silicone-Containing Heteroligands
[0086] These ligands are defined by the formula:
[0000] —(μ)SiR x R y R z
[0000] where the—denotes a bond to the transition metal and μ is sulfur or oxygen.
[0087] The substituents on the Si atom, namely R x , R y and R z are required in order to satisfy the bonding orbital of the Si atom. The use of any particular substituent R x , R y or R z is not especially important to the success of this invention. It is preferred that each of R x , R y and R z is a C 1-4 hydrocarbyl group such as methyl, ethyl, isopropyl or tertiary butyl (simply because such materials are readily synthesized from commercially available materials).
Amido Ligands
[0088] The term “amido” is meant to convey its broad, conventional meaning. Thus, these ligands are characterized by (a) a metal-nitrogen bond, and (b) the presence of two substituents (which are typically simple alkyl or silyl groups) on the nitrogen atom.
Alkoxy Ligands
[0089] The term “alkoxy” is also intended to convey its conventional meaning. Thus these ligands are characterized by (a) a metal oxygen bond, and (b) the presence of a hydrocarbyl group bonded to the oxygen atom. The hydrocarbyl group may be a ring structure and/or substituted (e.g. 2, 6 di-tertiary butyl phenoxy).
Phosphole Ligands
[0090] The term “phosphole” is also meant to convey its conventional meaning. “Phosphole” is also meant to convey its conventional meaning. “Phospholes” are cyclic dienyl structures having four carbon atoms and one phosphorus atom in the closed ring. The simplest phosphole is C 4 PH 4 (which is analogous to cyclopentadiene with one carbon in the ring being replaced by phosphorus). The phosphole ligands may be substituted with, for example, C 1-20 hydrocarbyl radicals (which may, optionally, contain halogen substituents); phosphido radicals; amido radicals; silyl or alkoxy radicals.
Boron Heterocyclic Ligands
[0091] These ligands are characterized by the presence of a boron atom in a closed ring ligand. This definition includes heterocyclic ligands which also contain a nitrogen atom in the ring. These ligands are well known to those skilled in the art of olefin polymerization and are fully described in the literature (see, for example, U.S. Pat. Nos. 5,637,659; 5,554,775 and the references cited therein).
[0092] Preferred boron heterocyclic ligands have the formula:
[0000]
[0000] wherein R 18 is a C 1-4 alkyl radical.
[0093] The loading of the catalysts on the support should be such to provide from about 0.010 to 0.50, preferably from 0.015 to 0.40, most preferably from 0.015 to 0.036 mmol of metal M, preferably group 4 metal (e.g. Ti) from the catalysts per gram of support (support treated with Zr(SO 4 ) 2 .4H 2 O)) and calcined and treated with an activator
[0094] The catalyst may be added to the support in a hydrocarbyl solvent such as those noted above. The concentration of catalyst in the solvent is not critical. Typically, it may be present in the solution in an amount from about 5 to 15 weight %.
[0095] The supported catalyst (e.g. support, Zr(SO 4 ) 2 , activator and catalyst) typically has a reactivity in a dispersed phase reaction (e.g. gas or slurry phase) greater than 1,300 g of polymer per gram of support per hour normalized to an ethylene partial pressure of 200 psig (1,379 kPa) and a temperature of 90° C. in the presence of 1-hexene comonomer.
[0096] The supported catalyst of the present invention may be used in dispersed phase polymerizations in conjunction with a scavenger such as an aluminum alkyl of the formula Al(R 30 ) 3 wherein R 30 is selected from the group consisting of C 1-10 alkyl radicals, preferably C 2-4 alkyl radicals. The scavenger may be used in an amount to provide a molar ratio of Al:Ti from 20 to 2,000, preferably from 50 to 1,000, most preferably 100 to 500. Generally the scavenger is added to the reactor prior to the catalyst and in the absence of additional poisons, over time declines to 0.
[0097] The supported catalyst will have a kinetic profile for a plot of ethylene consumption in standard liters of ethylene per minute against time in minutes, corrected for the volume of ethylene in the reactor prior to the commencement of the reaction, in a 2 liter reactor over a period of time from 0 to 60 minutes is such that the ratio of the maximum peak height over the first 10 minutes to the average ethylene consumption from 10 to 60 minutes taken at not less than 40, preferably greater than 60, most preferably from 120 to 300 data points, is less than 7.0, preferably less than 6, most preferably 5.5.
[0098] The supported catalyst may be used in conjunction with an antistatic agent. In one embodiment the antistatic is added directly to the supported catalyst. The antistatic may be added in an amount from 0 (e.g. optionally) up to 150,000 parts per million (ppm), preferably from 15,000 up to 120,000 ppm based on the weight of the supported catalyst.
[0099] In a further embodiment the antistatic may be added to the reactor in an amount from 0 to 100, preferably from 10 to 80 ppm based on the weight of the polymer produced (i.e. the weight of polymer in the fluidized bed or the weight of polymer dispersed in the slurry phase reactor). If present the antistatic agent may be present in an amount from about 0 to 100, preferably from about 10 to 80 most preferably from 20 to 50 ppm based in the weight of polymer. From the productivity of the catalyst it is fairly routine to determine the feed rate of the antistatic to the reactor based on the catalyst feed rate.
Antistatic “Polysulfone” Additive
[0100] The antistatic polysulfone additive comprises at least one of the components selected from:
(1) a polysulfone copolymer; (2) a polymeric polyamine; and (3) an oil-soluble sulfonic acid, and, in addition, a solvent for the polysulfone copolymer.
[0104] Preferably, the antistatic additive comprises at least two components selected from above components (1), (2) and (3). More preferably, the antistatic additive comprises a mixture of (1), (2) and (3).
[0105] According to the present invention, the polysulfone copolymer component of the antistatic additive (often designated as olefin-sulfur dioxide copolymer, olefin polysulfones, or poly(olefin sulfone)) is a polymer, preferably a linear polymer, wherein the structure is considered to be that of alternating copolymers of the olefins and sulfur dioxide, having a one-to-one molar ratio of the comonomers with the olefins in head to tail arrangement. Preferably, the polysulfone copolymer consists essentially of about 50 mole percent of units of sulfur dioxide, about 40 to 50 mole percent of units derived from one or more 1-alkenes each having from about 6 to 24 carbon atoms, and from about 0 to 10 mole percent of units derived from an olefinic compound having the formula ACH═CHB where A is a group having the formula —(C x H 2x )—COOH wherein x is from 0 to about 17, and B is hydrogen or carboxyl, with the provision that when B is carboxyl, x is 0, and wherein A and B together can be a dicarboxylic anhydride group.
[0106] Preferably, the polysulfone copolymer employed in the present invention has a weight average molecular weight in the range 10,000 to 1,500,000, preferably in the range 50,000 to 900,000. The units derived from the one or more 1-alkenes are preferably derived from straight chain alkenes having 6-18 carbon atoms, for example 1-hexene, 1-heptene, 1-octene, 1-decene, 1-dodecene, 1-hexadecene and 1-octadecene. Examples of units derived from the one or more compounds having the formula ACH═CHB are units derived from maleic acid, acrylic acid, 5-hexenoic acid.
[0107] A preferred polysulfone copolymer is 1-decene polysulfone having an inherent viscosity (measured as a 0.5 weight percent solution in toluene at 30° C.) ranging from about 0.04 dl/g to 1.6 dl/g.
[0108] The polymeric polyamines that can be suitably employed in the antistatic of the present invention are described in U.S. Pat. No. 3,917,466, in particular at column 6 line 42 to column 9 line 29.
[0109] The polyamine component in accordance with the present invention has the general formula:
[0000] R 20 N[(CH 2 CHOHCH 2 NR 21 ) a —(CH 2 CHOHCH 2 NR 21 —R 22 —NH) b —(CH 2 CHOHCH 2 NR 23 ) c H x ]H 2-x
[0000] wherein R 21 is an aliphatic hydrocarbyl group of 8 to 24 carbon atoms; R 22 is an alkylene group of 2 to 6 carbon atoms; R 23 is the group R 22 —HNR 21 ; R 20 is R 21 or an N-aliphatic hydrocarbyl alkylene group having the formula R 21 NHR 22 ; a, b and c are integers from 0 to 20 and x is 1 or 2; with the proviso that when R 20 is R 21 then a is greater than 2 and b=c=0, and when R 20 is R 21 NHR 22 then a is 0 and the sum of b+c is an integer from 2 to 20.
[0110] The polymeric polyamine may be prepared for example by heating an aliphatic primary monoamine or N-aliphatic hydrocarbyl alkylene diamine with epichlorohydrin in the molar proportion of from 1:1 to 1:1.5 at a temperature of 50° C. to 100° C. in the presence of a solvent, (e.g. a mixture of xylene and isopropanol) adding a strong base, (e.g. sodium hydroxide) and continuing the heating at 50 to 100° C. for about 2 hours. The product containing the polymeric polyamine may then be separated by decanting and then flashing off the solvent.
[0111] The polymeric polyamine is preferably the product of reacting an N-aliphatic hydrocarbyl alkylene diamine or an aliphatic primary amine containing at least 8 carbon atoms and preferably at least 12 carbon atoms with epichlorohydrin. Examples of such aliphatic primary amines are those derived from tall oil, tallow, soy bean oil, coconut oil and cotton seed oil. The polymeric polyamine derived from the reaction of tallowamine with epichlorohydrin is preferred. A method of preparing such a polyamine is disclosed in U.S. Pat. No. 3,917,466, column 12, preparation B.1.0
[0112] The above-described reactions of epichlorohydrin with amines to form polymeric products are well known and find extensive use in epoxide resin technology.
[0113] A preferred polymeric polyamine is a 1:1.5 mole ratio reaction product of N-tallow-1,3-diaminopropane with epichlorohydrin. One such reaction product is “Polyflo™ 130” sold by Universal Oil Company.
[0114] According to the present invention, the oil-soluble sulfonic acid component of the antistatic is preferably any oil-soluble sulfonic acid such as an alkanesulfonic acid or an alkylarylsulfonic acid. A useful sulfonic acid is petroleum sulfonic acid resulting from treating oils with sulfuric acid.
[0115] Preferred oil-soluble sulfonic acids are dodecylbenzenesulfonic acid and dinonylnaphthylsulfonic acid.
[0116] The antistatic additive preferably comprises 1 to 25 weight % of the polysulfone copolymer, 1 to 25 weight % of the polymeric polyamine, 1 to 25 weight % of the oil-soluble sulfonic acid and 25 to 95 weight % of a solvent. Neglecting the solvent, the antistatic additive preferably comprises about 5 to 70 weight % polysulfone copolymer, 5 to 70 weight % polymeric polyamine and 5 to 70 weight % oil-soluble sulfonic acid and the total of these three components is preferably 100%.
[0117] Suitable solvents include aromatic, paraffin and cycloparaffin compounds. The solvents are preferably selected from among benzene, toluene, xylene, cyclohexane, fuel oil, isobutane, kerosene and mixtures thereof.
[0118] According to a preferred embodiment of the present invention, the total weight of components (1), (2), (3) and the solvent represents essentially 100% of the weight of the antistatic additive.
[0119] One useful composition, for example, consists of 13.3 weight % 1:1 copolymer of 1-decene and sulfur dioxide having an inherent viscosity of 0.05 determined as above, 13.3 weight % of “Polyflo™ 130” (1:1.5 mole ratio reaction product of N-tallow-1,3-diaminopropane with epichlorohydrin), 7.4 weight % of either dodecylbenzylsulfonic acid or dinonylnaphthylsulfonic acid, and 66 weight % of an aromatic solvent which is preferably toluene or kerosene.
[0120] Another useful composition, for example, consists of 2 to 7 weight % 1:1 copolymer of 1-decene and sulfur dioxide having an inherent viscosity of 0.05 determined as above, 2 to 7 weight % of “Palyflo™ 130” (1:1.5 mole ratio reaction product of N-tallow-1,3-diaminopropane with epichlorohydrin), 2 to 8 weight % of either dodecylbenzylsulfonic acid or dinonylnaphthylsulfonic acid, and 78 to 94 weight % of an aromatic solvent which is preferably a mixture of 10 to 20 weight % toluene and 62 to 77 weight % kerosene.
[0121] According to a preferred embodiment of the present invention, the antistatic is a material sold by Octel under the trade name STADIS™, preferably STADIS 450, more preferably STADIS 425.
Gas Phase Polymerization
[0122] Fluidized bed gas phase reactors to make polyethylene are generally operated at low temperatures from about 50° C. up to about 120° C. (provided the sticking temperature of the polymer is not exceeded) preferably from about 75° C. to about 110° C. and at pressures typically not exceeding 3,447 kPa (about 500 psi) preferably not greater than about 2,414 kPa (about 350 psi).
[0123] Gas phase polymerization of olefins is well known. Typically, in the gas phase polymerization of olefins (such as ethylene) a gaseous feed stream comprising of at least about 80 weight % ethylene and the balance one or more C 3-6 copolymerizable monomers typically, 1-butene, or 1-hexene or both, together with a ballast gas such as nitrogen, optionally a small amount of C 1-2 alkanes (i.e. methane and ethane) and further optionally a molecular weight control agent (typically hydrogen) is fed to a reactor and in some cases a condensable hydrocarbon (e.g. a C 4-6 alkane such as pentane). Typically, the feed stream passes through a distributor plate at the bottom of the reactor and vertically traverses a bed of polymer particles with active catalyst, typically a fluidized bed but the present invention also contemplates a stirred bed reactor. A small proportion of the olefin monomers in the feed stream react with the catalyst. The unreacted monomer and the other non-polymerizable components in the feed stream exit the bed and typically enter a disengagement zone where the velocity of the feed stream is reduced so that entrained polymer falls back into the fluidized bed. Typically the gaseous stream leaving the top of the reactor is then passed through a compressor. The compressed gas is then cooled by passage through a heat exchanger to remove the heat of reaction. The heat exchanger may be operated at temperatures below about 65° C., preferably at temperatures from 20° C. to 50° C. If there is a condensable gas it is usually condensed and entrained in the recycle stream to remove heat of reaction by vaporization as it recycles through the fluidized bed.
[0124] Polymer is removed from the reactor through a series of vessels in which monomer is separated from the off gases. The polymer is recovered and further processed. The off gases are fed to a monomer recovery unit. The monomer recovery unit may be selected from those known in the art including a distillation tower (i.e. a C 2 splitter), a pressure swing adsorption unit and a membrane separation device. Ethylene and hydrogen gas recovered from the monomer recovery unit are fed back to the reactor. Finally, make up feed stream is added to the reactor below the distributor plate.
Slurry Polymerization
[0125] Slurry processes are conducted in the presence of a hydrocarbon diluent such as an alkane (including isoalkanes), an aromatic or a cycloalkane. The diluent may also be the alpha olefin comonomer used in copolymerizations. Preferred alkane diluents include propane, butanes, (i.e. normal butane and/or isobutane), pentanes, hexanes, heptanes and octanes. The monomers may be soluble in (or miscible with) the diluent, but the polymer is not (under polymerization conditions). The polymerization temperature is preferably from about 5° C. to about 200° C., most preferably less than about 110° C. typically from about 10° C. to 80° C. The reaction temperature is selected so that the ethylene copolymer is produced in the form of solid particles. The reaction pressure is influenced by the choice of diluent and reaction temperature. For example, pressures may range from 15 to 45 atmospheres (about 220 to 660 psi or about 1,500 to about 4,600 kPa) when isobutane is used as diluent (see, for example, U.S. Pat. No. 4,325,849) to approximately twice that (i.e. from 30 to 90 atmospheres—about 440 to 1,300 psi or about 3,000-9,100 kPa) when propane is used (see U.S. Pat. No. 5,684,097). The pressure in a slurry process must be kept sufficiently high to keep at least part of the ethylene monomer in the liquid phase.
[0126] The reaction typically takes place in a jacketed closed loop reactor having an internal stirrer (e.g. an impeller) and at least one settling leg. Catalyst, monomers and diluents are fed to the reactor as liquids or suspensions. The slurry circulates through the reactor and the jacket is used to control the temperature of the reactor. Through a series of let down valves the slurry enters a settling leg and then is let down in pressure to flash the diluent and unreacted monomers and recover the polymer generally in a cyclone. The diluent and unreacted monomers are recovered and recycled back to the reactor.
[0127] The slurry reaction may also be conducted in a continuous stirred tank reactor.
The Polymer
[0128] The resulting polymer may have a density from about 0.910 g/cc to about 0.960 g/cc. The resulting polymers may be used in a number of applications such as blown and cast film, extrusion and both injection and rotomolding applications. Typically the polymer may be compounded with the usual additives including heat and light stabilizers such as hindered phenols; ultra violet light stabilizers such as hindered amine stabilizers (HALS); process aids such as fatty acids or their derivatives and fluoropolymers optionally in conjunction with low molecular weight esters of polyethylene glycol.
[0129] The present invention will now be illustrated by the following non limiting example.
Catalyst
[0130] The Borabenzene complex was prepared following the literature preparation found in Herberich, G. E.; Schmidt, B.; Englert, U. Organometallics, 1995, 14, 471-480. The titanium precursor complex was prepared using the preparation found in U.S. Pat. No. 6,147,172 issued Nov. 14, 2000 to Brown et al., assigned to NOVA Chemicals International S.A.
Complexation
[0131] The final catalyst molecule was prepared by adding an ethereal solution (20 mL) of the borabenzene salt (0.2 g, 2.1 mmol) to a solution of the titanium precursor (0.8 g, 2.1 mmol) dissolved in ether (25 mL) at −90° C. The resultant yellow solution was stirred overnight and gradually warm to room temperature. Ether was removed in vacuo and the product was extracted into dichloromethane (2×10 mL) and volatiles were removed again. The crude product was extracted into toluene (2×10 mL) and layered with heptane to crystallize a solid product which was isolated by filtration (0.6 g, 68%).
[0132] The aluminoxane was a 10% MAO solution in toluene supplied by Albemarle.
[0133] The support was silica SYLOPOL 2408 obtained from W.R. Grace.
[0000] Preparation of the Support (Apart from the Control)
[0134] A 10% aqueous solution of the Zr(SO 4 ).4H 2 O was prepared and impregnated into the support by incipient wetness impregnation procedure. The solid support was dried in air at about 135° C. to produce a free flowing powder. The resulting powder was subsequently dried in air at 200° C. for about 2 hours under air and then under nitrogen at 600° C. for 6 hours.
NAA Characterization
[0135] A sample of Zr(SO 4 ) 2 treated SYLOPOL 2408 prepared as above was determined to have a sulfur:zirconium ratio of 0.703 by NAA analysis; which is consistent with the ratio expected for pure Zr(SO 4 ) 2 .
XRD Analysis
[0136] A 1 gram sample of pure Zr(SO 4 ) 2 .4H 2 O was dehydrated in a muffle furnace at 600° C. for 6 hours and the solid was analyzed by XRD analysis, which showed 100% of the Zr(SO 4 ) 2 remained.
[0137] The above shows that zirconia is not formed by the calcination process of Zr(SO 4 ) 2 .4H 2 O at up to 600° C. under nitrogen.
[0138] To a slurry of calcined support in toluene was added a toluene solution of 10 weight % MAO (4.5 weight % Al, purchased from Albemarle) plus rinsings (3×5 mL). The resultant slurry was mixed using a shaker for 1 hour at ambient temperature. To this slurry of MAO-on-support was added a toluene solution of catalyst to give a molar ratio of Al:Ti of 120:1. After two hours of mixing at room temperature using a shaker, the slurry was filtered, yielding a colorless filtrate. The solid component was washed with toluene and pentane (2×), then separated ˜400 mTorr and sealed under nitrogen until use.
[0139] For the comparative example the same procedure was used except that the support was not treated with Zr(SO 4 ).4H 2 O.
Polymerization
[0140] A 2 L reactor fitted with a stirrer (˜675 rpm) containing a NaCl seed bed (160 g) (stored for at least 3 days at 130° C.) was conditioned for 30 minutes at 105° C. An injection tube loaded in the glovebox containing the catalyst formulation was inserted into the reactor system, which was then purged 3 times with nitrogen and once with ethylene at 200 psi. Pressure and temperature were reduced in the reactor (below 2 psi and between 60 and 85° C.) and TIBAL (500:1 Al:Ti) was injected via gastight syringe followed by a 2 mL precharge of 1-hexene. After the reactor reached 85° C. the catalyst was injected via ethylene pressure and the reactor was pressurized to 200 psi total pressure with 1-hexene fed with a syringe pump at a mole ratio of 6.5% C 6 /C 2 started 1 minute after catalyst injection. The temperature of reaction was controlled at 90° C. for a total runtime of 60 minutes. Reaction was halted by stopping the ethylene flow and turning on reactor cooling water. The reactor was vented slowly to minimize loss of contents and the polymer/salt mixture was removed and allowed to air dry before being weighed.
[0141] Fouling was measured by collecting the polymer from the reactor (including lumps and sheeted material) and sieving through a number 14 sieve (1.4 mm openings) the product (lightly brushing but not “pushing” product through) to determine what percent of the polymer did not pass through the sieve as a percent of the total polymer produced. The results of the experiments are set forth in Table 1 below.
[0000]
TABLE 1
Time
AL:Ti
Productivity
Max
to
Rate of
Max height 1-10/
Molar
gPE/g
C 2
Max
Rise
Average C 2
Support
ratio
catalyst
Flow
Flow
scLM/min
concentration
Fouling %
Catalyst
120:1
1333
2.75
1.50
1.83
5.47
58.9
Zr(SO 4 ) 2 /2408.
Catalyst
120:1
1500
3.82
1.94
1.96
7.47
66.7
2408
[0142] FIG. 1 is a kinetic profile of the catalyst on silica and modified silica. As noted above the catalyst is extremely “hot” and both catalysts have a very significant initial rate of reaction. However, after about a minute it is clear the modified catalyst has a lower and more consistent rate of reaction.
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A supported catalyst system comprising a phosphinimine ligand containing catalyst on a porous inorganic support treated with a metal salt has improved reactor continuity in a dispersed phase reaction in terms of initial activation and subsequent deactivation. The resulting catalyst has a lower consumption of ethylene during initiation and a lower rate of deactivation. Preferably the catalyst is used with an antistatic agent.
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RELATED APPLICATIONS
[0001] This application is a continuation of co-pending application Ser. No. 10/468,331 filed 27 Jan. 2004.
BACKGROUND OF THE INVENTION
[0002] This invention relates to the medical use of compounds, and to methods of identifying further useful compounds, particularly in the treatment of diabetes, obesity, hyperlipidaemia, hypercholesterolaemia, atherosclerosis, cancer and inflammation, or other conditions where alterations in lipid or eicosanoid status may be desirable.
SUMMARY OF INVENTION
[0003] Perfluorooctanoic acid (PFOA) and other perfluorinated fatty acids or fluoroalkyl molecules are synthetic molecules used in industrial applications, principally as surfactants. The effects of these compounds on laboratory animals and cells has been studied, as have the effects of occupational exposure in humans (see, for example, Gilliland & Mandel (1993) J Occup Med 35(9), 950-954; Kees et al (1992) J Med Chem 35, 944-953). U.S. Pat. No. 4,624,851 suggests treatment of symptoms of cancer using fluorine containing acids; no experimental data is presented.
[0004] We have surprisingly found that such compounds may have beneficial effects. We have found that such compounds may be useful in treatment of diabetes, obesity, hyperlipidaemia, hypercholesterolaemia, atherosclerosis, cancer and inflammation, or other conditions where alterations in lipid or eicosanoid status may be desirable.
[0005] A first aspect of the invention provides a method of treatment of a patient in need of modulation (preferably reduction) of body mass or modulation (preferably prevention or reduction) of increase in body mass, and/or in need of modulation (preferably reduction) of plasma insulin, plasma glucose, plasma triglycerides and/or plasma cholesterol, comprising administering to the patient an effective amount of a compound of formula I as defined herein.
[0006] The compound of formula I is
[0000] Z 1 —X—Z 2
[0007] wherein
[0008] Z 1 represents —C0 2 H or a derivative thereof;
Z 2 represents F, H, —C0 2 H or a derivative thereof; and
[0010] X represents fluorinated alkylene;
or a solvate thereof;
which compounds are referred to hereinafter as “the compounds of the invention”.
[0012] A further aspect of the invention provides a method of treatment of a patient in need of an antitumour agent or an antiinflammatory agent, or in need of modulation in lipid or eicosanoid status, comprising administering to the patient an effective amount of a compound of formula I as defined herein. A compound of formula I is considered to be effective as an antitumour agent or an antiinflammatory agent or in modulating lipid or eicosanoid status (i.e. type and concentration of lipid or eicosanoid, either systemically or in a particular locus or tissue).
[0013] The patient may be a patient with or at risk of excessive inflammation, for example with or at risk of arthritis, or a patient with or at risk of developing a tumour. The compound may reduce the development, growth or metastasis of a tumour.
[0014] The compound may be useful in treating any condition or disorder in which the patient has or is at risk of excessive inflammation. The patient may have an allergic or autoimmune disease. The patient may have, for example, psoriasis, inflammatory bowel disease, asthma or rheumatism.
[0015] A further aspect of the invention provides a method of treatment of a patient who is overweight or obese and/or has diabetes, hyperlipidaemia, atherosclerosis, coronary heart disease, stroke, obstructive sleep apnoea, arthritis (for example osteoarthritis) and/or reduced fertility, or is at risk of developing such a condition, comprising administering to the patient an effective amount of a compound of formula I as defined herein.
[0016] A further aspect of the invention provides a method of treatment of a patient in need of modulation of PPAR (for example PPARα, δ or γ) activity, comprising administering to the patient an effective amount of a compound of formula I as defined herein. The compound may be a PPAR agonist or a PP AR antagonist; it may be an agonist for one PPAR and an antagonist for a different PPAR. Preferably the patient is in need of an increase in PPARα or PPARγ activity and the compound is a PPARα or PPARγ agonist. Alternatively, the patient may be in need of a decrease in PPARα or PPARγ activity and the compound may be a PPARα or PPARγ antagonist. In a further alternative, the patient may be in need of an increase in PPARδ activity and the compound is a PPARδ agonist. In a still further alternative, the patient may be in need of a decrease in PPARδ activity and the compound may be a PPARδ antagonist. PPARδ may have opposing effects to PPARα or PPARγ (see, for example, WO01/07066).
[0017] A further aspect of the invention provides a method of treatment of a patient in need of modulation of lipid or eicosanoid status or function, for example in need of modulation of the activity of a lipid metabolising or binding entity (including a lipid metabolising enzyme and a lipid binding polypeptide, for example a lipid transporting polypeptide), for example cycloxygenase (for example cycloxygenase I or cycloxygenase II) activity or phospholipase A (for example phospholipase A2) or lipoxygenase, comprising administering to the patient an effective amount of a compound of formula I as defined herein. Preferably the patient is in need of a decrease in a lipid metabolising or binding activity, for example cycloxygenase (for example cycloxygenase I or cycloxygenase II) activity or phospholipase A or lipoxygenase and the compound is an inhibitor of such activity. For example, inappropriate lipoxygenase activity may be involved in inflammation, hypersensitivity, asthma and some vascular diseases; thus a decrease in a lipoxygenase activity may be useful in such a condition.
[0018] Alternatively, the patient may be in need of an increase in such activity and the compound may be an activator of such activity.
[0019] Further preferences in relation to the patient and compound are indicated below.
[0020] Compounds of formula I may exhibit tautomerism. All tautomeric forms and mixtures thereof are included within the scope of the invention.
[0021] Compounds of formula I may also contain one or more asymmetric carbon atoms and may therefore exhibit optical and/or diastereoisomerism. Diastereoisomers may be separatedusing conventional techniques, e.g. chromatography or fractional crystallisation. The various stereoisomers may be isolated by separation of a racemic or other mixture of the compounds using conventional, e.g. fractional crystallisation or HPLC, techniques. Alternatively the desired optical isomers may be made by reaction of the appropriate optically active starting materials under conditions which will not cause racemisation or epimerisation, or by derivatisation, for example with a homochiral acid followed by separation of the diastereomeric esters by conventional means (e.g. HPLC, chromatography over silica). All stereoisomers are included within the scope of the invention.
[0022] When referred to herein, derivatives of —C0 2 H groups include groups which are commonly derived from a carboxylic acid and/or groups that contain a central carbon atom (i.e. the carbon atom that is attached to X) that is at the same oxidation state as —C(O)OH. Derivatives of —C0 2 H groups therefore includes groups such as:
[0000] (i) esters, e.g. those formed with an alcohol of formula R 1 0H, wherein R 1 represents aryl or alkyl;
(ii) thioesters, e.g. those formed with a thiol of formula R 1 SH, wherein R 1 is as herein before defined; and
(iii) salts, e.g. those formed with a nitrogen-containing base such as ammonia, an alkylamine, a dialkylamine, a trialkylamine and pyridine or alkali or alkaline earth metal salts (e.g. Na, K, Cs, Mg or Ca salts).
Preferred derivatives of —CO 2 H groups include those that are pharmaceutically acceptable.
[0023] Where the term fluorine is used herein, it is intended (where appropriate) that reference to other halogens, for example chlorine or bromine or more than one halogen, is included. However, it is strongly preferred that the halogen is fluorine.
[0024] It is preferred that the compound of Formula I comprises at least two fluorine atoms, preferably at least three, four, five, six, seven or eight fluorine atoms.
[0025] The term “aryl”, when used herein, includes C 6-10 aryl groups such as phenyl, naphthyl and the like. Aryl groups may be substituted by one or more substituents including —OH, cyano, halo, nitro, amino, alkyl and alkoxy. When substituted, aryl groups are preferably substituted by between one and three substituents.
[0026] The term alkyl, when used herein, refers to alkyl groups of 1 to 16, preferably 1 to 10 (e.g. 1 to 6) carbon atoms.
[0027] The term alkoxy, when used herein, refers to alkoxy groups of 1 to 16, preferably 1 to 10 (e.g. 1 to 6) carbon atoms.
[0028] Alkyl and alkoxy groups as defined herein may be straight-chain or, when there is a sufficient number (i.e. a minimum of three) of carbon atoms, be branched-chain and/or cyclic and/or heterocyclic. Further, when there is a sufficient number (i.e. a minimum of four) of carbon atoms, such alkyl and alkoxy groups may also be part cyclic/acyclic. Such alkyl and alkoxy groups may also be saturated or, when there is a sufficient number (i.e. a minimum of two) of carbon atoms, be unsaturated and/or interrupted by one or more oxygen and/or sulfur atoms. Alkyl and alkoxy groups may also be substituted by one or more halo, and especially fluoro, atoms.
[0029] The term “halo”, when used herein, includes fluoro, chloro, bromo and iodo.
[0030] The terms alkylamine, dialkylamine and trialkylamine, when used herein, refer to amines bearing one, two or three alkyl groups as defined herein, respectively.
[0031] The term alkylene, when used herein, refers to alkylene groups of 1 to 20, preferably 2 to 17 (e.g. 6 to 12) carbon atoms. Alkylene groups may be straight-chain or, when there is a sufficient number (i.e. a minimum of two or three, as appropriate) of carbon atoms, be branched-chain and/or cyclic and/or heterocyclic. Further, when there is a sufficient number (i.e. a minimum of four) of carbon atoms, such alkylene groups may also be part cyclic/acyclic. Such alkylene chains may also be saturated or, when there is a sufficient number (i.e. a minimum of two) of carbon atoms, be unsaturated and/or interrupted by one or more oxygen and/or sulfur atoms.
[0032] Preferred compounds of formula I include those in which:
[0033] alkylene group X is at least 50% fluorinated;
[0034] alkylene group X contains between 2 and 17 carbon atoms;
[0035] Z 1 represents —CO 2 H, an ammonium, (C 1-10 alkyl)ammonium, di-(C 1-10 alkyl)ammonium or tri-(C 1-10 alkyl) ammonium salt of —CO 2 H, or —CO 2 R 1 ;
[0036] Z 2 represents F, H, —CO 2 H or —CO 2 R 1 ;
[0037] R 1 represents C 1-6 alkyl.
[0038] More preferred compounds of formula I include those in which:
[0039] alkylene group X is at least 75% fluorinated;
[0040] alkylene group X is straight-chain, saturated and contains between 4 and 14 carbon atoms;
[0041] Z 1 represents —CO 2 H, an ammonium, (C 1-6 alkyl)ammonium, di-(C 1-6 alkyl) ammonium or
[0042] tri-(C 1-6 alkyl)ammonium salt of —CO 2 H, or —CO 2 R1;
[0043] Z 2 represents F, —CO 2 H or —CO 2 R 1 ;
[0044] R 1 represents straight-chain, unsubstituted, saturated C 1-4 alkyl.
[0045] Even more preferred compounds of formula I include those in which:
[0046] alkylene group X is at least 90% fluorinated;
[0047] alkylene group X is straight-chain, saturated and contains between 6 and 12 carbon atoms;
[0048] Z 1 represents —CO 2 H, an ammonium salt of —CO 2 H, or —CO 2 R 1 ;
[0049] R 1 represents straight-chain, unsubstituted, saturated C 1-2 alkyl.
[0050] Particularly preferred compounds of formula I may be or comprise a member of the following group:
[0051] Perfluoroheptanoic acid; perfluorooctanoic acid; perfluorononanoic acid; perfluorodecanoic acid; perfluoroundecanoic acid; perfluorododecanoic acid; perfluorotetradecanoic acid; perfluorohexadecanoic acid; perfluorooctadecanoic acid; perfluorosuccinic acid; perfluoroglutaric acid; perfluoroadipic acid; perfluorosuberic acid; perfluoroazelaic acid; perfluorosebacic acid; perfluoro-1,10-decanedicarboxylic acid;
[0052] methyl perfluoroheptanoate; methyl perfluorooctanoate; methyl perfluorononanoate; methyl perfluorodecanoate; methyl perfluoroundecanoate; methyl perfluorododecanoate; methyl perfluorotridecanoate; methyl perfluorotetradecanoate; methyl perfluoropentadecanoate; methyl
[0053] perfluorohexadecanoate; methyl perfluoroocta-decanoate; dimethyl perfluorosuccinate; dimethyl perfluoroglutarate; dimethyl perfluoroadipate; dimethyl perfluorosuberate; dimethyl perfluoroazelate;
[0054] dimethyl perfluorosebacate; perfluoro-1,10-decanedicarboxylic acid, dimethyl ester; and dimethyl perfluorododecanedioate.
[0055] These compounds may be obtained from any suitable supplier, for example 3M, DuPont, Miteni or Dyneon.
[0056] Examples of fluoroalkyl carbonyl compounds that may be useful include alpha-branched fluoroalkylcarbonyl fluorides and derivatives thereof, as described in U.S. Pat. No. 6,013,795 or U.S. Pat. No. 6,015,838 (both incorporated herein by reference) and references given therein, for example U.S. Pat. No. 2,567,011 (incorporated herein by reference). Methods of preparing same are also described. These compounds may also be useful in the synthesis of further compounds of the invention.
[0057] It is preferred that the compound is not a compound as discussed in U.S. Pat. No. 6,028,109, which are indicated to be PPAR agonists. Thus, it is preferred that the compound is not a compound represented by formula (I) of U.S. Pat. No. 6,028,109 (shown in FIG. 8 ).
[0058] Particularly preferred compounds of formula I include fluorinated fatty acids, such as perfluorinated fatty acids, for example perfluorooctanoic acid (PFOA) or a derivative or pharmaceutically acceptable salt or ester thereof (e.g. ammonium perfluorooctanoate (APFO)) The chemical formula for APFO is CF 3 (CF 2 ) 6 COO − NH 4 + (octanoic acid, pentadecafluoro-, ammonium salt; C-8, FC-143; CAS Registry No 3825-26-1). It may be obtained from DuPont (DuPont Chemical Solutions Enterprise, DuPont-Strassel, D-61343 Bad Homburg, Germany). Common contaminants of APFO include ammonium perfluoroheptanoate (CAS 6130-43-ammonium perfluorohexanoate (CAS 68259-11-0), ammonium perfluoropentanoate (CAS 21615-47-4), and branched chain homologs that are generically known as ammonium perfluoroisooctanoate, ammonium perfluoroisoheptanoate, ammonium perfluoroisohexanoate and ammonium perfluoroisopentanoate. Whilst it is considered that the effects observed in Example 1 using an APFO preparation arise from the administration of APFO itself, it will be appreciated that one or more contaminants, for example one or more of the possible contaminants listed above, may contribute to the effects observed.
[0059] It is preferred that the compound is not PFOS (perfluorooctylsulphonate) or perfluorodecanoic acid or a derivative or salt or ester thereof; these compounds may have toxic or environmentally undesirable effects.
[0060] It is preferred that the compound of formula I (or identified or identifiable by a screening method of the invention, as discussed below) is metabolically stable; for example it is preferred that the compound has a similar rate of metabolism to perfluorooctanoic acid. The compound may be considered to be a lipid mimetic which may be metabolically stable.
[0061] A further aspect of the invention provides the use of a compound of formula I as defined herein in the manufacture of a medicament for the treatment of a patient in need of modulation (preferably reduction) of body mass or modulation (preferably prevention or reduction) of increase in body mass, and/or in need of modulation (preferably reduction) of plasma insulin, plasma glucose, plasma triglycerides, leptin and/or plasma cholesterol. The patient may (for example in relation to a decrease in the above-listed parameters) be overweight or obese and/or have diabetes, hyperlipidaemia and/or atherosclerosis, or be at risk of developing such a condition. The risk may arise from genetic factors, age, or environmental factors, such as diet.
[0062] The patient may have other condition(s) associated with obesity, for example coronary heart disease, stroke, obstructive sleep apnoea, arthritis (for example osteoarthritis) or reduced fertility.
[0063] Accordingly, a further aspect of the invention provides the use of a compound of formula I as defined herein in the manufacture of a medicament for the treatment of a patient who is overweight or obese and/or has diabetes, hyperlipidaemia, atherosclerosis, coronary heart disease, stroke, obstructive sleep apnoea, arthritis (for example osteoarthritis) and/or reduced fertility, or is at risk of developing such a condition.
[0064] A further aspect of the invention provides the use of a compound of formula I in the manufacture of a medicament for the treatment of a patient in need an antitumour agent or an antiinflammatory agent or of modulation of lipid or eicosanoid status. Preferences in relation to such a patient are noted above.
[0065] As is well known to those skilled in the art, obesity may be described as a state of excessive accumulation of body fat. Obesity may be determined by determining the body mass index (BMI) for a patient, and/or by measuring subcutaneous fat deposits in the arm using a “pinch test”. The BMI is defined as weight (in kilograms) divided by the square of the height in metres. A BMI of 25-30 is considered as overweight and more than 30 as obese. Preferably, treatment leads to lowering of the BMI to less than about 29 to 31, or to a point at which health risks from being overweight are no longer significant.
[0066] It will be appreciated that the treatment of the invention may be used in combination with other treatments for the relevant condition. For example in relation to obesity, the patient may follow a calorie-restricted diet and/or follow a program of physical exercise.
[0067] The medicament may compose more than one (e.g. two) compounds of formula I (such as perfluorinated fatty acids or their derivatives). The medicament may comprise a prodrug, for example a molecule which is converted to a molecule with the required biological activity following administration of the medicament to the patient.
[0068] Compounds of formula I may be particularly useful in the treatment of patients with diabetes. For example, the compound may be useful in treating type II diabetes.
[0069] In type I diabetes, the compounds may be useful as an insulin sensitiser and may therefore allow the dose of insulin administered to be reduced, thereby lowering costs and potentially reducing side effects of insulin administration. Existing anti-diabetic agents, for example the thiazolidinedione class of agents, may have the undesirable effect of stimulating weight gain.
[0070] Compounds of formula I, such as perfluoroalkyl carboxylic acid compounds and their derivatives (e.g. PFOA or APFO or derivatives thereof), are considered to have the desirable effect of preventing weight gain as well as being useful as anti-diabetic agents.
[0071] Compounds of the invention may be useful in the concomitant treatment of a number of abnormalities, for example diabetes, obesity and hyperlipidaemia. Thus, it may be possible to treat a patient with these conditions (which may often occur together) with a single compound or preparation. This may have benefits, for example in relation to patient compliance, the avoidance of drug interactions, ease of formulation and marketing.
[0072] It is preferred that the patient is mammalian, most preferably human or, less preferably a domesticated animal, for example an animal kept as a pet or in agriculture, for example horse, cow, cat or dog.
[0073] It is preferred that the compound is a compound wherein the plasma insulin levels are modulated (preferably reduced) in a mammal following administration of the compound to the mammal, relative to either preadministration levels or a control mammal which has not been administered the compound. It is particularly preferred that plasma insulin levels are modulated (for example reduced) (for example relative to a control animal) in a male Fischer 344 rat following administration of the compound to the rat, as described in Example 1. It is sufficient for a reduction to be found at any time following first administration of the compound to the mammal (preferably rat), but it is preferred that such reduction is found (i.e. appears or is still present) at least seven days after first administration of the compound. It is preferred that a reduction of insulin levels of at least 1, 2, 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75 or 80% is achieved.
[0074] It will be appreciated that the comparative measurements are made on animals at substantially the same stage of feeding, i.e. at substantially the same time of day or at substantially the same time following ingestion of food.
[0075] When the mammal is a rat, it is preferred that plasma insulin levels are modulated (preferably reduced) following administration of the compound at a level of between 30 and 5000 or 3000 ppm of the diet, preferably between about 50 and 500 ppm, still more preferably about 300 ppm. It is preferred that the test is conducted using the methods and conditions described in Example 1. It is preferred that the change in insulin level is not accompanied by any adverse clinical symptoms or change in behaviour/activity of the mammal. Thus, the animals may be observed in relation to standard clinical chemistry analyses, blood pressure and/or dizziness. Thus, it is preferred that insulin levels are modulated (preferably reduced) following administration of an amount of the compound that does not produce a significant adverse effect on the animal.
[0076] Tests may be performed on more than one animal for a compound or given dose of a compound, as known to those skilled in the art.
[0077] Alternatively or in addition, it is preferred that plasma cholesterol, glucose and/or trigylceride levels are modulated (preferably reduced), and/or leptin levels modulated, in a mammal following administration of the compound to the mammal, relative to either preadministration levels or a control mammal which has not been administered the compound. Preferences indicated above in relation to modulation (for example reduction) of insulin levels apply similarly in relation to modulation (for example reduction) of plasma cholesterol, glucose and trigylceride levels, and to modulation of leptin levels, Alternatively or in addition, eicosanoid status (i.e. type or concentration) may be modulated (preferably reduced) in a mammal (or in a particular locus or tissue) following administration of the compound to the mammal, relative to either preadministration levels or a control mammal which has not been administered the compound.
[0078] Alternatively or in addition, it is preferred that bodyweight or bodyweight gain is modulated (preferably reduced) in a mammal following administration of the compound to the mammal, relative to either preadministration levels (for bodyweight) or a control mammal (for bodyweight or bodyweight gain) which has not been administered the compound. Preferences indicated above in relation to modulation (for example reduction) of insulin levels apply similarly in relation to modulation (for example reductions) m bodyweight or bodyweight gain.
[0079] Food consumption (expressed as weight of food consumed per unit bodyweight) may be increased following administration of the compound to the mammal, relative to either pre administration levels or a control mammal which has not been administered the compound. The increase may not be seen immediately after commencing administration of the compound; an initial decrease may be seen, which may be followed by an increase.
[0080] Whilst not wishing to be bound by theory, it is considered that a compound of the invention, for example a perfluorinated fatty acid, for example APFO or PFOA, may bind to a peroxisome proliferator activated receptor (PPAR), for example PPARα, PPARδ or PPARγ (Kliewer et al (1994) PNAS, 91, 7355-7359; reviewed in Gelman et al (1999) Cell Mol Life Sci 55, 932-943; Kersten et al (2000) Nature 405, 421-424 and Issemann & Green (1990) Nature 347, 645-650) and may be a PPAR agonist or antagonist. It is preferred that the compound binds to a peroxisome proliferator activated receptor (PPAR), for example PPARα, PPARδ or PPARγ. It is further preferred that the compound is a PPARα, PPARδ or PPARγ modulator, for example a PPARα, PPARδ or PPARγ agonist or antagonist. It is particularly preferred that the compound is a PPARα or PPARγ agonist or a PPARδ antagonist. Any suitable method may be used for determining whether a compound binds to and/or is a modulator, for example an agonist or antagonist of a PPAR.
[0081] Also whilst not wishing to be bound by theory, a compound of the invention, for example a perfluorinated fatty acid, for example APFO or PFOA, may bind to a lipid metabolising or binding entity, for example a cycloxygenase, for example COXI or COXII, or phospholipase A, for example Phospholipase A2, or lipoxygenase and may be a modulator, for example an activator or inhibitor, of such an entity's activity (including degree of activation). It is preferred that the compound binds to a lipid metabolising enzyme, for example a cycloxygenase, for example COXI or COXII. It is further preferred that the compound is a modulator of the activity of a lipid metabolising enzyme, for example a cycloxygenase, for example COXI or COXII. Any suitable method may be used for determining whether a compound binds to and/or is a modulator, for example an activator or inhibitor of a lipid binding or metabolising entity.
[0082] A further aspect of the invention provides the use of a compound of formula I as defined herein in the manufacture of a medicament for treating a patient in need of modulation of PPAR (for example PPARα, PPARδ (also known as β) or PPARγ) activity. Preferably the patient is in need of an increase in PPAR (preferably PPARα and/or PPARγ) activity and the compound of formula I as defined herein is a PPAR (for example a PPARα or γ) agonist. Alternatively, the patient is in need of a decrease in PPAR (preferably PPARδ) activity and the compound of formula I as defined herein is a PPAR (for example a PPARδ) antagonist.
[0083] A further aspect of the invention provides the use of a compound of formula I as defined herein in the manufacture of a medicament for treating a patient in need of modulation of a lipid metabolising entity activity, for example cycloxygenase (for example cyclooxygenase I or cyclooxygenase II) activity or phospholipase A (for example phospholipase A2) activity or lipoxygenase activity.
[0084] A further aspect of the invention provides a screening method for identifying a drug-like compound or lead compound for the development of a drug-like compound in which (1) a mammal is exposed to a compound of formula I as defined herein (for example a perfluorinated fatty acid) or derivative thereof (2) the plasma insulin, glucose, cholesterol, triglyceride and/or leptin level of the mammal is measured, and/or bodyweight of the mammal is measured, and/or lipid or eicosanoid status (i.e. type and level of at least one lipid or eicosanoid) or function (for example assessed by degree of responsiveness to the mammal to a lipid or eicosanoid) of the mammal is measured.
[0085] The method preferably comprises the step of selecting a compound on exposure to which the plasma insulin, glucose, cholesterol, and/or triglyceride level of the mammal is changed, preferably reduced, and/or leptin level of the mammal is modulated, and/or bodyweight or bodyweight increase is changed, preferably reduced. Preferences for this aspect of the invention include those indicated above in relation to investigating effects on insulin, cholesterol, glucose, triglyceride or leptin levels, or on bodyweight. For example, it is preferred that the mammal is a rodent, for example a rat or a mouse, or other laboratory animal such as a dog.
[0086] A further aspect of the invention provides a screening method for identifying a drug-like compound or lead compound for the development of a drug-like compound in which (1) a mammal is exposed to a compound of formula I as defined herein (for example a perfluorinated fatty acid) or derivative thereof (2) the plasma insulin, glucose, cholesterol, triglyceride and/or leptin level of the mammal is measured, and/or bodyweight of the mammal is measured, and/or lipid or eicosanoid status (i.e. type and level of at least one lipid or eicosanoid) or function (for example assessed by degree of responsiveness to the mammal to a lipid or eicosanoid) of the mammal is measured.
[0087] A further aspect of the invention provides a screening method for identifying a drug-like compound or lead compound for the development of a drug-like compound in which (1) a compound of formula I as defined herein or related compound is exposed to a PPAR polypeptide (2) the binding of the compound to the PPAR polypeptide is measured or the change in the activity of the PPAR polypeptide is measured. Suitable methods by which binding of the compound to the PPAR polypeptide or effect on activity of the PPAR polypeptide may be measured are described, for example, in U.S. Pat. No. 6,028,109. The method may comprise the step of selecting a compound that binds to the PPAR polypeptide and/or changes its activity, for example nucleic acid binding activity and/or transcription factor activity. It is preferred that the selected compound increases PPARα or PPARγ activity i.e. acts as a PPARα or PPARγ agonist, or decreases PPARδ activity, i.e. acts as a PPARδ antagonist.
[0088] A further aspect of the invention provides a screening method for identifying a drug-like compound or lead compound for the development of a drug-like compound in which (1) a compound of formula I as defined herein or related compound is exposed to a lipid metabolising or binding entity, for example cycloxygenase (for example cyclooxygenase I or cyclooxygenase II) or phospholipase A (for example phospholipase A2) (2) the binding of the compound to the lipid metabolising or binding entity is measured or the change in the activity of the lipid metabolising or binding entity is measured. Suitable methods by which binding of the compound to the lipid metabolising or binding entity or effect on activity of the lipid metabolising or binding entity may be measured will be well known to those skilled in the art. Methods similar to those described in, for example, U.S. Pat. No. 6,028,109, may be suitable, as noted above. The method may comprise the step of selecting a compound that binds to the lipid metabolising or binding entity and/or changes its activity, for example production of arachidonic acid from appropriate phospholipid (phospholipase A) or production of prostaglandin from arachidonic acid (cyclooxygenase). It is preferred that the selected compound decreases the enzymic or binding activity i.e. acts as an inhibitor of the enzyme or binding entity.
[0089] A screening method of the invention may involve comparing the effect achieved using the test compound with that achieved using APFO or PFOA or other compound with desirable properties, as indicated above. A screening method of the invention may involve determining whether the test compound is able to compete with APFO or PFOA or other compound with desirable properties, as indicated above, for example whether it competes with APFO or PFOA for binding to a PPAR polypeptide, for example PPARα, or other lipid metabolising or binding entity; for example COXI, COXII or phospholipase A2.
[0090] Useful screening methods (for example in which the effect of the test compound is compared with that of APFO or PFOA or other compound with desirable properties, as indicated above) also include lipid displacement assays, cell (for example adipocyte) differentiation assays, or other phenotypic assays, insulin sensitisation assays, antiinflammatory screen, or investigation of effects on eicosanoid biosynthesis. The compound may be tested in animal models useful in investigating conditions of interest as noted above, such as obesity, diabetes, hyperlipidaemia or carcinogenesis. Such models include obese (ob/ob) or diabetic (db/db) mice, APC/min mice, BB rat or human tumour xenograft models, as known to those skilled in the art.
[0091] A further aspect of the invention provides a screening method for identifying a drug-like compound or lead compound for the development of a drug-like compound in which (1) a cell is exposed to a compound of formula I as defined herein (for example a perfluorinated fatty acid) or derivative thereof (2) the phenotype (for example differentiation) and/or eicosanoid biosynthesis of the cell is measured. The method preferably comprises the step of selecting a compound on exposure to which the phenotype, for example differentiation, of the cell is changed, and/or eicosanoid biosynthesis of the cell is changed, preferably reduced.
[0092] The screening methods may be useful in identifying a drug-like compound or lead compound for the development of a drug-like compound for treating diabetes, obesity, hypercholesterolaemia and/or hyperlipidaemia.
[0093] The methods may further comprise the step of determining whether the compound is toxic or carcinogenic, for example at a concentration sufficient to elicit a change in bodyweight or bodyweight gain, plasma insulin, glucose, cholesterol, triglyceride and/or leptin levels. Such methods will be well known to those skilled in the art.
[0094] It will be appreciated that the compound may preferably be tested in more than of the screening methods of the invention. For example, a compound may be tested for its effect on a PPAR polypeptide, and for its effect on a mammal to which it is administered. The toxicity or carcinogenicity of the compound may also be determined.
[0095] The term “drug-like compound” is well known to those skilled in the art, and may include the meaning of a compound that has characteristics that may make it suitable for use in medicine, for example as the active ingredient in a medicament. Thus, for example, a drug-like compound may be a molecule that may be synthesised by the techniques of organic chemistry, less preferably by techniques of molecular biology or biochemistry, and is preferably a small molecule, which may be of less than 5000 Daltons molecular weight. A drug-like compound may additionally exhibit features of selective interaction with a particular protein or proteins and be bioavailable and/or able to penetrate cellular membranes, but it will be appreciated that these features are not essential.
[0096] The term “lead compound” is similarly well known to those skilled in the art, and may include the meaning that the compound, whilst not itself suitable for use as a drug (for example because it is only weakly potent against its intended target, non-selective in its action, unstable, difficult to synthesise or has poor bioavailability) may provide a starting-point for the design of other compounds that may have more desirable characteristics.
[0097] These “lead” compounds may then be developed further, for example by molecular modelling/and or experiments to determine a structure activity relationship, in order to develop more efficacious compounds, for example by improving potency, selectivity/specificity and pharmacokinetic properties.
[0098] The methods may be performed ill vitro, either in intact cells or tissues (for example liver cells or adipocytes), with broken cell or tissue preparations or at least partially purified components. Alternatively, they may be performed in vivo. The cells tissues or organisms in/on which the use or methods are performed may be transgenic. In particular they may be transgenic for a PPAR polypeptide or lipid metabolising or binding entity.
[0099] It will be appreciated that the polynucleotide encoding the PPAR (for example PPARα, β or γ) or lipid metabolising or binding entity may be mutated in order to encode a variant of the PPAR, for example by insertion, deletion, substitution, truncation or fusion, as known to those skilled in the art. It is preferred that the PPAR or lipid metabolising or binding entity is not mutated in a way that may materially affect its biological behaviour, for example its nucleic acid binding or transcription factor activity or lipid metabolising or binding activity, as appropriate.
[0100] The following references relate to the sequences and tissue distribution of PPARs: Auboeuf et al (1997) Diabetes 46(8), 1319-1327; Braissant et al (1996) Endocrinol 137(1), 354-366; Mukherjee et al (1994) J Steroid Biochem Mol Biol 51, 157-166; Mukerjee et al (1997) J Biol Chem 272, 8071-8076.
[0101] The following references and GenBank Accession numbers relate to the sequences and/or tissue distribution of the indicated polypeptides.
[0102] U63846 Human COX-1 cDNA (PTSG1); Hla (1996) Prostaglandins 51, 81-85.
[0103] NM000963 Human COX2 cDNA (PTSG2); Hla & Neilson (1992) PNAS 89(16), 7384-7388; Jones et al (1993) J Biol Chem 268(12), 9049-9054; Appleby et al (1994) Biochem J 302, 723-727; Kosaka et al (1994) Eur J Biochem 221(3), 889-897.
[0104] AF306566 Human phospholipase A2 (secreted form); Valentin et al (2000) Biochem Biophys Res Commun 279(1), 223-228.
[0105] NMO21628 Human lipogenase ALOXE3.
[0106] XM005818 Human lipoxygenase ALOXE5.
[0107] XM008328 Human lipoxegenase ALOXI2.
[0108] NM001141 Human lipoxegenase ALOXI5; Brash et al (1997) PNAS 94(12), 6148-6152.
[0109] NM005090 and NM 003706 Human phospholipase A2 (cPLA2-gamma) Underwood et al (1998) J Biol Chem 273(34), 21926-21932 and Pickard et al (1999) J Biol Chem 274(13), 8823-8831
[0110] M68874 Human phospholipase A2 (cPLA2) Sharp et al (1991) J Biol Chem 266(23), 14850-14853.
[0111] It will be appreciated that such a compound may be an agonist or antagonist of the PPAR polypeptide used in the screen and that the intention of the screen is to identify compounds that act as agonists or antagonists of the PPAR, even if the screen makes use of a binding assay rather than an activity assay, for example transcription factor activity or nucleic acid (for example DNA) binding activity. It will be appreciated that the action of a compound found to bind the PPAR polypeptide may be confirmed by performing an assay of transcription factor activity or nucleic acid binding activity in the presence of the compound.
[0112] Likewise, such a compound may be an inhibitor or activator of the lipid metabolising or binding entity used in the screen and that the intention of the screen is to identify compounds that act as inhibitors or activators of the lipid metabolising or binding entity, even if the screen makes use of a binding assay rather than an activity assay, for example lipid metabolising activity, for example prostaglandin production from arachidonic acid for COXI or COXII. It will be appreciated that the action of a compound found to bind the lipid metabolising or binding entity may be confirmed by performing an assay of the appropriate enzyme or binding activity in the presence of the compound. It is preferred that the assay is capable of being performed in a “high throughput” format. This may require substantial automation of the assay and minimisation of the quantity of a particular reagent or reagents required for each individual assay. A scintillation proximity assay (SPA) based system, as known to those skilled in the art, may be beneficial. Combinatorial chemistry techniques may be used in generating compounds to be tested.
[0113] A further aspect of the invention provides a kit of parts of screening system comprising (1) a library of compounds each of formula I as herein defined or a derivative thereof, and (2) a PPAR polypeptide or polynucleotide encoding a PPAR polypeptide, and/or a test mammal. The kit may optionally comprise reagents useful in measuring plasma insulin, glucose, triglyceride and/or cholesterol levels, or in measuring PPAR activity, for example nucleic acid binding. Such reagents will be apparent to those skilled in the art, and may include reagents useful in performing transactivation assays or DNA binding assays.
[0114] A further aspect of the invention provides a kit of parts of screening system comprising (1) a library of compounds each of formula I as herein defined or a derivative thereof, and (2) a lipid metabolising or binding entity (for example COXI or COXII or phospholipase A2 or lipoxygenase) or polynucleotide encoding a lipid metabolising or binding entity. The kit may optionally comprise reagents useful in measuring plasma insulin, glucose, triglyceride, cholesterol and/or leptin levels, or in measuring the activity of the lipid metabolising or binding entity, for example a substrate of the lipid metabolising or binding entity (for example arachidonic acid in the case of COXII or lipoxygenase) or reagent useful in measuring a product of a lipid metabolising enzyme, for example in assessing eicosanoid biosynthesis. As well known to those skilled in the art, reagents may include labelled ligand, for example radiolabelled or fluorescently labelled. Direct binding or displacement of ligand may be measured. Binding may be measured using fluorescence resonance energy transfer (FRET) techniques. The kit may optionally include reagents useful in cell differentiation assays, for example adipocyte differentiation assays, as will be known to those skilled in the art.
[0115] A further aspect of the invention provides a compound identifiable or identified by a screening method of the invention. A further aspect of the invention provides a compound identified or identifiable by a screening method of the invention for use in medicine. A further aspect of the invention provides a pharmaceutical composition comprising a compound identified or identifiable by a screening method of the invention and a pharmaceutically acceptable excipient. Preferences in relation to properties of such compounds are as indicated above and in relation to the first aspect of the invention.
[0116] A compound identified or identifiable by a screening method of the invention is also provided for use in the manufacture of a composition for use as a food supplement or a food additive. The invention also relates to a food product comprising a foodstuff and a compound of formula I as defined herein or a compound identified or identifiable by a screening method of the invention, wherein the food is not laboratory rodent, for example rat or mouse, feed. It is preferred that the food is not laboratory animal feed.
[0117] Preferably, the food (the term including food product and foodstuff) is suitable for administration to an animal (for example a domesticated animal as discussed above but not a laboratory rodent) or human, for example an adult human, baby or infant.
[0118] A further aspect of the invention provides the use of a compound identified or identifiable by a screening method of the invention in the manufacture of a medicament for the treatment of a patient in need of modulation (for example reduction) of body mass or modulation (preferably reduction or prevention) of increase in body mass, and/or in need of modulation (preferably reduction) of plasma insulin, plasma glucose, plasma triglycerides and/or plasma cholesterol, and/or in need of modulation of plasma leptin. The patient may be obese and/or have diabetes, hyperlipidaemia and/or atherosclerosis, or be at risk of developing such a condition.
[0119] A further aspect of the invention provides the use of a compound identified or identifiable by a screening method of the invention in the manufacture of a medicament for the treatment of a patient who is overweight or obese and/or has diabetes, hyperlipidaemia, atherosclerosis, coronary heart disease, stroke, obstructive sleep apnoea, arthritis (for example osteoarthritis) and/or reduced fertility, or is at risk of developing such a condition.
[0120] A further aspect of the invention provides the use of compound identified or identifiable by a screening method of the invention in the manufacture of a medicament for treating a patient in need of modulation of PPAR (for example PPARα) or modulation of lipid or eicosanoid status or function, or of lipid metabolising or binding entity (for example COXI, COXII, phospholipase A or lipoxygenase) activity. Preferably the patient is in need of an increase in PPAR (preferably PPARα or PPARγ) activity and the compound is a PPAR (for example a PPARα or PPARγ) agonist. Alternatively, the patient may be in need of a decrease in activity of a lipid metabolising or binding entity and the compound is an inhibitor of that lipid metabolising or binding entity (or entities).
[0121] The compounds may be administered in any suitable way, usually parenterally, for example intravenously, intraperitoneally or intravesically, in standard sterile, non-pyrogenic formulations of diluents and carriers. The compounds may also be administered topically. The compounds of the invention may also be administered in a localised manner, for example by injection. Preferably, the compounds are administered orally. The compounds may be administered as a tablet or capsule or as a supplement added to food or drink. A slow-release formulation may be used.
[0122] A further aspect of the invention provides a method of treatment of a patient in need of modulation (preferably reduction) of body mass or modulation (for example reduction or prevention) of increase in body mass, and/or in need of modulation (for example reduction) of plasma insulin, plasma glucose, plasma triglycerides, plasma cholesterol and/or leptin, comprising administering to the patient an effective amount of a compound identified or identifiable by the screening method of the invention. A further aspect of the invention provides a method of treatment of a patient who is overweight or obese and/or has diabetes, hyperlipidaemia, atherosclerosis, coronary heart disease, stroke, obstructive sleep apnoea, arthritis (for example osteoarthritis) and/or reduced fertility, or is at risk of developing such a condition, comprising administering to the patient an effective amount of a compound identified or identifiable by the screening method of the invention.
[0123] Preferences in relation to the patient and compound are as indicated above.
[0124] A further aspect of the invention provides a method of treatment of a patient in need of modulation of PPAR (for example PPARα., δ or γ) activity, or of lipid or eicosanoid status or function, or of a lipid metabolising or binding entity activity, comprising administering to the patient an effective amount of a compound identified or identifiable by the screening method of the invention.
[0125] Preferably the patient is in need of an increase in PPAR (preferably PPARα. or γ) activity and the compound is a PPAR (for example a PPARα. or γ) agonist. Further preferences in relation to the patient and compound are as indicated above. Alternatively, the patient may be in need of a decrease in activity of a lipid metabolising or binding entity and the compound is an inhibitor of that lipid metabolising or binding entity or entities.
[0126] The invention is now described in more detail by reference to the following, non-limiting, Figures and Examples:
DETAILED DESCRIPTION OF THE DRAWINGS
[0127] FIG. 1 : Growth curves for male Fischer 344 rats administered APFO in diet.
[0128] FIG. 2 : Food consumption by Fischer 344 rats administered APFO in diet.
[0129] FIG. 3 : Food utilisation in Fischer 344 rats administered APFO in diet.
[0130] FIG. 4 : Effect of APFO treatment on plasma insulin concentration.
[0131] FIG. 5 : Effect of APFO on plasma cholesterol concentration.
[0132] FIG. 6 : Effect of APFO on plasma glucose concentration.
[0133] FIG. 7 : Effect of APFO on plasma triglyceride concentration.
[0134] FIG. 8 : compounds indicated to be PPAR agonists in U.S. Pat. No. 6,028,109
[0135] FIG. 9 : Effect of APFO treatment on mouse body weights
[0136] FIG. 10 : Effect of APFO treatment on mouse food consumption
[0137] FIG. 11 : Effect of APFO treatment on mouse food consumption (expressed as grams food consumed per unit body weight).
[0138] FIG. 12 : Effect of APFO treatment on mouse plasma insulin concentration. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0139] FIG. 13 : Effect of APFO treatment on mouse plasma triglyceride concentration. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0140] FIG. 14 : Effect of APFO on mouse plasma glucose concentration. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0141] FIG. 15 : Effect of APFO treatment on mouse plasma cholesterol. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0142] FIG. 16 : Effect of APFO treatment on mouse plasma leptin. Values are Mean±3D. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0143] FIG. 17 : Effect of APFO treatment of mouse epididimal fat pad weight. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0144] FIG. 18 : Effect of APFO treatment on rat body weight.
[0145] FIG. 19 : Effect of APFO treatment on rat food consumption.
[0146] FIG. 20 : Effect of APFO on rat food consumption (expressed as grams food consumed per unit body weight).
[0147] FIG. 21 : Effect of APFO treatment on plasma insulin concentration. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0148] FIG. 22 : Effect of APFO treatment on rat plasma glucose concentration. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0149] FIG. 23 : Effect of APFO treatment on rat plasma triglyceride concentration. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0150] FIG. 24 : Effect of APFO treatment on rat plasma cholesterol. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0151] FIG. 25 : Effect of APFO treatment on rat plasma leptin concentration.
[0152] FIG. 26 : Cytotoxic effect of APFO on HepG2 cells (A), HT-29 cells (B) and MCF7 cells (C).
[0153] FIG. 27 : Effect of prophylactic APFO treatment on tumour volume in an HT-29 xenograft model. *=APFO administration. Arrow indicates the point of tumour cell implantation. Tumour measurement began on day 1.
[0154] FIG. 28 : Effect of prophylactic APFO administration on tumour volume between day 1 and day 15 of treatment. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0155] FIG. 29 : Effect of prophylactic APFO administration on tumour weight. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0156] FIG. 30 : Effect of therapeutic APFO treatment on tumour volume in an HT-29 xenograft model. *=APFO administration. Arrow indicates the point of tumour cell implantation. Tumour measurement and APFO administration began on day 1 .
[0157] FIG. 31 : Effect of therapeutic APFO administration on tumour volume between day 1 and day 17 of treatment. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0158] FIG. 32 : Effect of therapeutic APFO administration on tumour weight. Values are Mean±SD. Significantly different from respective control group (0 mg/kg); *p<0.05; **p<0.01; ***p<0.001.
[0159] FIG. 33 : Effect of prophylactic APFO administration on nu/nu mouse body weight.
[0160] FIG. 34 : Effect of therapeutic APFO administration on nu/nu mouse body weight.
[0161] FIG. 35 : Activation of Mouse PPARα by APFO.
[0162] FIG. 36 : Interaction of APFO with Ligand Binding Domain of Human PPARγ.
DETAILED DESCRIPTION OF THE INVENTION
Example 1
Effect of Per Fluorinated Fatty Acid on Insulin, glucose, cholesterol and triglyceride levels, and on Body Weight
Methods
[0163] Male Fisher 344 rats (initially 6 weeks old) were administered ammonium perfluorooctanoate (APFO, 300 ppm) in the diet for periods of time up to one year. Control rats received powdered diet that did not contain APFO.
[0164] Body weights were initially determined daily and then weekly. Food consumption was determined weekly. Clinical observations were made daily.
[0165] Rats were sacrificed at 1, 2, 7, 14, 28, 90, 182 and 365 days. There were 8 rats per group. At sacrifice blood was sampled by cardiac puncture and submitted for clinical chemistry.
[0166] The following assay methods/kits were used:
[0000]
Assay
Supplier
Kit Number
ALT
Roche Diagnosis
MPR 1087 568
AST
Roche
Unimate 3 0736414
Diagnostics
Glucose
Roche
MPR2 1442 449
Diagnostics
Triglycerides
Roche
Peridochrom GPO-PAP
Diagnostics
701 882
Cholesterol
Roche
CHOD-AP MPR3 236691
Diagnostics
Insulin
Amersham
RNP 2567
Results
[0167] Administration of APFO to male Fischer 344 rats lead to marked reductions in bodyweight gain ( FIG. 1 ). Treated animals had body weights approximately 25-30% lower than concurrent controls. This weight change was not accompanied by any adverse clinical symptoms or changes in activity.
[0168] Food consumption expressed per rat was markedly decreased (to approximately 50% of control consumption) during the first week of treatment. However, after this time, food consumption per rat increased to 80-90% of control values ( FIG. 2 ).
[0169] When expressed as weight of food consumed per unit bodyweight, food consumption was decreased by approximately 30% during the first week of APFO administration. However, at later times APFO-treated animals consumed between 10 and 30% more food per unit bodyweight than controls ( FIG. 3 ).
[0170] Plasma cholesterol, glucose and insulin concentrations were decreased at all time points examined ( FIGS. 4-6 ), while plasma triglycerides were decreased at 7 days and beyond ( FIG. 7 ).
[0171] These data suggest that APFO and related compounds may be useful for treatment of obesity, diabetes, hypertriglycerideaemia and hypercholesterolaemia and diseases where alterations in lipid or eicosanoid status may be desirable, such as arthritis or cancer.
Example 2
Effect of APFO in Reversing Obesity and Diabetes
[0172] The effect of APFO in animal models of obesity and diabetes was studied in order to establish the therapeutic potential of APFO to reverse obesity and diabetes.
[0173] The studies reported in Example 1 involving the administration of APFO to Sprague Dawley rats for up to one year, demonstrated the compound's anti-diabetic and anti-obesity potential. Following an initial reduction in food consumption during the first week of the study, an increase in food consumption per unit body weight was coupled to a marked reduction in body weight gain in treated animals throughout the test period. Furthermore, plasma cholesterol and insulin concentrations were decreased at all time points examined, while plasma glucose and triglycerides were decreased at 7 days and 5 beyond.
[0174] In this Example, these observations in healthy rats are extended by investigations in two models of metabolic disease—the obese mouse (ob/ob) and the diabetic GK/Mol. rat.
[0000] 1.1 Mouse Model (ob/ob)
[0175] The C57BL/6J-ob/ob mouse is an obese, leptin-deficient animal that is widely accepted as a model of obesity and diabetes. Age-paired, disease-free (lean) animals (C57BL/6J−+/+) were also included in the study to observe the ‘normal’ response.
[0176] 1.1.1 Experimental Design and Methods.
[0177] Three groups (n=5) of ob/ob (C57BL/6J-ob/ob) mice were treated with 3 dose levels of APFO (5, 15 and 25 mg/kg/day). Animals were administered APFO, dissolved in water, by oral gavage, daily for 14 days. One group of 10 ob/ob mice was also treated with vehicle (water) alone. Additionally, to observe the ‘normal’ response, 5 age-paired, disease-free animals (C57BL/6J−+/+) were administered 25 mg/kg APFO and a similar disease-free control group was administered vehicle only.
[0178] Twenty-four hours after the last dose the animals were killed by an increasing concentration of carbon dioxide. Blood was collected by cardiac puncture and plasma prepared and stored at −70° C. until analysed. Major tissues were weighed, sampled, flash frozen in liquid nitrogen and stored at −70° C.
[0179] Plasma was analysed for triglycerides, cholesterol and glucose using kits purchased from Sigma (Poole, Dorset). Concentrations of plasma insulin and leptin were determined using commercially available enzymeimmunoassay-based kits from Amersham Life Sciences and Crystalchem Inc., (Chicago) respectively. All assays were carried out as specified by the manufacturer.
[0180] 1.1.2 Results and Discussion.
[0181] Both strains of mice treated at 25 mg/kg/day lost bodyweight over the treatment period. In +/+mice this was only apparent after day 4; these animals also lost less weight, as a percentage of initial bodyweight, than the ob/ob mice (26% versus 33%). In ob/ob mice treated at 15 mg/kg/day 20% bodyweight loss was noted over the study period. Animals treated at 5 mg/kg/day were unaffected ( FIG. 9 ). No other adverse clinical observations were observed.
[0182] The bodyweight losses were reflected in marked, APFO dose-related, decreases in food consumption (76%, 53% and 17% lower than control mice at the high, intermediate and low dose levels respectively) ( FIG. 10 ). In +/+mice a decrease in food consumption was evident over the first nine days of treatment, following which there was a steep recovery towards control values without equalling them. The overall consumption was still 31% lower than in +/+controls. When expressed in terms of food consumed per gram of bodyweight the pattern of effect was similar, although the recovery in values seen in +/+mice after day 9 was greater and the subsequent values more nearly equal to those of their controls ( FIG. 11 ).
[0183] There was a very marked reduction (greater than 90%) in plasma insulin concentrations in all treated ob/ob mice, which was broadly related to dose level ( FIG. 12 ). In +/+mice, control insulin levels were notably lower than in the ob/ob mice. However, APFO-treatment still led to a marked reduction in plasma insulin concentrations.
[0184] APFO-treated (15 or 25 mg/kg/day) ob/ob mice showed dose-related reductions in plasma glucose down to approximately 20% of control values, similarly plasma triglyceride concentrations were decreased to 40% of control values ( FIGS. 13 and 14 ). At 5 mg/kg/day administered to ob/ob mice, glucose was reduced by approximately 50% but there was no effect on triglyceride concentrations ( FIG. 14 ). In +/+mice, APFO (25 mg/kg/day) decreased glucose and triglycerides to 55% and 35% of control plasma values respectively.
[0185] At a dose of APFOOf 25 mg/kg/day to both strains there was an approximate 30% reduction in plasma cholesterol concentrations. This was not evident at the low and mid dose levels in the ob/ob mice ( FIG. 15 ).
[0186] Plasma leptin concentrations in the ob/ob mice were below the levels of quantitation; this was expected as there is an early stop codon within the leptin gene of this mouse strain. Treatment of the +/+mouse, which possesses a normal leptin gene, with APFO (25 mg/kg/day) resulted in decreased plasma leptin concentrations to, or below the level of quantitation ( FIG. 16 ).
[0187] Epididymal fat pad (white adipose tissue) weights were 7-fold higher in control ob/ob mice compared to control +/+mice. APFO-treatment decreased the weight of the epididymal fat pads in a dose-related manner in ob/ob mice and +/+mice ( FIG. 17 ).
[0188] 1.1.3 Conclusions.
[0189] In summary, there were a number of significant physiological effects that could be related to the administration of APFO. In lean controls, there was a slight reduction in body weight, and this loss reached a nadir after 10 days with no weight loss occurring after this time. Food consumption in this group remained constant.
[0190] At the high and intermediate dose levels, ob/ob mice continued to lose body weight. At 25 mg/kg, ob/ob mice also displayed appetite loss (reflected in body weight changes). In this group there was also marked reduction in glucose levels. This appeared to suggest that the anti-obesity effects may have been due to reduced food consumption. However, in animals treated with 5 mg/kg APFO, a 17% reduction in food consumption was associated with a 50% reduction in plasma glucose levels, which suggested that the anti-obesity effects observed in ob/ob mice were due to metabolic changes caused by APFO, and not to a loss of appetite.
[0191] These data suggest that APFO causes weight loss in obese animals, but not, significantly, in lean animals and so may be used as an anti-obesity agent. Additionally the APFO-induced decreases in plasma glucose and insulin suggest that this chemical may be of therapeutic use in Type II diabetes.
1.2 Rat GK/Mol Model.
[0192] The GK/Mol rat is a non-obese, diabetic animal that is widely accepted as a model of Type II diabetes. In order to measure the ‘normal’ response, non-diabetic Wistar rats were also used in the study.
1.2.1 Experimental Design and Methods.
[0193] Three groups (n=5) of GK/Mol rats were administered 3 dose levels of APFO (3, 10 and 30 mg/kg). Animals were administered APFO by oral gavage, daily for 14 days. One group of 10 GK/Mol rats was also treated with vehicle (water) alone. Additionally, to observe the ‘normal’ response, 5 age-paired, disease-free Wistar rats were administered 30 mg/kg APFO and a similar disease-free group was administered vehicle only.
[0194] Twenty-four hours after the last dose the animals were killed by an increasing concentration of carbon dioxide. Blood was collected by cardiac puncture and plasma prepared and stored at −70° C. until analysed. Major tissues were weighed, sampled, flash frozen in liquid nitrogen and stored at −70° C.
[0195] Plasma was analysed for, triglycerides, cholesterol, glucose, insulin and leptin as described in section 1.1.1.
1.2.2 Results and Discussion.
[0196] APFO administration to GK/Mol rats resulted in a dose-dependent decrease in body weight gain to 90%, 71% and 44% of control values at the low, mid and high dose levels respectively ( FIG. 18 ). There was no effect on bodyweight gain in treated Wistar rats.
[0197] Treated GK/Mol rats had slightly lower total food consumption (86-98% of control values), although this difference was not related to dose level ( FIG. 19 ). There was no difference in food consumption between treated Wistar rats and their controls. No pattern was discernible when the data were expressed as food eaten per gram of body weight ( FIG. 20 ).
[0198] There was a marked dose-dependent reduction in the plasma concentration of insulin, reaching about 10% of control values in both strains of rat ( FIG. 21 ).
[0199] Plasma glucose concentrations in GK/Mol rats were lowered by APFO to about 85% of control values at dose levels of 30 mg/kg/day ( FIG. 22 ). Plasma Triglycerides ( FIG. 23 ) and cholesterol ( FIG. 24 ) concentrations were lower by between 10 and 20% in treated GK/Mol rats. In Wistar rats, plasma cholesterol was reduced to 73% of control values.
[0200] Group mean plasma concentrations of leptin ( FIG. 25 ) were slightly lower (by approximately 40%) in Wistar rats treated at 30 mg/kg/day than in their controls. There were no differences in leptin concentrations in the GK/Mol rats that could be indicative of a treatment-related effect.
1.2.3 Conclusions.
[0201] The GK/mol study followed a similar pattern to the investigation in Sprague Dawley rats (Example 1). APFO caused a reduction in the levels of glucose, triglycerides and cholesterol coupled to reduced weight gain in treated animals; there was also a marked reduction in the level of plasma insulin.
[0202] In conclusion APFO demonstrated anti-diabetic effects in a rat model for type II diabetes, further indicating it may be an effective agent for the treatment of this condition.
2. Therapeutic Potential of APFO as an Anti-cancer Agent.
[0203] The effect of APFO in vitro against human tumour cell lines and in vivo in a human tumour xenograft model was examined.
2.1 In Vitro Anti-Tumour Activity.
[0204] Three human cancer cell lines were exposed to APFO and cytotoxicity levels assessed in order to assess APFO's functions as an anti-cancer agent.
2.1.1 Experimental Design and Methods.
[0205] HT-29 cells (human colon tumour-derived), MCF7 cells (human breast cancer-derived) and HepG2 cells (human liver cancer-derived) were cultured in Dulbecco's Modified Eagles Medium (DMEM) supplemented with 10% heat inactivated foetal calf serum, 2 mM L-glutamine, penicillin (50 lU/ml), streptomycin (50 μg/ml) and 1% non-essential amino acids. Cells were harvested by trypsinisation and diluted to 5×10 4 cells/ml, and 2000 μ1 of cell suspension was plated into each well of a 96 well plate and allowed to attach overnight at 37° C. with 5% C0 2 . Cells were exposed to various concentrations of APFO in growth medium (0.01, 0.03, 0.1, 0.3, 1, 3, 10, 30 and 100 and 100 μM) for four hours. 20 μ1 of a 5 mg/lm MTT solution was added to each well and the cells were incubated for 4 hours at 37° C. The medium was removed and 200 μI DMSO was added to dissolve formazan crystals.
[0206] Plates were read at 570 nm and background at 690 nm was subtracted. Results were displayed graphically as percentage cell survival versus APFO concentration.
2.1.2Results and Discussion.
[0207] APFO elicited a cytotoxic effect after 4 hours at concentrations exceeding 500 μM ( FIG. 26 ).
2.1.3 Conclusions
[0208] This study indicated that APFO was effective at killing a range of human cancers in vitro.
2.2 HT-29 Xenograft Model in Nude Mice.
[0209] The objective of this study was to examine the anti-tumour capabilities of APFO in a xenografted animal model. Effects of APFO on tumour progression were tested on a human colon cancer-derived cell line xenografted into immune-deficient nu/nu mice. Prophylactic and therapeutic effects of APFO were assessed by measurement of tumour size at regular intervals during administration of APFO.
2.2.1 Experimental Design and Methods.
[0210] Athymic nude (nu/nu) mice from ICRF stock (HsdOla:ICRF-nu) were obtained from Clare Hall (Potters Bar, UK). All animals were female and approximately 9 weeks old. Animals, housed in isolator cages and handled under laminar flow, were divided into one control group and two treatment groups, with 5 female mice per group for both the prophylactic and therapeutic schedules
[0211] HT-29 cells were cultured according to the conditions described in section 2.1.1. Cells were harvested, pooled by centrifugation and resuspended in 5 ml medium to which 5 ml Matrigel (basement membrane matrix) was added. 100 μl of cell suspension was injected subcutaneously into each flank of the mice (1.75×10 6 cells per flank). In order to assess the prophylactic effect of APFO, half of the animals were administered the compound immediately following tumour cell implantation. For the therapeutic schedule, APFO was injected once tumours had developed.
[0212] Animals were administered APFO, dissolved in water, by intra-peritoneal (ip) injection 3 times per week for one month. The doses of APFO were 15 mg/kg and 25 mg/kg bodyweight. The volume of the dosing solution was 10 ml/kg bodyweight. Control animals received an equivalent volume of water.
[0213] Animal bodyweights were recorded throughout the study. Tumour growth was measured 3 times per week using digital calipers and the volume was calculated using the formula:
[0000]
4
/
3
π
·
{
(
d
1
+
d
2
)
3
4
}
[0000] Where d 1 =mean length (n=2) and d 2 =mean width (n=2). (NB, n=4 if tumour was an irregular shape).
[0214] The maximum permitted tumour volume, according to the terms of the Home Office licence, was 1.44 cm 3 . Results were expressed graphically for each time point as mean tumour volumes. Tumour weights were recorded at the end of the study, and tumour samples were either snap frozen in liquid nitrogen or fixed in formal saline for further analysis.
2.2.2 Results and Discussion.
[0215] HT-29-derived tumours developed approximately 14 days into the study.
[0216] Tumour growth in both prophylactic and therapeutic groups proceeded at a much faster rate in control groups compared to tumours in APFO-treated animals ( FIGS. 27 and 30 respectively). Consequently, the therapeutic study was not completed because control animals were lost either because tumour volume exceeded the permitted size, or because the tumours were deemed ulcerated and again continuance was not permitted under the terms of the Project Licence. Hence, animals in the therapeutic study were injected at 8 time points compared to 13 time points in the prophylactic study.
[0217] Tumour growth rate in animals treated prophylactically was markedly slower in APFO-treated animals, with a lag phase of 15 days for control groups compared to 22 days for APFO-treated mice ( FIG. 27 ). In animals administered 25 mg/kg APFO, tumour growth reached a plateau after 26 days, while in animals dosed at 15 mg/kg, tumour volume continued to increase ( FIG. 27 ). Tumour volume in the prophylactic groups increased 18 fold in controls, 8 fold at 15 mg/kg and 6 fold at 25 mg/kg between the start of tumour measurement (day 1) and the end of the study (day 15) ( FIG. 28 ). Upon necroscopy, in the 15 mg/kg and 25 mg/kg groups respectively, tumour weights were 22% and 58% smaller than in control animals ( FIG. 29 ).
[0218] Tumour growth rate was also markedly slower in animals treated therapeutically with APFO, with a lag phase of 17 days in control tumours compared to 26 days in treated mice ( FIG. 30 ). No plateau was reached in the highest dose group, but the study was incomplete as animals were treated for a shorter period than intended.
[0219] Tumour volume increased 15-fold in controls, 14-fold at 15 mg/kg, and 7-fold at 25 mg/kg between day 1 and day 17 ( FIG. 31 ). Tumour weights were 45% and 37% smaller in the 15 mg/kg and 25 mg/kg dose groups respectively ( FIG. 32 ). It should be noted that 5 animals (4 controls and 1 high dose animal) had been lost from the study, thus affecting mean values of final tumour weights.
[0220] Tumours were removed from animals at the end of the study period and examined macroscopically. Control tumours from the prophylactic group were solid, while APFO-treated animals produced tumours that were fluid-filled, suggesting cell death in the centre of the tumours. Differences between control and treated groups were less obvious in animals treated therapeutically, but these animals were dosed for a shorter period. Samples of tumours were formalin fixed and also flash frozen in liquid nitrogen for histopathalogical examination.
[0221] Animal body weights were monitored and recorded throughout the study. There was no significant difference between control and treated animals in either the prophylactic or therapeutic groups in animals implanted with HT-29 cells ( FIGS. 33 and 34 ).
2.2.3 Conclusions.
[0222] In summary, APFO demonstrated anti-tumour capabilities in a human cancer cell line when either given concomitantly with the tumour cells or following tumour establishment. Additionally, body weight remained unaffected by the test agent, suggesting that treatment-associated weight loss would not occur, a major advantage for chemotherapeutic agent. It is probable that treatment-associated weight loss did not occur because APFO selectively targets obese subjects and not lean subjects (eg. nu/nu mice).
[0223] Finally, APFO showed anti-tumour capabilities against HT-29 cells, a human colon cancer cell line, thus demonstrating that it is capable of inhibiting the growth of human tumour cells.
3. The Potential Anti-Inflammatory Properties of APFO.
3.1 In Vitro Studies
[0224] The ability of APFO (or other test compound) to inhibit cyclooxygenase 1 (COX1) and cyclooxygenase 2 (COX-2) inhibition is examined using an EIA-based human COX inhibitor assay kit as described by the manufacturer (Cayman Chemical, Michigan).
3.2 In Vivo Studies.
[0225] The anti-inflammatory potential of APFO (or other test compound) is examined in a rat model. Animals are dosed with APFO or dexamethasone, after which the animal's immune system is challenged with lipopolysaccharide (LPS) and plasma cytokines are measured. The study may consist of one control group and three treatment groups, with 10 male CD rats (80-120 g) per group. The control group is administered vehicle (water) only followed by LPS (30 μg per 100 g rat) 24 hrs later. Treatment group 1 animals receive APFO (or other test compound) at 30 mg·kg. Treatment group 2 animals receive APFO (or other test compound) at 30 mg·kg followed by LPS (30 μg per 100 g rat) 24 hrs later. Treatment group 3 animals received dexamethasone (10 mg·ml in corn oil) followed by LPS (30 μg per 100 g rat) 1 hour later. The plasma from 5 animals per group is harvested 1 hour or 2 hours post-treatment. Plasma cytokines (I1-6, 20 Il-1β and TNF) are measured using commercially available kits as specified by the manufacturer (Endogen Inc., Massachusetts).
[0000] 4. Interaction of APFO with PPAR Isoforms
[0226] Transactivation assays involving mouse PPAR alpha cDNA and ligand binding assays using human PPAR gamma were performed in order to demonstrate that APFO interacts with PPAR isoforms.
4.1 Mouse PP AR Transactivation Assay
4.1.1 Experimental Design and Methods
[0227] COS-1 cells (cultured in medium described in section 2.1.1 but without non-essential amino acids) were plated into 6 well tissue culture dishes at 3×10 5 cells per well and allowed to adhere overnight at 37° C. The next day the medium was aspirated and the cells washed with PBS, pH7.4, and 200 μl of a transient transfection cocktail was added to each well. The transfection cocktail was composed of 50 ng of vector DNA carrying mouse PPAR alpha, 500 ng of plasmid DNA containing the PPAR response element of liver fatly acid binding protein and, as a transfection control, 500 ng of a vector harbouring β-Galactosidase. DNA was dissolved in PBS containing 50 μg·ml DEAF-Dextran. Control cells were exposed to a transfection cocktail that contained no plasmid DNA. Cells were incubated at 37° C. for 30 minutes before 2 ml of medium containing 80 μM chloroquine was added and the cells incubated for a further 2.5 hours at 37° C. The medium was aspirated and the cells shocked with 10% DMSO in medium for 2.5 minutes at room temperature. Cells were washed with PBS then allowed to recover at 37° C. in growth medium for 24 hours.
[0228] Transiently transfected cells were exposed to APFO (dissolved in water) in medium at 0, 3, 10, 30, 100, 300 and 100 μM for 16 hours at 37° C. Cells were then washed, lysed, and luciferase and β-Galactosidase activities were measured using kits according to the methods specified by the manufacturer (Promega, Madison, USA) by flash luminescence and spectophotometry respectively. Luciferase expression was normalised by dividing by the flash luminescence reading with constitutive β-Galactosidase expression levels measured at 415 nm following a colourimetric assay.
[0229] Data were graphed, fitted to non-linear regression curves and EC 50 values calculated using GraphPad Prism software.
4.1.2 Results and Discussion
[0230] Activation of mouse PPAR alpha by APFO occurred, with an effective concentration (EC 50 ) of 102 μlM. ( FIG. 27 ).
4.1.3 Conclusions
[0231] The data presented here demonstrate that APFO is a mouse PPAR alpha activator at μM concentrations.
4.2 PPAR Gamma Ligand Binding Studies
[0232] His-tagged human PPARγ ligand binding domain was expressed in E. Coli as described previously [Palmer, CAN and Wolf, C R. FEES Letts. 431, 476-480, (1998)]. The receptor protein was partially purified by nickel affinity chromatography.
4.2.1Ligand Binding Studies.
[0233] This recombinant receptor protein has been used previously to study interactions with the fluorescent fatty acid—cis-parinaric acid (CPA)[Palmer CAN and Wolf C R. FEES Letts. 431, 476-480, (1998); Causevic M, Wolf C R and Palmer CAN. FEES Letts. 463, 205-210, (1999)]. On binding to the receptor, changes in the spectral properties of the fatty acid occurs. These are quantitatively related to the binding of the ligand to the receptor and can be used to calculate binding constants. A competitive displacement assay can be utilised to examine the binding characteristics of other compounds. APFO was assayed for its ability to displace cis-parinaric acid from PPARy by this method. Data were analysed as described in section 4.1.
4.2.2 Results and Discussion.
[0234] Competitive ligand binding assays using the ligand binding domain of human PPAR gamma showed that displacement of cis-parinaric acid occurred, with an EC 50 of 355 μM ( FIG. 28 ).
3.2.4 Conclusions
[0235] These data indicate that APFO interacts with the ligand binding domain of human PPAR gamma.
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The molecules of formula (I) are useful in treating diabetes, obesity, hypercholesterolaemia, hyperlipidaemia, cancer, inflammation or other conditions in which modulation of lipis of eicosanoid status or functions may be desirable. Formula (I): Z 1 —Z 1 —Z 2 wherein a) Z 1 represents CO 2 H or a derivative thereof; b) Z 2 represents F, H, —CO 2 H or a derivative thereof; and c) X represents fluorinated alkylene; or a solvate thereof, for example a perfluorinated fatty acid or derivative thereof.
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CROSS REFERENCE TO RELATED APPLICATIONS
This is a U.S. national stage of application No. PCT/JP2011/074180, filed on Oct. 20, 2011. Priority under 35 U.S.C. §119(a) and 35 U.S.C. §365(b) is claimed from Japanese Patent Application No. 2010-236612, filed on Oct. 21, 2010, the disclosure of which are also incorporated herein by reference.
TECHNICAL FIELD
The present invention relates to a transmission control device, a hybrid vehicle, a transmission control method, and a computer program.
BACKGROUND ART
The limitation of the torque of the engine in response to the torque required by a driver is a measure for reducing the exhaust gas of a vehicle. This gives a constant limitation on the torque of the engine even though the driver fully depresses the accelerator pedal, so that the vehicle is controlled to output torque less than the maximum torque (for example, see patent literature PTL1).
CITATION LIST
Patent Literature
PTL1: JP 2006-280049 A
SUMMARY OF INVENTION
Technical Problem
When a vehicle shifts the gears, the torque of the engine is temporarily reduced in order to transfer the gear from a gear number before the shift into neutral. After that, the gear is shifted to the gear number after the shift in order to return the torque of the engine that has temporarily been reduced. At that time, if the vehicle is in a mode in which the torque of the engine is limited in response to the request torque from the driver, the torque is limited even when the torque of the engine is returned after the gear has been shifted to the gear number after the shift from neutral. This causes the delay of the return of the torque in the gear shifting and aggravates the drivability.
In light of the foregoing, an objective of the present invention is to provide a transmission control device, a hybrid vehicle, a transmission control method, and a computer program that can improve the drivability in the gear shifting in a mode in which the torque of the engine is limited in response to the torque required by the driver.
Solution to Problem
An aspect of the present invention is directed to a transmission control device. According to the aspect of the present invention, the transmission control device of a hybrid vehicle that includes an engine and an electric motor, that is capable of running by the engine or the electric motor or capable of running by cooperation between the engine and the electric motor, includes: an output limitation means for limiting torque output from the engine and/or the electric motor; and an automatic gear shifting means for shifting a gear number according to a variation in a vehicle speed, in which the automatic gear shifting means performs a control for temporarily reducing the torque output from the engine in neutral while a gear is transferred from a gear number before the shift to a gear number after the shift through neutral once, and, when the gear shifting is performed during output limitation, the output limitation means performs a control for temporarily cancelling the output limitation in a process for returning the torque that has temporarily been reduced in neutral, and adding torque by the electric motor to torque of the engine.
Another aspect of the present invention is directed to a hybrid vehicle. The hybrid vehicle includes the transmission control device according to the present invention.
Still another aspect of the present invention is directed to a transmission control method. The transmission control method of a hybrid vehicle, that includes an engine and an electric motor, that is capable of running by the engine or the electric motor or capable of running by cooperation between the engine and the electric motor, and that includes an output limitation means for limiting torque output from the engine and/or the electric motor, and an automatic gear shifting means for shifting a gear number according to a variation in a vehicle speed, the automatic gear shifting means performing a control for temporarily reducing the torque output from the engine in neutral while a gear is transferred from a gear number before the shift to a gear number after the shift through neutral once, includes a step in which, when the gear shifting is performed during output limitation, the output limitation means performs a control for temporarily cancelling the output limitation in a process for returning the torque that has temporarily been reduced in neutral, and adding torque by the electric motor to torque of the engine.
Still another aspect of the present invention is directed to a computer program. The computer program causes an information processing apparatus to implement a function of the transmission control device according to the present invention.
Advantageous Effects of Invention
The present invention can improve the drivability in the gear shifting in a mode in which the torque of the engine is limited in response to the torque required by the driver.
BRIEF DESCRIPTION OF DRAWINGS
{FIG. 1 } It shows a block diagram for illustrating an exemplary structure of a hybrid vehicle according to an embodiment of the present invention.
{FIG. 2 } It shows a block diagram for illustrating an exemplary configuration of a function implemented in a hybrid ECU illustrated in FIG. 1 .
{FIG. 3 } It shows a flowchart for illustrating a process in an output limitation control unit and a transmission control unit illustrated in FIG. 2 .
{FIG. 4 } It shows a view for illustrating the relationship between the limited acceleration and the gear numbers and the variation in the torque in the gear shifting at the output limitation control in the output limitation control unit illustrated in FIG. 2 .
{FIG. 5 } It shows a view for describing the variation in the torque by the transmission control in the transmission control unit illustrated in FIG. 2 .
DESCRIPTION OF EMBODIMENTS
Hereinafter, a hybrid vehicle according to an embodiment of the present invention will be described with reference to FIGS. 1 to 5 .
FIG. 1 is a block diagram for illustrating an exemplary structure of a hybrid vehicle 1 . The hybrid vehicle 1 is an example of a vehicle. The hybrid vehicle 1 is driven by an engine (internal combustion engine) 10 and/or an electric motor 13 through a gear box having an automated mechanical/manual transmission. The hybrid vehicle 1 can performs an output limitation for limiting the torque output from the engine 10 and/or the electric motor 13 . Note that the automated mechanical/manual transmission is a transmission that can automatically shift the gears while having the same structure as a manual transmission.
The hybrid vehicle 1 includes the engine 10 , an engine Electronic Control Unit (ECU) 11 , a clutch 12 , the electric motor 13 , an inverter 14 , a battery 15 , a transmission 16 , a motor ECU 17 , a hybrid ECU 18 , a wheel 19 , and a key switch 20 . Note that the transmission 16 includes the above-mentioned automated mechanical/manual transmission and is operated by a shift unit 21 (not shown in the drawings) including a drive range (hereinafter, referred to as a D (Drive) range).
The engine 10 is an example of an internal combustion engine, and is controlled by the engine ECU 11 . The engine 10 internally combusts gasoline, light oil, Compressed Natural Gas (CNG), Liquefied Petroleum Gas (LPG), alternative fuel, or the like in order to generate power for rotating a shaft and transfer the generated power to the clutch 12 .
The engine ECU 11 is a computer working in coordination with the motor ECU 17 according to the instructions from the hybrid ECU 18 , and controls the engine 10 , for example, the amount of fuel injection and the valve timing. For example, the engine ECU 11 includes a Central Processing Unit (CPU), an Application Specific Integrated Circuit (ASIC), a microprocessor (micro-computer), a Digital Signal Processor (DSP), and the like, and internally has an operation unit, a memory, an Input/Output (I/O) port, and the like.
The clutch 12 is controlled by the hybrid ECU 18 , and transfers the shaft output from the engine 10 to the wheel 19 through the electric motor 13 and the transmission 16 . In other words, the clutch 12 mechanically connects the rotating shaft of the engine 10 to the rotating shaft of the electric motor 13 by the control of the hybrid ECU 18 in order to transfer the shaft output of the engine 10 to the electric motor 13 . On the other hand, the clutch 12 cuts the mechanical connection between the rotating shaft of the engine 10 and the rotating shaft of the electric motor 13 so that the shaft of the engine 10 and the rotating shaft of the electric motor 13 can rotate at different rotational speeds from each other.
For example, the clutch 12 mechanically connects the rotating shaft of the engine 10 to the rotating shaft of the electric motor 13 , for example, when the hybrid vehicle 1 runs by the power of the engine 10 and this causes the electric motor 13 to generate electric power, when the driving force of the electric motor 13 assists the engine 10 , and when the electric motor 13 starts the engine 10 .
Alternatively, for example, the clutch 12 cuts the mechanical connection between the rotating shaft of the engine 10 and the rotating shaft of the electric motor 13 when the engine 10 stops or is in an idling state and the hybrid vehicle 1 runs by the driving force of the electric motor 13 , and when the hybrid vehicle 1 decelerates or runs on the down grade and the electric motor 13 generates electric power (regenerates electric power) while the engine 10 stops or is in an idling state.
Note that the clutch 12 differs from the clutch operated by the driver's operation of a clutch pedal, and is operated by the control of the hybrid ECU 18 .
The electric motor 13 is a so-called motor generator that supplies a shaft output to the transmission 16 by generating the power for rotating the shaft using the electric power supplied from the inverter 14 , or that supplies electric power to the inverter 14 by generating the electric power using the power for rotating the shaft supplied from the transmission 16 . For example, when the hybrid vehicle 1 accelerates or runs at a constant speed, the electric motor 13 generates the power for rotating the shaft to supply the shaft output to the transmission 16 in order to cause the hybrid vehicle 1 to run in cooperation with the engine 10 . Further, the electric motor 13 works as an electric generator, for example, when the electric motor 13 is driven by the engine 10 , or when the hybrid vehicle 1 runs without power, for example, the hybrid vehicle 1 decelerates or runs on the down grade. In that case, electric power is generated by the power for rotating the shaft supplied from the transmission 16 and is supplied to the inverter 14 in order to charge the battery 15 .
The inverter 14 is controlled by the motor ECU 17 , and converts the direct voltage from the battery 15 into an alternating voltage or converts the alternating voltage from the electric motor 13 into a direct voltage. When the electric motor 13 generates power, the inverter 14 converts the direct voltage of the battery 15 into an alternating voltage and supplies the electric power to the electric motor 13 . When the electric motor 13 generates electric power, the inverter 14 converts the alternating voltage from the electric motor 13 into a direct voltage. In other words, in that case, the inverter 14 works as a rectifier and a voltage regulator for supplying a direct voltage to the battery 15 .
The battery 15 is a secondary cell capable of being charged and discharged. The battery 15 supplies electric power to the electric motor 13 through the inverter 14 when the electric motor 13 generates power. Alternatively, the battery 15 is charged with the electric power generated by the electric motor 13 when the electric motor 13 generates electric power.
The transmission 16 includes an automated mechanical/manual transmission (not shown in the drawings) that selects one of a plurality of gear ratios (change gear ratios) according to the shift instruction signal from the hybrid ECU 18 in order to shift the change gear ratios and transfer the gear-shifted power of the engine 10 and/or of the electric motor 13 to the wheel 19 . Alternatively, the transmission 16 transfers the power from the wheel 19 to the electric motor 13 , for example, when the vehicle decelerates or runs on the down grade. Note that the automated mechanical/manual transmission can also shift the gear position to a given gear number by the driver's hand operation.
The motor ECU 17 is a computer working in coordination with the engine ECU 11 according to the instructions from the hybrid ECU 18 , and controls the electric motor 13 by controlling the inverter 14 . For example, the motor ECU 17 includes a CPU, an ASIC, a microprocessor (micro-computer), a DSP, and the like, and internally has an operation unit, a memory, an I/O port, and the like.
The hybrid ECU 18 is an example of a computer. For hybrid driving, the hybrid ECU 18 obtains accelerator opening level information, brake operation information, vehicle speed information, the gear position information obtained from the transmission 16 , and the engine rotational speed information obtained from the engine ECU 11 in order to refer to the information, control the clutch 12 and supply the shift instruction signal in order to control the transmission 16 . For hybrid driving, the hybrid ECU 18 further gives the control instructions of the electric motor 13 and the inverter 14 to the motor ECU 17 based on the obtained SOC information on the battery 15 and other information, and gives the control instruction of the engine 10 to the engine ECU 11 . For example, the hybrid ECU 18 includes a CPU, an ASIC, a microprocessor (micro-computer), a DSP, and the like, and internally has an operation unit, a memory, an I/O port, and the like.
Note that a computer program to be executed by the hybrid ECU 18 can be installed on the hybrid ECU 18 that is a computer in advance by being stored in a non-volatile memory inside the hybrid ECU 18 in advance.
The engine ECU 11 , the motor ECU 17 , and the hybrid ECU 18 are connected to each other, for example, through a bus complying with the standard of the Control Area Network (CAN) or the like.
The wheel 19 is a drive wheel for transmitting the driving force to the road surface. Note that, although only a wheel 19 is illustrated in FIG. 1 , the hybrid vehicle 1 actually includes a plurality of the wheels 19 .
The key switch 20 is a switch that is turned ON/OFF, for example, by insertion of a key by the user at the start of drive. Turning ON the switch activates each unit of the hybrid vehicle 1 , and turning OFF the key switch 20 stops each unit of the hybrid vehicle 1 .
FIG. 2 is a block diagram for illustrating an exemplary configuration of a function implemented in the hybrid ECU 18 that executes a computer program. In other words, once the hybrid ECU 18 executes a computer program, an output limitation control unit 30 and a transmission control unit 31 are implemented.
The output limitation control unit 30 performs a control for setting an acceleration that is accepted at each of the gear numbers. This limits the acceleration to a predetermined acceleration according to the gear number and the vehicle speed, for example, even when the driver depresses the accelerator to rapidly accelerate the vehicle. Concretely, a target torque is limited in order to prevent acceleration equal to or more than the predetermined acceleration. This will be described in detail below with reference to FIG. 4 .
The transmission control unit 31 controls the automatic gear shifting of the hybrid vehicle 1 . Note that the transmission control unit 31 controls the automatic gear shifting during output limitation in cooperation with the output limitation control unit 30 .
Next, a process for the transmission control during output limitation that is performed in the hybrid ECU 18 executing a computer program will be described with reference to the flowchart illustrated in FIG. 3 . Note that the flow illustrated in FIG. 3 is one cycle of the process and the process is repeatedly performed as long as the key switch 20 is in the ON state.
At the “Start” of FIG. 3 , the key switch 20 is in the ON state and the hybrid ECU 18 executes a computer program and the output limitation control unit 30 and the transmission control unit 31 are implemented by the hybrid ECU 18 . The process goes to step S 1 . Note that the hybrid vehicle 1 runs in an output limitation mode at the “Start”.
In step S 1 , the transmission control unit 31 determines whether a condition for shifting gears is satisfied. For example, at an acceleration mode in which the vehicle speed of the hybrid vehicle 1 gradually increases or at a deceleration mode in which the vehicle speed of the hybrid vehicle 1 gradually decreases, the gear shifting is performed according to the increase or the decrease in the vehicle speed. When it is determined in step S 1 that the condition for shifting gears is satisfied, the process goes to step S 2 . On the other hand, when it is determined in step S 1 that the condition for shifting gears is not satisfied, step S 1 of the process is repeated.
The transmission control unit 31 reduces the torque of the engine 10 in order to shift the gear position into neutral in step S 2 , and shifts the gear position to a gear number according to the vehicle speed in step S 3 . At that time, the transmission control unit 31 temporarily disengages the clutch 12 and then reduces the torque of the engine 10 . After that, the transmission control unit 31 shifts the gear position into neutral in order to shift the gear number and then controls the clutch 12 to be engaged again.
In step S 4 , the transmission control unit 31 cancels the limitation of the torque and the process goes to step S 5 .
In step S 5 , the transmission control unit 31 causes the electric motor 13 to assist the engine 10 and the process goes to step S 6 .
In step S 6 , the transmission control unit 31 determines whether the torque of the engine 10 returns to the state before the gear shifting has been performed. When it is determined in step S 6 that the torque of the engine 10 returns to the state before the gear shifting has been performed, the process goes to step S 7 . On the other hand, when it is determined in step S 6 that the torque of the engine 10 does not return to the state before the gear shifting has been performed, the process goes back to step S 5 .
In step S 7 , the transmission control unit 31 causes the electric motor 13 to terminate assisting the engine 10 and terminates a cycle of the process.
Next, the relationship between the limited acceleration and the gear numbers and the variation in the torque of the engine 10 when the gear shifting is performed at the output limitation control in the output limitation control unit 30 will be described with reference to FIG. 4 . At the upper part of FIG. 4 , the limited accelerations when the gear number is set at a second speed, a third speed, and a fourth speed are illustrated with dashed lines and the acceleration of the hybrid vehicle 1 is illustrated with a solid line. At the lower part of FIG. 4 , the variation in the torque of the engine 10 of the hybrid vehicle 1 is illustrated while corresponding to the drawing of the upper part.
As illustrated at the upper part of FIG. 4 , the hybrid vehicle 1 accelerates at the second speed that is the starting gear number (a period T 1 ). After the acceleration has reached the limited acceleration of the second speed, the acceleration is regulated along the limited acceleration only while the acceleration reaches the limited acceleration of the second speed (a period T 2 ). When the gear shifting is performed at that time (a period T 3 ), the gear number is shifted into neutral and the torque of the engine 10 is temporarily reduced. After the gear shifting has been completed, the torque of the engine 10 returns and the vehicle accelerates to the limited acceleration of the third speed.
After the hybrid vehicle 1 has continued running at the limited acceleration of the third speed and the vehicle speed further has increased (a period T 4 ), the gear shifting is performed again (a period T 5 ). When the gear shifting is performed at that time (the period T 5 ), the gear number is shifted into neutral and the torque of the engine 10 is temporarily reduced. After the gear shifting has been completed, the torque of the engine 10 returns and the vehicle accelerates to the limited acceleration of the fourth speed. After that, the hybrid vehicle 1 runs at the limited acceleration of the fourth speed (a period T 6 ).
FIG. 5 enlarges the torque of the engine 10 in detail when the gear shifting is performed in FIG. 4 (the period T 3 or the period T 5 ). FIG. 5 illustrates a request torque tr 1 by the driver, a limited torque tr 2 by the output limitation control, a target torque tr 3 , a limited torque at gear shifting tr 4 , and an actual torque tr 5 of the engine 10 , and a normal torque at gear shifting tr 6 as a comparison example. FIG. 5 further illustrates an assisting region A (shaded region) in which the electric motor 13 assists the engine 10 , an unstable region D of the engine torque, and a return rate r.
Note that a knocking possibly occurs at the unstable region D of the engine torque depending on the characteristics of the engine 10 . Thus, the engine torque preferably comes out of the unstable region D as soon as possible.
When the output limitation is not performed, the torque of the engine 10 starts to return to the required torque tr 1 as illustrated with the normal torque at gear shifting tr 6 because the required torque tr 1 is equal to the target torque. On the other hand, when the output limitation is performed, the torque of the engine 10 starts to return to the target torque tr 3 that has been set according to the limited acceleration. When the accelerator is depressed for a rapid acceleration, the target torque tr 3 becomes smaller than the required torque tr 1 according to the acceleration control as illustrated in FIG. 5 .
As described above, when the target torque tr 3 becomes smaller than the required torque tr 1 , the difference between the actual torque and the target torque becomes smaller in comparison with the case in which the output limitation is not performed. Thus, a P (proportion) I (integration) control according to the difference is performed, so that the rate until the return is completed becomes small. As a result, the feeling of acceleration decreases and the drivability is aggravated. Accordingly, it takes more time until the torque returns to the target torque in comparison with the case in which the output limitation is not performed. Thus, the time when the actual torque is in the unstable region D of the engine torque becomes long, so that the engine becomes unstable. As described above, the rise of the torque of the engine 10 becomes slower in comparison with the case without limitation so that the actual torque tr 5 of the engine cannot reach the target torque tr 3 within the return rate r.
In light of the foregoing, for example, the transmission control unit 31 causes the electric motor 13 to assist the engine 10 in order to enable the torque to return to the target torque in the same time as in the case in which the output limitation is not performed.
Here, on the assumption that a T is the actual torque of the engine 10 , a TI is the proportion torque, a TP is the integration torque, a Tref is the target torque, a ΔT is the difference between the target torque and the actual torque, and an I is the gain in the proportion control,
T=TI+TP (1)
TI=ΔT·I (2)
Δ T=Tref −T (3)
can be expressed. The actual torque T is PI-controlled as shown in the expression (1). The TI is obtained by multiplying the difference ΔT between the actual torque T and the target torque (the expression 3) by the I gain as shown in the (expression 2). Then, the I gain is set as a large value at the timing when the actual torque T returns to the target torque Tref. As a result, to obtain a desired T, the torque of the electric motor 13 is added to the torque of the engine 10 and the electric motor 13 assists the engine 10 . Further, when the gear number is shifted into neutral at that time, the gain I is changed. After that, when the fact that the gear shifting has been completed is notified from the transmission 16 , the gain I returns to the original. As an example of the variations in the gain I, the gain I when the torque returns from neutral is ten times as much as the gain I when the gear shifting is completed.
This enables the torque to reach the target torque tr 3 in the period of the return rate r as described with the limited torque at gear shifting tr 4 even when the output limitation is performed. At that time, the region in which the electric motor 13 assists the engine 10 corresponds to the assisting region A. Note that increasing the torque of the engine 10 also enables the actual torque tr 5 of the engine to reach the target torque tr 3 in the period of the return rate r. As described above, applying the control only by the engine 10 enables the present control to be applied to a vehicle other than a hybrid vehicle. Such a control only by the engine 10 is preferably not applied in the present embodiment because the control is performed for the hybrid vehicle 1 and the control only by the engine 10 causes poor fuel efficiency.
(Effect)
In the hybrid vehicle 1 , when the gear shifting is performed while the output limitation control unit 30 performs the output limitation, the output limitation is temporarily cancelled during the process for returning the torque that has been reduced in neutral. Further, the assistance is controlled in order to add the torque by the electric motor 13 to the torque of the engine 10 . Thus, the drivability when the gear shifting is performed can be improved.
(Other Embodiments)
The above-mentioned return rate r can variably be set according to the gross weight of the hybrid vehicle 1 or the degree of the upgrade surface on which the hybrid vehicle 1 runs. For example, when the clutch 12 is temporarily disengaged and the gear position is shifted into neutral for gear shifting while the gross weight of the hybrid vehicle 1 is large, or while the upgrade surface on which the hybrid vehicle 1 runs is steep, the amount of the deceleration is larger in comparison with the case when the gross weight of the hybrid vehicle 1 is small, or when the surface on which the hybrid vehicle 1 runs is flat. In light of the foregoing, the return rate r is shortened when the gross weight of the hybrid vehicle 1 is large, or when the upgrade surface on which the hybrid vehicle 1 runs is steep in comparison with the case when the gross weight of the hybrid vehicle 1 is small, or when the surface on which the hybrid vehicle 1 runs is flat. This causes the rise of the torque to be rapid after the clutch 12 has been engaged again after the gear number has been changed, so that the feeling of decreasing speed with the gear shifting can be reduced.
To change the return rate r, it is preferable that a threshold is provided to the gross weight of the hybrid vehicle 1 or to the upgrade surface on which the hybrid vehicle 1 runs and the return rate r is shortened when the gross weight or the upgrade surface exceeds the threshold. Note that it is preferable to monitor both of the gross weight of the hybrid vehicle 1 and the upgrade surface on which the hybrid vehicle 1 runs and change the return rate r when one of the gross weight and the upgrade exceeds the threshold. Alternatively, both of the gross weight of the hybrid vehicle 1 and the upgrade surface on which the hybrid vehicle 1 runs are monitored, and the return rate r can be changed in two stages when one of the gross weight and the upgrade surface exceeds the threshold and when both of the gross weight and the upgrade surface exceed the thresholds. It is preferable in that case that the return rate r when both of the gross weight of the hybrid vehicle 1 and the upgrade surface on which the hybrid vehicle 1 runs exceed the thresholds is further shorter than the return rate r when one of the gross weight and the upgrade exceeds the threshold.
Further, although the engine 10 has been described as an internal combustion engine, the engine 10 can also be a heat engine including an external combustion engine.
While the computer program executed by the hybrid ECU 18 is installed on the hybrid ECU 18 in advance in the description above, the computer program can be installed on the hybrid ECU 18 as a computer by attaching removable media recording the computer program (storing the computer program), for example, to a drive (not shown in the drawings) and storing the computer program read from the removable media in a non-volatile memory inside the hybrid ECU 18 , or receiving, by a communication unit (not shown in the drawings), a computer program transmitted through a wired or wireless transmission medium and storing the computer program in a non-volatile memory inside the hybrid ECU 18 .
Further, each ECU can be implemented by an ECU combining each of the ECUs. Alternatively, an ECU can newly be provided by the subdivision of the function of each ECU.
Note that the computer program executed by the computer can be for performing the process in chronological order according to the order described herein or can be for performing the process in parallel or at the necessary timing, for example, when the computer program is invoked.
Further, the embodiments of the present invention are not limited to the above-mentioned embodiments, and can be variously modified without departing from the gist of the invention.
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To improve the drivability of an automobile at the time of transmission which restricts a torque of an engine, a hybrid automobile is structured which performs transmission control for performing control so that an output restriction is temporarily released in a step of restoring a torque that is reduced once in neutral at the time of transmission during the output restriction by an output restriction control unit and a torque by a motor is added to the torque of the engine.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to lubricating compositions. In particular, the present invention relates to a lubricant composition obtained by compounding molybdenum dithiocarbamate, molybdenum dithiophosphate, and/or a molybdenum amine compound; and a (poly)glycerol ether and/or a (poly)oxyalkylene glycol monoalkyl ether, in a base oil. More particularly, the present invention relates to a lubricating oil composition which exhibits excellent stability to hydrolysis and excellent friction reduction even after deterioration with water, and a grease which is used for universal joints including constant velocity joints (CVJ) for automobiles, constant velocity gears, and transmission gears, and which has excellent friction and abrasion properties.
2. Description of the Related Art
The automotive field is today confronted with strict fuel regulations, and exhaust gas regulations, etc. against the background of environmental pollution, e.g. global greenhouse effect, air pollution, and acid rain, and in order to preserve limited petroleum resources from exhaustive use. Improvements in mileage are the most effective way to respond to such regulations at present.
Improvements in engine oil, such as low viscosity engine oils and the addition of friction modifiers, as well as improvements in automobiles themselves, e.g. light weight vehicles and improved engines, are important means for achieving low fuel consumption in the automotive field. Engine oil acts as a lubricant between pistons and liners, and friction loss can be reduced by decreasing the viscosity of the engine oil due to the high fluid lubrication in this portion. However, the decreases in oil viscosity in recent years have also created such problems as deteriorated sealing properties and accelerated wear. Engine oil also plays an important role in the valve train and bearings. Low viscosity oil will cause increased wear due to mixed lubrication or boundary lubrication in these systems. Friction modifiers and extreme pressure agents are added to the oil to decrease friction and prevent wear.
Generally used friction modifiers include, for example, higher fatty acids, e.g. oleic acid and stearic acid; higher alcohols, e.g. oleyl alcohol; esters; amines; sulfide oils; chlorinated oils; and organic molybdenum compounds. Generally used extreme pressure agents include, for example, sulfide oils; sulfur compounds, e.g. sulfides; phosphorous compounds; and organic metals e.g. zinc dithiophosphate (ZnDTP).
For example, Japanese Laid-Open Patent No. 59-25890 discloses glycerin monoalkyl ether or glycerin monoalkenyl ether as the friction modifier, as well as a common lubricant composition produced by combining ZnDTP with an ash-free detergent-dispersant.
The addition of organic molybdenum friction modifiers providing low friction in mixed or boundary lubrication is inevitable in order to solve all the problems associated with the lowering of lubricating oil viscosity. Japanese Laid-Open Patent No. 5-279686 proposes an improvement in frictional properties without deterioration in other properties such as abrasion resistance by compounding an organic molybdenum compound; a fatty acid ester; a metallic detergent, such as calcium sulfonate, magnesium sulfonate, calcium phenate, and magnesium phenate; an ash-free detergent-dispersant, such as benzylamine and its boron derivative, and alkenylsuccinic imide and its boron derivative; and wear improvers such as ZnDTP and zinc dithiocarbamate (ZnDTC).
Alternatively, Japanese Laid-Open Patent No. 5-311186 discloses a drastic decrease in the friction coefficient of lubricating oil which contains a combination of a metal dithiocarbamate and an oil-soluble amine; sulfoxy molybdenum dithiocarbamate and/or sulfoxy molybdenum organophosphorodithioate; and a fatty acid ester and/or organic amides, in a selected ratio.
However, neither of the compositions disclosed in Japanese Laid-Open Patent Nos. 5-279686 and 5-311186 show reduced friction when oil contains water even with the addition of the molybdenum compound.
Inclusion of water in an engine oil formed during fuel combustion is inevitable. In particular, when engine oil is not heated, that is during repeated short distance operation cycles water content in the engine oil increases as the water does not evaporate. Water causes not only deterioration of the additives but also the activation of blow-by gas, resulting in significantly adverse effects on the engine oil. Thus, the development of an oil which can maintain decreased friction while maintaining fuel saving performance with little deterioration even when water is included has been needed.
Recently, CVJs have been widely employed for front engine front drive vehicles, four wheel drive vehicles, and front engine rear drive vehicles with independent suspension. CVJs are used to transmit power from the engine to the wheels, and the power must be smoothly transmitted even during steering. Thus, a CVJ generally consists of a combination of a plunging-type joint at the engine side capable of sliding in the axial direction and a fixed-type joint fixed in the axial direction at the wheel side. Since the sliding friction in the rotational direction occurs through the rolling-sliding motion during the reciprocating motion in the plunging-type joint, various noises and vibrations, e.g. vibrations during idling in an automatic transmission vehicle, lateral vibration during starting and accelerating, beat oscillations at certain speeds, and booming occur. Decreased vibration is an important issue to be solved for the development of more comfortable and quieter vehicles. Thus, not only has the joint itself been improved to decrease such vibrations, but the grease filled in the joint as well.
As there is a correlation between the vibration and the friction coefficient, and further as reduced fuel consumption is increasingly demanded, greases for providing decreased friction are being sought.
Molybdenum disulfide, sulfur-phosphorous additives, and lead additives have been conventionally used in grease for CVJs. Recently, organic molybdenum compounds have been used instead of the above additives, in order to produce grease exhibiting lower vibration or lower friction. Japanese Laid-Open Patent No. 6-184583 discloses a grease composition for CVJs comprising a urea grease, molybdenum dithiophosphate, molybdenum dithiocarbamate, and ZnDTC. Additionally, Japanese Laid-Open Patent No. 4-178499 discloses a grease composition for CVJs comprising a urea thickener, sulfurized molybdenum dialkyldithiocabamate, zinc dithiophosphate, and sorbitan fatty acid esters.
Although, long drain lubricating oils are now desirable with the aim of achieving a maintanance free lubricating composition, it is becoming an important problem to maintain this in addition to reduced fuel consumption. Engine oils undergo the most severe oxidative deterioration among lubricating oils, and the deterioration starts with the running of the vehicles. Additives also deteriorate along with this oil deterioration. Thus, improvements in the additives are also essential for maintaining the fuel saving properties of lubricating oil. That is, because the use of oil-soluble molybdenum compounds is essential for fuel savings, it is even more important to effectively draw out and maintain the properties of the molybdenum compounds.
Further, the friction of the grease compositions set forth above is not satisfactory and must be further lowered. Demand on greases has shifted to increasingly severe site conditions due to the decreased quantity of grease fillable in smaller and light weight CVJs, higher power output and higher vehicle speeds. Thus, low frictional performance is required for such greases in addition to high durability and high friction resistance.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a lubricating composition suitable for lubricating oil or grease.
In accordance with the present invention, a lubricating composition comprising:
a component (A) comprising at least one molybdenum compound selected from the group consisting of sulfurized oxymolybdenum dithiocarbamates (hereinafter "MoDTC") represented by the following general formula: ##STR1## (wherein R 1 , R 2 , R 3 and R 4 are independent hydrocarbly groups, and X 1 represents an oxygen or sulfur atom);
sulfurized oxymolybdenum dithiophosphates (hereinafter "MoDTP") represented by the following general formula: ##STR2## (wherein R 5 , R 6 , R 7 and R 8 are independent hydrocarbly groups, and X 2 represents an oxygen or sulfur atom); and
molybdenum amine compounds (hereinafter "MoAm") obtained by reacting a hexavalent molybdenum compound with an amine compound represented by the following general formula: ##STR3## (wherein both R 9 and R 10 represent a hydrogen atom and/or hydrocarbyl group, and R 9 and R 10 are not hydrogen atoms at the same time): and
a component (B) comprising a (poly)glycerin ether represented by the following general formula: ##STR4## (wherein both R 11 and R 12 represent a hydrogen atom and/or hydrocarbyl group, R 11 and R 12 are not hydrogen atoms at the same time, and n ranges from 1 to 10); and/or
a (poly)oxyalkylene glycol monoalkyl ether represented by the following general formula:
R.sup.13 O--(R.sup.14 --O--).sub.m H (5)
(wherein R 13 represents a hydrocarbyl group, R 14 represents an alkylene group, and m ranges from 1 to 10).
A second embodiment of the present invention provides a lubricating composition comprising:
a component (A) comprising at least one molybdenum compound selected from the group consisting of MoDTC represented by the following general formula: ##STR5## (wherein R 1 , R 2 , R 3 , R 4 and X 1 have the same meanings as described above);
MoDTP represented by the following general formula: ##STR6## (wherein R 5 , R 6 , R 7 , R 8 and X 2 have the same meanings as described above); and
MoAm obtained by reacting a hexavalent molybdenum compound with an amine compound represented by the following general formula: ##STR7## (wherein R 9 and R 10 have the same meanings as described above): a component (B) comprising a (poly)glycerin ether represented by the following general formula: ##STR8## (wherein R 11 , R 12 , and n have the same meanings as described above); and/or
a (poly)oxyalkylene glycol monoalkyl ether represented by the following general formula:
R.sup.13 O--(R.sup.14 --O--).sub.m H (5)
(wherein R 13 , R 14 and m have the same meanings as described above): and
a component (C) comprising a ZnDTP represented by the following general formula: ##STR9## (wherein a represents a figure of zero or one-third, and both R 15 and R 16 represent a hydrocarbyl group); and/or
a zinc dithiocarbamates (hereinafter "ZnDTC") represented by the following general formula: ##STR10## (wherein both R 17 and R 18 represent a hydrocarbyl group).
DESCRIPTION OF PREFERRED EMBODIMENT
The molybdenum compounds as the essential component (A) in the lubricating composition according to the present invention include MoDTCs represented by the general formula (1) set forth above, MoDTPs represented by the general formula (2), and MoAms. These molybdenum compounds can be used alone or in combination.
In general formulae (1) to (3), R 1 through R 10 are independent hydrocarbyl groups, e.g. alkyl, alkenyl, alkylaryl, cycloalkyl, cycloalkenyl group, or the like.
Examples of alkyl groups include methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl, pentyl, isopentyl, neopentyl, tert-pentyl, hexyl, heptyl, octyl, 2-ethylhexyl, nonyl, decyl, undecyl, dodecyl, tridecyl, isotridecyl, myristyl, palmityl, stearyl, eicosyl, docosyl, tetracosyl, triacontyl, 2-octyldodecyl, 2-dodecylhexadecyl, 2-tetradecyloctadecyl, and monomethyl- branched isostearyl groups.
Examples of alkenyl groups include vinyl, allyl, propenyl, isopropenyl, butenyl, isobutenyl, pentenyl, isopentenyl, hexenyl, heptenyl, octenyl, nonenyl, decenyl, undecenyl, dodecenyl, tetradecenyl, and oleyl groups.
Examples of alkylaryl groups include phenyl, tolyl, xylyl, cumenyl, mesityl, benzyl, phenethyl, styryl, cinnamyl, benzhydryl, trityl, ethylphenyl, propylphenyl, butylphenyl, pentylphenyl, hexylphenyl, heptylphenyl, octylphenyl, nonylphenyl, α-naphthyl, and β-naphthyl groups.
Examples of cycloalkyl and cycloalkenyl groups include cyclopentyl, cyclohexyl, cyclobutyl, methylcyclopentyl, methylcyclohexyl, methylcycloheptyl, cyclopentenyl, cyclohexenyl, cycloheptenyl, methylcyclopentenyl, methylcyclohexenyl, and methylcycloheptenyl.
Both R 9 and R 10 can be a hydrogen atom, but cannot be a hydrogen atom at the same time.
R 1 through R 10 may be the same or different from each other. Thus, R 1 through R 4 , R 5 through R 8 , and R 9 through R 10 may be the same or different from each other. When R 1 through R 4 are different from each other, the life of the lubricating composition can be prolonged.
When the lubricating compositions according to the present invention are compounded in a conventionally used base oil for lubricating oil as a lubricating oil composition, R 1 through R 4 in MoDTC represented by the general formula (1) are each preferably an alkyl group having 8 to 13 carbon atoms, R 5 through R 8 in MoDTP represented by the general formula (2) are each preferably an alkyl group having 6 to 13 carbon atoms, and R 9 through R 10 in MoAm represented by the general formula (3) are each preferably an alkyl group having 6 to 18 carbon atoms.
The lubricating composition according to the present invention can also be compounded in a base grease comprising a base oil and a thickener. In such a case, R 1 through R 4 , R 5 through R 8 , and R 9 and R 10 are each preferably an alkyl group having 1 to 16 carbon atoms, more preferably 2 to 13 carbon atoms, and most preferably 2 to 8 carbon atoms.
Both X 1 and X 2 in MoDTC represented by the general formula (1) and MoDTP represented by the general formula (2) may each be a sulphur or oxygen atom. Although both X 1 and X 2 can be only sulfur atoms or only oxygen atoms, it is preferable that the sulfur/oxygen atomic ratio ranges from 1/3 to 3/1 in view of lubricating properties and corrosion resistance.
The MoDTC represented by the general formula (1) used in the present invention can be preferably synthesized by the method described in, for example, Japanese Patent Publication No. 56-12638, in which the MoDTC is obtained by reacting molybdenum trioxide or a molybdate with an alkaline metal sulfide or alkaline metal hydrosulfide, and then by reacting the resultant with carbon dioxide and a secondary amine at an adequate temperature.
The MoDTP represented by the general formula (2) used in the present invention can be preferably synthesized by the method described in, for example, Japanese Patent Laid-Open Nos. 61-87690 and 61-106587, in which the MoDTP is obtained by reacting molybdenum trioxide or a molybdate with an alkaline metal sulfide or alkaline metal hydrosulfide, and then by reacting the resultant with P 2 S 5 and a secondary alcohol at an adequate temperature.
The MoAm used in the present invention is a salt of a molybdic acid (H 2 MoO 4 ) with a primary or secondary amine, and is preferably synthesized by the method disclosed in, for example, Japanese Patent Laid-Open No. 61-285293, in which the MoAm is obtained by reacting a hexavalent molybdenum compound, e.g. molybdenum trioxide or a molybdate, with a primary or secondary amine represented by the following general formula (3) at a temperature ranging from room temperature to 100° C.: ##STR11##
Although the chemical formula of the MoAm obtained by the reaction set forth above is not clear, it will probably be as follows: ##STR12## (wherein b is within a range of 0.95≦b≦1.05, and c is within a range of 0≦c≦1).
When a base oil for lubricating oil is used in the lubricating composition according to the present invention, the molybdenum compounds as component (A) may be at least one compound of MoDTC, MoDTP, and MoAm. When two or more compounds are used together, at least one compound among them is preferably MoDTC. Although the content of the added molybdenum compound is not limited, it is preferably 0.001 to 1 wt % as reduced molybdenum amount, more preferably 0.005 to 0.5 wt %, and most preferably 0.01 to 0.1 wt % of the base oil, because an extremely low content does not sufficiently lower friction, whereas an excessive content causes slag formation and corrosion.
When a base grease is used in the lubricating composition according to the present invention, the molybdenum compound as component (A) may be at least one compound of MoDTC, MoDTP, and MoAm. When two or more compounds are used together, at least one compound among them is preferably MoDTC. Although the content of the added molybdenum compound is not limited, it is preferably 0.01 to 10 wt %, and more preferably 1 to 5 wt % of the base grease, because an extremely low content does not sufficiently lower friction, whereas an excessive content does not further improve grease properties, but may be harmful to the grease.
In the lubricating composition according to the present invention, the compound represented by the general formula (4) as component (B) is a (poly)glycerin ether. In the general formula (4), R 11 and R 12 are each a hydrogen atom or a hydrocarbyl group, both may be the same or different from each other, and both are preferably alkyl, alkenyl, or alkylaryl groups, similar to R 1 through R 10 as described above, but both R 11 and R 12 cannot be hydrogen atoms at the same time.
R 11 and R 12 are each preferably a hydrogen atom or a straight chain or branched chain alkyl or alkenyl group having 1 to 20 carbon atoms, and more preferably a straight chain or branched chain alkyl or alkenyl group having 12 to 20 carbon atoms. In particular, a straight chain alkyl or alkenyl group, e.g. a lauryl, oleyl, stearyl group, are preferable.
Further, n ranges from 1 to 10, in other words, the compound may be a monoglycerin ether or polyglycerin ether. As a compound having a larger n is difficult to synthesize, n ranges preferably from 1 to 3.
The compound represented by the general formula (5) is a (poly)oxyalkyleneglycol ether. R 13 in the general formula (5) is a hydrocarbyl group, preferably a straight chain or branched chain alkyl, alkenyl, or alkylaryl group, similar to R 1 through R 10 as described above, and more preferably a linear group. In detail, an alkyl or alkenyl group having 1 to 20 carbon atoms is preferable, an alkyl or alkenyl group having 12 to 20 carbon atoms is more preferable, and a lauryl or oleyl group is the most preferable.
R 14 is an alkylene group, preferably an alkylene group having 2 to 4 carbon atoms, e.g. an ethylene, propylene, or butylene group. The (R 12 --O) m portion is obtained by adding ethylene oxide, propylene oxide, butylene oxide or the like. An addition reaction of alkylene oxide may be homopolymerization, or random or block copolymerization.
Further, m ranges from 1 to 10, in other words, the compound may be a monooxyalkyleneglycol ether or polyoxyalkyleneglycol ether. As a the compound having a larger m decreases the solubility to oil and thermal stability, m is preferably 1 to 5, and more preferably 2 to 4.
When a base oil for lubricating oil is used in the lubricating composition according to the present invention, (poly)glycerin ethers and (poly)oxyalkyleneglycol ethers as the component (B) may be used alone or in combinations of at least two kinds. Although the content of the component (B) is not limited, it is preferably 0.01 to 5 wt %, and more preferably 0.1 to 1 wt % of the base oil for lubricating oil, because an extremely low content does not sufficiently lower friction when water is included, whereas an excessive content decreases the solubility to oil.
Both (poly)glycerin ether represented by the general formula (4) and (poly)oxyalkylene glycol ether represented by the general formula (5) compounded in the base oil for lubricating oil are not hydrolyzed with water included in the lubricating oil. Thus, such additives are superior to any ester-type additives readily hydrolyzed, and exhibit excellent lubricating properties when they are used with molybdenum compounds.
When a base grease is used in the lubricating composition according to the present invention, (poly)glycerin ethers and (poly)oxyalkyleneglycol ethers as the component (B) may be used alone or in combinations of at least two kinds. Although the content of the component (B) is not limited, it is preferably 0.01 to 10 wt %, and more preferably 1 to 5 wt % of the base grease, because an extremely low content does not sufficiently lower friction, whereas an excessive content does not further improve grease properties, but may be harmful to the base grease.
Both (poly)glycerin ether represented by the general formula (4) and (poly)oxyalkylene glycol ether represented by the general formula (5) compounded in the base grease exhibit excellent lubricating properties when they are used with molybdenum compounds. Additionally, the lubricating composition further comprising ZnDTP and/or ZnDTC exhibits even more improved lubricating properties.
In ZnDTP represented by the general formula (6) as the component (C) usable in the lubricating oil and grease compositions according to the present invention, both R 15 and R 16 are each a hydrocarbyl group, both may be the same or different from each other, and preferably an alkyl, alkenyl or alkylaryl group. Among them, an alkyl group having 3 to 14 carbon atoms is more preferable.
In R 15 and R 16 in at least one ZnDTP used, 60% or more of the hydrocarbyl group is preferably at least one primary alkyl group, and 40% or less of the hydrocarbyl group may be secondary and/or tertiary alkyl groups.
The prefix a is zero or one-third. The compound is termed neutral ZnDTP when a=0, and termed basic ZnDTP when a=1/3 (one-third).
The ZnDTP used in the lubricating oil and grease compositions according to the present invention can be synthesized by the method described in, for example, Japanese Patent Publication No. 48-37251, in which the compound is obtained by synthesizing an alkyl-substituted dithiophosphoric acid through the reaction of P 2 S 5 with a predetermined alcohol, and by neutralizing or alkalifying the resultant with zinc oxide to form a zinc salt of the resultant.
The ZnDTPs represented by the general formula (6) as the component (C) can be used alone or in combinations of at least two kinds, in the lubricating oil composition of the present invention. Although the content of the component (C) is not limited, it is preferably 0.001 to 1 wt % as reduced phosphorus amount, more preferably 0.005 to 0.5 wt %, and most preferably 0.01 to 0.15 wt % of the base oil for lubricating oil, because an extremely low content does not have sufficient extreme pressure effect, whereas an excessive content deactivates the catalyst in an exhaust gas catalytic converter due to phosphorus in the ZnDTP.
The ZnDTPs represented by the general formula (6) as the component (C) can be used alone or in combinations of at least two kinds, in the grease composition of the present invention. Although the content of the component (C) is not limited, it is preferably 0.01 to 10 wt %, and more preferably 1 to 5 wt % of the base grease, because an extremely low content does not have sufficient extreme pressure effect, whereas an excessive content decreases lubricating properties.
The ZnDTCs represented by the general formula (7) as the component (C) can also be used in the lubricating oil and grease compositions of the present invention. Both R 17 and R 18 in the ZnDTC are each a hydrocarbyl group, and both may be the same or different from each other. Such hydrocarbyl groups preferably include alkyl, alkenyl, and alkylaryl groups similar to R 1 through R 10 as described above, and more preferably alkyl groups having 3 to 14 carbon atoms.
The ZnDTCs represented by the general formula (7) as the component (C) can be used alone or in combinations of at least two kinds, in the lubricating oil and grease compositions of the present invention. Although the content of the component (C) is not limited, it is preferably 0.01 to 15 wt %, and more preferably 1 to 5 wt % of the base oil for lubricating oil or base grease, because an extremely low content does not have sufficient extreme pressure effect, whereas an excessive content decreases lubricating properties.
The lubricating composition according to the present invention contains the components (A) and (B) described above as essential constituents, and may further contain the optional component (C), the base oil for lubricating oil and base grease.
Examples of usable base oil for lubricating oil include mineral oils and synthetic oils. The term mineral oils used here means those obtained from crude oil through separation, distillation and purification, and includes paraffinic oils, naphthenic oils, their hydrogenated oils, their purified oils, and hydrogenolyzed VHVI oils. The term synthetic oils used here means chemically synthesized lubricating oils, and include poly-α-olefins, polyisobutylene or polybutene, diesters, polyol esters, phosphate esters, silicate esters, polyalkyleneglycols, polyphenylethers, silicones, fluorides, alkylbenzene and the like.
The base grease that can be used in the present invention comprises a base oil and a thickener. Examples of thickeners include metallic soaps containing metallic components, such as aluminum, barium, calcium, lithium, and sodium; complex soaps, such as a lithium complex, calcium complex, and aluminum complex; organic non-soap thickeners, such as urea, diurea, triurea, tetraurea, arylureas, and terephthalamates; and inorganic non-soap thickeners, such as bentonite, and silica aero gels. Among them, urea is preferably used. Such thickeners can be used alone or in combination. Although the content of the thickener is not limited, it is preferably 3 to 40 wt %, and more preferably 5 to 20 wt % of the base grease comprising the base oil and the thickener.
Examples of usable base oils in the grease composition in accordance with the present invention include various base oils for lubricating oil, e.g. mineral lubricating base oils, synthetic lubricating base oils, and mixtures thereof. Mineral oils are generally prepared by purifying crude oil through solvent and/or hydrogenation purification processes, as well as other purification processes. Examples of suitable synthetic lubricating base oils include α-olefinic polymers having 3 to 12 carbon atoms, e.g. α-olefinic oligomers; dialkyl diesters having 4 to 12 carbon atoms, e.g. sebacates, such as 2-ethylhexyl sebacate and dioctyl sebacate, azelates, and adipates; polyol esters, e.g. esters obtained by the reaction of trimethylolpropane or pentaerythritol with monobasic acids having 3 to 12 carbon atoms; alkylbenzenes having 9 to 40 carbon atoms; polyglycols obtained by condensation of butyl alcohol with propylene oxide; and phenyl ethers having 2 to 5 ether sequences and 3 to 6 phenylene segments. The mineral and synthetic lubricating base oils can be used alone or in combination. The amount of the base oil to be compounded is adequately determined depending on required properties and is generally 70 to 95 wt % of the base grease comprising the base oil and the thickener.
Any well known additives can be incorporated within the object in accordance with the present invention, if necessary. In the lubricating oil composition, examples of such additives include friction reducers, e.g. higher fatty acids, higher alcohols, amines, and esters; sulfur-containing, chlorine-containing, phosphorus-containing, and organometallic extreme pressure agents; phenolic and amine antioxidants; neutral or highly basic alkaline earth metal sulfonates; carboxylate detergents; dispersants, e.g. succinic imide and benzyl amine; viscosity index improvers, e.g. high molecular weight poly(meth)acrylates, polyisobutylenes, polystyrenes, ethylene-propylene copolymers, and styrene-isobutylene copolymers; ester and silicone antifoaming agents; corrosion inhibitors; and flow-point decreasers. These additives may be used in an amount within usual usage.
On the other hand, in the grease composition, examples of additives include friction reducers, e.g. higher fatty acids, higher alcohols, amines, and esters; sulfur-, chlorine-, phosphorus-, and lead-containing extreme pressure agents; phenolic, amine, sulfur-containing and selenium-containing antioxidants; corrosion inhibitors, e.g. long-chain carboxylic acids and their derivatives, sulfonate salts, amines, and phosphate esters; solid lubricants, e.g. graphite, molybdenum disulfide, polyethylene, polytetrafluoroethylene (PTFE), and boron nitride; and other miscellaneous additives, e.g. flow-point reducers, viscosity index improvers, tackifiers, structure stabilizers, detergent-dispersants, antiseptic agents, antifoaming agents, ester friction reducers, coloring agents, sulfur- or chlorine-containing and organometallic extreme pressure agents, neutral and highly basic alkaline earth metal detergents, antistatic agents, emulsifiers, and demulsifiers. These additives may be used in an amount within usual usage.
The lubricating oil compositions in accordance with the present invention can be used as lubricating oils for internal combustion engines, e.g. vehicle engines including automobile engines, two cycle engines, aircraft engines, seacraft engines, and locomotive engines (such engines including gasoline, diesel, gas, turbine engines); automobile transmission fluids; trans-axle lubricants; gear lubricants, and metal working lubricants.
The lubricating grease composition in accordance with the present invention can be preferably used for universal joints including constant velocity joints, constant velocity gears, and speed change gears.
As described above, the present invention can provide a lubricating oil composition exhibiting a continuous friction decreasing effect against the deterioration due to included water by means of the combination of a base oil for lubricating oil, a molybdenum compound, a (poly)glycerin ether and/or (poly)oxyalkylene glycol ether, and optionally ZnDTP and/or ZnDTC.
Additionally, the present invention can provide a grease composition exhibiting excellent friction and abrasion characteristics by means of the combination of a base grease, a molybdenum compound, a (poly)glycerin ether and/or (poly)oxyalkylene glycol ether, and optionally ZnDTP and/or ZnDTC.
EXAMPLES
The lubricating composition in accordance with the present invention will now be explained in detail based on the following illustrative examples.
Materials used in Inventive products and Comparative products are as follows:
Base oil for lubricating oil: Mineral oil type high VI oil obtained by hydrogenolysis of raw mineral oil from crude oil. Kinematic viscosity: 4.1 cSt at 100° C., and VI: 126.
Base Grease: An aliphatic amine-type urea compound as a thickener was homogeneously dispersed in a purified mineral oil having a viscosity of 15 cSt at 100° C., so that the final viscosity became 287 cSt at 25° C.
Component (A)
Mo Compound 1: MoDTP in which R 5 through R 8 are each an 2-ethylhexyl group, and the S/O ratio in X 2 is 2.2 in the general formula (2).
Mo Compound 2: MoDTC in which R 1 through R 4 are each an 2-ethylhexyl group, and the S/O ratio in X 1 is 2.2 in the general formula (1).
Mo Compound 3: MoDTC in which R 1 through R 4 are each 2-ethylhexyl or isotridecyl groups, the ratio of the 2-ethylhexyl group to the isotridecyl group is 1:1, and the S/O ratio in X 1 is 2.2 in the general formula (1).
Mo Compound 4: MoAm compound synthesized by the following process:
In a nitrogen flow, one mole of molybdenum trioxide was dispersed into 540 ml of water, and then 2 mole of ditridecylamine was dropped into the dispersion in one hour and further aged for one hour while maintaining the temperature at 50° to 60° C. A light blue oily amine salt of molybdate (MoAm) was obtained by removing the aqueous layer, in which R 9 and R 10 are tridecyl groups. Said MoAm is a mixture wherein b is 0.95 to 1.05, and c is 0 to 1, in the general formula (8). The values of b and c were estimated.
Mo Compound 5: MoDTC in which R 1 through R 4 are n-butyl groups, and the S/O ratio in X 1 is 2.2 in the general formula (1).
Component (B)
Glycerin Ether 1: Glycerin monooleyl ether R 11 is an oleyl group, R 12 is a hydrogen atom, and n is 1 in the general formula (4)!.
Glycerin Ether 2: Glycerin dioleyl ether R 10 and R 12 are oleyl groups, and n is 1 in the general formula (4)!.
Glycerin Ether 3: Glycerin monostearyl ether R 11 is a stearyl group, R 12 is a hydrogen atom, and n is 1 in the general formula (4)!.
Glycerin Ether 4: Triglycerin monooleyl ether R 11 is an oleyl group, R 12 is a hydrogen atom, and n is 3 in the general formula (4)!.
Glycerin Ether 5: Glycerin monolauryl ether R 11 is a lauryl group, R 12 is a hydrogen atom, and n is 1 in the general formula (4)!.
Glycerin Ether 6: Diglycerin monomyristyl ether R 11 is a myristyl group, R 12 is a hydrogen atom, and n is 2 in the general formula (4)!.
Glycerin Ether 7: Diglycerin monolauryl ether R 11 is a lauryl group, R 12 is a hydrogen atom, and n is 2 in the general formula (4)!.
Component (B)
Ether 1: Lauryl alcohol ethoxylate R 13 is a lauryl group, R 14 is an ethylene group, and m is 3, in the general formula (5)!.
Ether 2: Oleyl alcohol ethoxylate R 13 is an oleyl group, R 14 is an ethylene group, and m is 3, in the general formula (5)!.
Ether 3: Lauryl alcohol propoxylate R 13 is a lauryl group, R 14 is a propylene group, and m is 4, in the general formula (5)!.
Ether 4: Oleyl alcohol propoxylate R 13 is an oleyl group, R 14 is a propylene group, and m is 2, in the general formula (5)!.
Ether 5: Octyl alcohol butoxylate R 13 is an octyl group, R 14 is a butylene group, and m is 8, in the general formula (5)!.
Ether 6: Myristyl alcohol ethoxypropoxylate R 13 is a myristyl group, R 14 is a 2:1 mixture of ethylene group:propylene group, and m is 3, in the general formula (5)!.
Ether 7: Lauryl alcohol ethoxypropoxylate R 13 is a lauryl group, R 14 is an ethylene and propylene groups, and m is 1 or 3, in the general formula (5)!.
Glycerin Ester 1: Glycerin monooleate
Glycerin Ester 2: Diglycerin monooleate
Glycerin Ester 3: Glycerin distearate
Glycerin Ester 4: Glycerin monolaurate
Glycerin Ester 5: Glycerin dioleate
Ester 6: Sorbitan monooleate
Ester 7: Sorbitan trioleate
Component (C)
ZnDTP 1: R 15 and R 16 are 2-ethylhexyl groups (primary alkyl group), and the molar ratio of neutral (a=0) salt to basic salt (a=1/3) is 55:45, in the general formula (6).
ZnDTP 2: R 15 and R 16 are dodecyl groups (primary alkyl group), and the molar ratio of neutral salt to basic salt is 62:38, in the general formula (6).
ZnDTP 3: R 15 and R 16 are 1:1 of secondary hexyl and isopropyl groups, and the molar ratio of neutral salt to basic salt is 62:38, in the general formula (6).
ZnDTP 4: R 15 and R 6 are 1:1 of 1,3-dimethylbutyl group (secondary alkyl group) and isopropyl group (secondary alkyl group), and the molar ratio of neutral salt to basic salt is 62:38, in the general formula (6).
ZnDTC 1: R 17 and R 18 are 2-ethylhexyl groups in the general formula (7).
ZnDTC 2: R 19 and R 20 are 1:1 of 1,3-dimethylbutyl group and isopropyl group in the general formula (7).
EXAMPLE 1
Inventive lubricating oil compositions and comparative lubricating oil compositioms were prepared by compounding based on the formulations shown in Tables 1 to 3. In these tables, the figures refer to wt % as reduced molybdenum amount in the base oil for lubricating oil for the Mo compound, wt % for glycerin ether and glycerin ester, and wt % as reduced phosphorus amount for ZnDTP, respectively.
The stability against hydrolysis of the lubricating oil compositions was evaluated as follows:
Hydrolysis of Lubricating Oil Composition
Into each lubricating oil composition, 0.2 wt % of water was added and the composition was preserved for one week at 93° C. to be used in the following friction coefficient measurement:
Friction Coefficient Measurement
The friction coefficient measurement was carried out with an SRV tester under the following conditions:
Line Contact: The test was carried out in a line contact, in other words, cylinder-on-plate method. An upper cylinder (15 mmφ×22 mm) was set on a plate (24 mmφ×7.85 mm) in the sliding direction, and reciprocated for 15 minutes to evaluate the friction coefficient. Both were made of stainless steel SUJ-2.
Load: 200N
Temperature: 80 ° C.
Test Duration: 15 minutes
Vibrational amplitude: 1 mm
Cycle: 50 Hz
Results are shown in Tables 1 to 3.
TABLE 1__________________________________________________________________________ Inventive Products 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17__________________________________________________________________________Mo Compound 1 0.01 0.03 0.02 0.1 0.04 0.04Mo Compound 2 0.05 0.08 0.08 0.08 0.08 0.08 0.02Mo Compound 3 0.08 0.08 0.07 0.08 0.08 0.08 0.04Mo Compound 4Glycerin Ether 1 0.5 0.5 0.5 0.5 0.5 0.3 0.5 0.5 0.2Glycerin Ether 2 0.4 1.0 0.5Glycerin Ether 3 0.5 0.5Glycerin Ether 4 0.5Glycerin Ether 5 0.5 0.1Glycerin Ether 6ZnDTP 1 0.07 0.05 0.05 0.07 0.07 0.06 0.07 0.07 0.08 0.07 0.01 0.07 0.045 0.06 0.07ZnDTP 2 0.02 0.02 0.08ZnDTP 3 0.01 0.025 0.01Precipitation None None None None None None None None None None None None None None None None NoneFriction CoefficientBefore Use 0.065 0.05 0.04 0.045 0.05 0.05 0.05 0.05 0.045 0.04 0.05 0.04 0.05 0.05 0.05 0.05 0.04After Deterioration 0.08 0.055 0.045 0.05 0.055 0.055 0.06 0.055 0.05 0.045 0.055 0.045 0.055 0.055 0.06 0.06 0.045__________________________________________________________________________
TABLE 2__________________________________________________________________________ Inventive Product 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33__________________________________________________________________________Mo Compound 1Mo Compound 2 0.08 0.08Mo Compound 3 0.08 0.08 0.1 0.1 0.08 0.05 0.15 0.1 0.1 0.04 0.04 0.08 0.08 0.08Mo Compound 4 0.08 0.04 0.04Glycerin Ether 1 0.2 2.0 0.5 0.5 0.5 0.5 0.3 0.5 0.2 0.5 0.2Glycerin Ether 2 0.3Glycerin Ether 3 0.07 1.0 0.3Glycerin Ether 4 0.5Glycerin Ether 5 0.2Glycerin Ether 6 1.0 0.3 0.5 1.0ZnDTP 1 0.07 0.04 0.07 0.02 0.14 0.07 0.07 0.1 0.05ZnDTP 2 0.07 0.03 0.07 0.01 0.07 0.07ZnDTP 3 0.04Precipitation None None None None None None None None None None None None None None None NoneFriction CoefficientBefore Use 0.04 0.04 0.55 0.04 0.04 0.05 0.07 0.05 0.04 0.05 0.05 0.07 0.075 0.07 0.04 0.045After Deterioration 0.045 0.045 0.06 0.045 0.05 0.055 0.08 0.04 0.045 0.055 0.06 0.075 0.085 0.075 0.045 0.05__________________________________________________________________________
TABLE 3__________________________________________________________________________ Comparative Products 1 2 3 4 5 6 7 8__________________________________________________________________________Mo Compound 1 0.08Mo Compound 2Mo Compound 3 0.08 0.08 0.08 0.08 0.08Mo Compound 4Glycerin Ether 1 0.5 0.5Glycerin Ether 2Glycerin Ether 3Glycerin Ether 4Glycerin Ether 5Glycerin Ether 6Glycerin Ester 1 0.5 0.5Glycerin Ester 2 0.5Glycerin Ester 3 0.5Glycerin Ester 4 0.5ZnDTP 1ZnDTP 2 0.07 0.07ZnDTP 3Precipitation Found None Found Found Found Found None FoundFriction CoefficientBefore Use 0.075 0.1 0.085 0.055 0.060 0.055 0.045 0.06After Deterioration 0.125 0.15 0.15 0.09 0.11 0.125 0.090 0.125__________________________________________________________________________
EXAMPLE 2
Inventive lubricating oil compositions and comparative lubricating oil compositions were prepared by compounding based on the formulations shown in Tables 4 to 6. In these tables, the figures refer to wt % as reduced molybdenum amount in the lubricating base oil for the Mo compound, wt % for glycerin ether and glycerin ester, and wt % as reduced phosphorus amount for ZnDTP, respectively.
Each composition was subjected to the measurements of stability against hydrolysis and the friction coefficient, similar to Example 1.
Results are shown in Tables 4 to 6.
TABLE 4__________________________________________________________________________Inventive Products 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49__________________________________________________________________________Mo Compound 1 0.01 0.01 0.02 0.02 0.02 0.08Mo Compound 2 0.06 0.07 0.03 0.02 0.03Mo Compound 3 0.07 0.07 0.07 0.07 0.07 0.07 0.07 0.05 0.02 0.07 0.1 0.05Mo Compound 4Ether 1 0.5 0.5 0.5 0.5 0.3 0.2 0.5 0.005 1.0 0.2Ether 2 0.5 0.3Ether 3 0.5 0.4Ether 4 0.5 0.5Ether 5 0.3 0.2ZnDTP 1 0.07 0.05 0.05 0.07 0.07 0.04 0.07 0.07 0.06 0.07 0.01 0.07 0.05 0.07 0.07ZnDTP 2 0.02 0.02 0.03 0.01 0.01ZnDTP 4 0.01Glycerin Ether 1Glycerin Ether 6Glycerin Ester 1Glycerin Ester 5Glycerin Ester 4Precipitation None None None None None None None None None None None None None None None NoneFriction CoefficientBefore Use 0.06 0.05 0.045 0.045 0.05 0.055 0.05 0.05 0.045 0.05 0.055 0.055 0.05 0.065 0.06 0.05After Deterioration 0.075 0.055 0.045 0.05 0.05 0.055 0.055 0.055 0.055 0.06 0.055 0.055 0.055 0.065 0.065 0.06__________________________________________________________________________
TABLE 5__________________________________________________________________________Inventive Products 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65__________________________________________________________________________Mo Compound 1Mo Compound 2 0.01 0.02 0.08 0.4Mo Compound 3 0.02 0.01 0.05 0.02 0.05 0.02 0.07 0.07 0.07 0.07 0.07 0.07 0.5 0.07 0.1Mo Compound 4 0.02 0.01Ether 1 0.2 0.6 1.0 0.05 0.3 5.0Ether 2 0.2 0.5 0.5Ether 3 0.1 2.0 0.5 0.5Ether 4 0.2 0.5Ether 5 0.5ZnDTP 1 0.01 0.02 0.005 0.02 0.5 0.05ZnDTP 2 0.04 0.05 0.05 0.07 0.01ZnDTP 4 0.01 0.02Glycerin Ether 1 0.5 0.5 0.5Glycerin Ether 6 0.5Glycerin Ester 1Glycerin Ester 5Glycerin Ester 4Precipitation None None None None None None None None None None None None None None None NoneFriction CoefficientBefore Use 0.055 0.055 0.06 0.055 0.065 0.055 0.05 0.06 0.065 0.065 0.06 0.06 0.06 0.05 0.05 0.05After Deterioration 0.065 0.065 0.07 0.07 0.07 0.055 0.055 0.075 0.075 0.08 0.075 0.065 0.065 0.055 0.055 0.055__________________________________________________________________________
TABLE 6__________________________________________________________________________Comparative Products 9 10 11 12 13 14 15__________________________________________________________________________Mo Compound 1 0.07Mo Compound 2Mo Compound 3 0.07 0.07 0.07 0.07Mo Compound 4Ether 1 0.5 0.5Ether 2Ether 3Ether 4Ether 5ZnDTP 1ZnDTP 2 0.07 0.07ZnDTP 4Glycerin Ether 1Glycerin Ether 6Glycerin Ester 1 0.5 0.5Glycerin Ester 5 0.5Glycerin Ester 4 0.5Precipitation Found None Found Found Found Found FoundFriction CoefficientBefore Use 0.075 0.1 0.095 0.055 0.060 0.055 0.045After Deterioration 0.125 0.15 0.15 0.09 0.11 0.125 0.090__________________________________________________________________________
EXAMPLE 3
Inventive grease compositions and comparative grease compositions were prepared by compounding based on formulations shown in Tables 7 to 9. In these tables, the figures refer to wt % in the base grease.
Each composition was subjected to the measurements of the friction coefficient based on the following conditions:
Friction Coefficient Measurement
Point Contact: The test was carried out in a point contact, in other words, ball-on-plate method. An upper ball (10 mmφ) was set on a plate (24 mmφ×7.85 mm), and reciprocated for 2 hours to evaluate the friction coefficient. Both were made of stainless steel SUJ-2.
Load: 200N
Temperature: 50° C.
Test Duration: 2 hours
Vibrational amplitude: 1 mm
Cycle: 50 Hz
Wear Resistance Measurement
The friction coefficient and wear track were evaluated using a high speed four-ball tester, under the following conditions:
Rotation: 1,800 rpm
Load: 40 kg
Temperature: 40° C.
Time: 60 minutes
Results are shown in Tables 7 to 9.
TABLE 7__________________________________________________________________________Inventive Products 66 67 68 69 70 71 72 73 74 75 76 77 78 79__________________________________________________________________________Component AMo Compound 2 3.0Mo Compound 1 3.0Mo Compound 3 3.0Mo Compound 5 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0Mo Compound 4 3.0Component BGlycerin Ether 1 3.0 3.0 3.0 3.0 3.0 3.0Glycerin Ether 2 3.0Glycerin Ether 5 3.0Glycerin Ether 7 3.0Glycerin Ether 3 3.0Ether 1 3.0Ether 2 3.0Ether 7 3.0Ether 4 3.0Component CZnDTP 1 3.0ZnDTP 2ZnDTP 4ZnDTC 1ZnDTC 2SRV Friction Coefficient 0.075 0.07 0.07 0.075 0.075 0.075 0.08 0.07 0.072 0.075 0.079 0.077 0.078 0.60High Speed Four-ball TestFriction Coefficient 0.052 0.051 0.052 0.055 0.05 0.051 0.057 0.051 0.055 0.058 0.057 0.057 0.059 0.040Abrasion Scar (mm) 0.66 0.64 0.67 0.61 0.6 0.65 0.68 0.65 0.6 0.65 0.62 0.67 0.70 0.60__________________________________________________________________________
TABLE 8__________________________________________________________________________Inventive Products 80 81 82 83 84 85 86 87 88 89 90 91 92 93__________________________________________________________________________Component AMo Compound 2 3.0 3.0Mo Compound 1 3.0 5.0Mo Compound 3 3.0 10.0 3.0Mo Compound 5 3.0 3.0 3.0 3.0 0.01 3.0Mo Compound 4 3.0 5.0Component BGlycerin Ether 1 0.01Glycerin Ether 2 3.0 10.0Glycerin Ether 5 3.0 5.0Glycerin Ether 7 3.0 5.0Glycerin Ether 3 3.0 3.0Ether 1 3.0 3.0 3.0Ether 2 5.0Ether 7Ether 4 3.0 5.0Component CZnDTP 1 3.0 3.0 3.0 3.0 3.0 0.01ZnDTP 2 3.0 3.0 5.0ZnDTP 4 3.0ZnDTC 1 3.0 3.0 3.0 10.0ZnDTC 2 3.0SRV Friction Coefficient 0.070 0.065 0.055 0.065 0.06 0.055 0.060 0.055 0.05 0.075 0.065 0.070 0.070 0.05High Speed Four-ball TestFriction Coefficient 0.04 0.050 0.047 0.049 0.045 0.032 0.042 0.045 0.042 0.048 0.045 0.05 0.052 0.050Abrasion Scar (mm) 0.53 0.57 0.53 0.55 0.5 0.50 0.52 0.52 0.49 0.53 0.51 0.55 0.57 0.43__________________________________________________________________________
TABLE 9______________________________________Comparative Products 16 17 18 19 20 21______________________________________Compo- Mo Compound 2nent A Mo Compound 1 3.0 Mo Compound 3 Mo Compound 5 3.0 3.0 3.0 Mo Compound 4Compo- Glycerin Ether 1 3.0nent B Glycerin Ether 2 Glycerin Ether 5 Glycerin Ether 7 Glycerin Ether 3 Ether 1 3.0 Ether 2 Ether 7 Ether 4Compo- ZnDTP 1 3.0 3.0nent C ZnDTP 2 ZnDTP 4 ZnDTC 1 3.0 ZnDTC 2Others Ester 6 3.0 Ester 7 3.0 Ester 1 3.0SRV Friction Coefficient 0.095 0.125 0.11 0.08 0.08 0.085High Friction 0.085 0.105 0.115 0.07 0.06 0.095Speed CoefficientFour-ball Abrasion 0.75 0.95 0.95 0.75 0.73 0.77Test Scar (mm)______________________________________
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A lubricating composition of the present invention comprises a base oil for lubricating oil or base grease; at least one molybdenum compound as component (A) selected from the group consisting of a selected sulfurized oxymolybdenum dithiocarbamate, a selected sulfurized oxymolybdenum dithiophosphate and a selected molybdenum amine compound; and a (poly)glycerol ether and/or a (poly)oxyalkylene glycol monoalkyl ether as component (B).
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BACKGROUND OF THE INVENTION
The present invention relates generally to cooking apparatus, such as for example household deep fat fryers, comprising a cooking vat adapted to be closed by a cover during the cooking phase, and relates more particularly to a device for condensing steam from the vat of such a cooking apparatus, this device comprising a receptacle containing a refrigerating agent and in which is disposed a conduit serving as a condensate channel comprising an inlet for steam to be condensed which passes through the receptacle and which is connected to the vat of the cooking apparatus, and a receptacle outlet and through which flows the water of condensation produced by the passage of the steam through the conduit cooled by the refrigerating agent.
It is known that for such cooking apparatus, the presence of a condensation device is particularly useful to eliminate steam containing bad smelling substances emitted in the course of cooking.
In a known condensation device of this type indicated above, of the heat exchange type, the receptacle is constituted by a cold water reservoir disposed outside on the side of the cooking apparatus, and the condenser channel is formed by a helicoidal tube disposed vertically in the reservoir and which has an inlet passing through an opening provided in the upper wall of the reservoir and is connected by tubing to the vat of the apparatus, and an outlet passing in a sealed manner through the bottom of the reservoir. Thus, during cooking, the vapors containing bad smelling substances flow through and condense in the tube cooled by the water, the condensate being collected in a collecting basin disposed below the reservoir. However, in this condensation device, the upper wall of the reservoir is constituted in fact by a cover which must be open so as to permit the introduction of the helicoidal tube into the reservoir, which complicates further the production of the reservoir. Moreover, the mounting of the helicoidal tube in the reservoir is difficult to carry out, in particularly at the level of the sealed engagement of the outlet through the bottom of the reservoir, resulting in a condensation device which is complicated to produce and cumbersome.
SUMMARY OF THE INVENTION
The invention particularly has for its object to overcome these drawbacks and to provide a device for condensing steam from a cooking apparatus, of the type described above, which will be simple to produce and low cost, and which will ensure efficient heat exchange and condensation.
According to the invention, the receptacle is shaped as a sealed casing made out of one piece of plastic material enclosing the conduit and leaving free the inlet and outlet of this latter, said casing comprising a filling opening for a refrigerating agent adapted to be closed in a sealed manner by a closure member.
Thus, the fact of making the receptacle about the conduit of a single piece, in the form of a sealed casing, permits avoiding any mounting operation of the conduit, contrary to the prior art, thereby substantially simplifying the production of the condensation device. Moreover, this production of the sealed casing enclosing the conduit permits avoiding any sealing joint at the level of the passage of the inlet and the outlet of the conduit through the casing, thereby effecting a reduction in the cost of production of the condensation device.
According to a preferred embodiment, the casing is formed by blow molding.
According to the preferred embodiment, the conduit is shaped as a serpentine formed by blow molding a plastic material.
The invention also relates to a cooking apparatus, such as for example a deep fat fryer, comprising an open housing adapted to be closed by a cover during the cooking phase and which is provided at its bottom with a base, a cooking vat disposed in the housing, and an open basin in its rear region, retractably mounted in the base of the housing and which contains at least one device for condensing cooking steam according to the invention.
BRIEF DESCRIPTION OF DRAWINGS
The characteristics and advantages of the invention will become more apparent from the description which follows, by way of non-limiting example, with reference to the accompanying drawings, in which:
FIG. 1 is a schematic vertical cross-sectional view of an electrical cooking apparatus, such as deep fat fryer, comprising two condensation devices according to the invention;
FIG. 2 is a schematic perspective view, on an enlarged scale, of a basin of the cooking apparatus of FIG. 1, in which are disposed the two condensation devices;
FIG. 3 is a perspective view, on an enlarged scale, of a condensation device;
FIG. 4 is a longitudinal cross-sectional view of the condensation device shown in FIG. 3; and
FIG. 5 is a cross-sectional view on the line V--V of FIG. 4.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The cooking apparatus 1 shown schematically in FIG. 1 is a household electrical deep fat fryer which comprises a housing or open receptacle 3, of generally substantially parallelepipedal shape, in which is disposed a metallic vat 5 adapted to be heated by electrical heating means, such as a shielded resistance 6, and containing a frying bath 7. The housing 3 is supported at its bottom 8 by a base 10, also of substantially parallelepipedal shape and preferably made of a single piece with the housing, and is adapted to be closed, during frying, by a cover 12 mounted hingedly in a removable manner on an upper edge 13 of the housing by disassembleable hinge means (not shown).
The cover 12 comprises on its internal surface a joint 13 so shaped as to effect a sealing between the vat 5 and the cover 12 when the latter is closed, as shown in FIG. 1.
The housing 3, the base 10 and the cover 12 are molded of a plastic material such for example as polypropylene which is particularly economical and easy to work with.
In the base 10 of the housing 3 is provided a recess 16 which opens at the front surface 17 of the base and in which is retractably mounted a tray or receptacle 18, better seen in FIG. 2, of parallelepipedal shape, open at its rear and at its upper side, and containing at least one steam condensation device, two in the example shown in FIG. 2, designated by the same overall reference numeral 20 in FIGS. 1, 2 and 3.
In this example, FIGS. 1 and 2, the tray 18 is shaped as a drawer which, on the one hand, is horizontally slidably mounted in the recess 16 of the base 10 by two horizontal rails 22, of which only one is shown in FIG. 2, engaging in two corresponding slideways (not shown) provided respectively on the two side walls of the recess 16, and, on the other hand, is removable. In FIGS. 1 and 2, there is shown at 24 a wide groove provided in the front surface 26 of the vat 18 and forming a gripping member adapted for withdrawing the tray.
The deep fat fryer 1, FIG. 1, also comprises conduit or connection means 28 establishing communicating between the upper volume of the vat 5 and each of the two condensation devices 20 disposed in the tray 18 (FIG. 2), and permitting the flow of steam.
As shown in FIGS. 3 and 4, each condensation device 20 comprises a receptacle 31 comprising a refrigerating agent 33 (FIG. 4) constituted in this case by ice, if desired colored by a non-toxic coloring agent, and a conduit 35 disposed in the receptacle 31 and serving as a condensate channel. The conduit 35 comprises an inlet 37 for the steam to be condensed and projects outside the reservoir 31, and an outlet 39 opening out of the reservoir 31 and through which is adapted to flow the water of condensation produced by the passage of the steam through the conduit 35 cooled by the ice.
According to the invention, the reservoir 31 is shaped as a sealed casing 40, made of a single piece of a plastic material, surrounding the conduit 35 and leaving free the inlet 37 and the outlet 39 of this latter, the casing 40 comprising an opening 42 (FIG. 4) for filling with water adapted to be closed in a sealed manner by a closure member, such as for example a plug 44.
The casing 40 is preferably made of a transparent plastic material such as for example polypropylene, and is formed either by blow molding or by molding about the conduit 35. It should be emphasized that the blow molding process has the advantage of being particularly economical.
In the embodiment shown in FIGS. 3 and 4, the casing 40 has a parallelepipedal shape and the conduit 35 is shaped as a serpentine which extends flat in a plane parallel to the longitudinal plane P of the casing and which is made either by blow molding or by molding a plastic material such as for example polypropylene. As will be seen in FIGS. 3 and 4, the inlet 37 and the outlet 39 of the conduit 35 project axially from the same lateral surface 46 of the casing 40; the water filling opening 42 is provided also in this side surface 46 of the casing, see FIG. 4.
In FIGS. 3 and 4, there is shown at 48 the small spacers of plastic material which connect the serpentine conduit 35 to the two longitudinal surfaces of the casing 40 so as to maintain the conduit correctly in place, and which are formed suitably during blow molding of the casing 40 about the conduit 35.
In this embodiment, FIGS. 3 and 4, the serpentine conduit 35 has a cross section of approximately rectangular shape, as shown in FIG. 5, and preferably comprises, in alternation over all its length, sections 51 of the same given cross section and sections 53 also of the same cross section but smaller than that of sections 51. The sections 53 thus define constrictions and are adapted to slow the speed of passage of the steam through the conduit 35 so as to increase the heat exchange time with the ice 33, and thereby to optimize the condensation of the steam.
After production in the form of a unitary assembly of the casing 40 provided with the internal conduit 35, water is poured into the casing 40 through the filling opening 22 which is then sealed hermetically by the plug 44. This assembly is then placed in the freezer of a refrigerator before use, so as to permit freezing of the water is contains.
It will be noted that a safety valve, known per se, may be arranged at the level of the filling opening 42.
With respect to FIG. 2, the two refrigerating casings 40 with an internal conduit 35 are mounted removably in the tray 18 and extend in the same longitudinal direction, parallel to each other. One of the two casings 40 is mounted reversed relative to the other casing so as to place beside each other the two steam inlets 37, as shown in FIG. 2.
The two refrigerating casings 40 with an internal conduit 35 rest on cross pieces 55 (FIG. 1) surmounting the wall of the bottom 57 of the tray 18 so as to create a lower region 59 adapted to collect the condensate flowing through the outlet 39 of each conduit 35. Preferably, the two casings 40 are slightly inclined, respectively toward the two longitudinal surfaces of the tray 18 so as to facilitate the flow of condensate through the outlet 39 of each internal conduit 35.
As shown in FIG. 1, the conduit means 28 for the cooking steam, between the vat 5 and each of the two condensation devices 20 mounted in the tray 18, comprise a first conduit 61 which is integrated into the cover 12 of the housing 3 and of which one end 61a opens into the upper volume of the vat 5, and a second conduit 63 which extends vertically through a through opening 64 provided in the housing 3, from the upper edge 13 of its rear surface 66; the conduit 63 has a joint 68 adapted to ensure sealing at the level of the opening 64. The conduit 63 has an L-shaped cross section whose vertical branch 63a passes through the opening 64 and is connected sealingly to the other end 61b of the conduit 61, and whose horizontal branch 63b is closed and comprises two openings 71 which empty into the rear region of the tray 18. To each opening 71 of the horizontal branch 63b of the conduit 63 is sealing connected the inlet 37 of the internal conduit 35 of each of the two refrigerating casings 40, which inlet 37 of the conduit 35 is provided with a sleeve forming a sealing joint 72, as shown in FIGS. 3 and 4.
Referring to FIGS. 1 and 2, the evacuation and elimination of the steam present in the fryer takes place in the following manner.
In the course of frying, the steam (indicated by the arrows) which is given off and which contains the bad smelling substances, escapes through the conduit 61, flowing downwardly through the conduit 63 and entering, via each of the two inlet openings 71, the corresponding inlet 37 of the serpentine conduit 35 of each of the two refrigerating casings 40. It then circulates through each conduit 65, being slowed by the constricted sections 53 of this latter, and condenses in the conduit 35 which is cooled by the frozen water 33; the water of condensation containing the bad smelling substances flows through the outlet 39 of each conduit 35 and falls into the collecting region 59 of the tray 18.
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The invention discloses a device for condensing steams from the vessel of a cooking apparatus, comprising a receptacle (31) containing a refrigerant (33) and in which is placed a conduit (35) comprising a steam feed inlet connected to the vessel, and an outlet for draining the condensed water. The receptacle is shaped as a sealed unitary plastic case (40) surrounding the conduit while leaving clear its inlet and outlet, the case comprising a filler neck (42) for the refrigerant which is hermetically closed by a sealing element (44).
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BACKGR0UND OF THE INVENTION
The present invention relates generally to rotating heads and, more particularly, to a rotating head having an elastomeric member sealingly engageable with a kelly and a lid for retaining bolts which connect the elastomeric member to an inner barrel in the event any of said bolts become inadvertently unthreaded.
BRIEF DESCRIPTION OF THE DRAWINGS
Th single FIGURE in the drawings shows a rotating head which is constructed in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Shown in the drawings is a rotating head 10 which is constructed in accordance with the present invention. In general, the rotating head 10 includes: a cylindrically shaped outer barrel 12 having an upper end 14, a lower end 16 and an outer barrel bore 18 extending axially therethrough intersecting the upper and the lower ends 14 and 16 and forming an inner peripheral surface; an inner barrel 22 having an upper end 24, a lower end 26, an inner barrel bore 28 extending axially therethrough intersecting the upper and the lower end 24 and 26 and forming an inner peripheral surface; a seal assembly 32 for providing a substantially fluid tight seal between the inner barrel 22 and the outer barrel 12; a rotating support assembly 34 for rotatingly supporting the inner barrel 22 on the outer barrel 12; a rotary drive member 36 having an upper end 38, a lower end 40 and a drive bore 42 extending therethrough intersecting the upper and the lower ends 38 and 40, the rotary drive member 36 being mounted on the lower end 26 portion of the inner barrel 22; and a bowl 44 having an upper end 46, a lower end 48 and a bowl opening 50 extending therethrough intersecting the upper end 46 and the lower end 48, the upper end 46 portion of the bowl 44 being connected to the lower end 16 portion of the outer barrel 12 and a discharge opening 52 being formed through a portion of the bowl 44 generally between the upper end 46 and the lower end 48 which extends generally perpendicularly with respect to the axially axis of the bowl opening 50.
During drilling operations at an oil well, gas well or oil and gas well drilling site (referred to herein simply as a well drilling site), a kelly (shown in dashed-lines and designated by the reference numeral 54) is extended into the well borehole (not shown in the drawing) and drilling fluid is passed into the borehole. A plurality of blowout preventers (not shown in the drawing) are connected to the well borehole and the rotating head 10 generally is connected to the uppermost blowout preventer, the kelly 54 extending through the rotating head 10 and the blowout preventers and into the well borehole. During the drilling operations, the drilling fluid is passed from the well borehole, up through the blowout preventers and up through the bowl 44 portion of the rotating head 10 in a direction 56, the rotating head 10 being designed to divert the received drilling fluid out through the discharge opening 52 in a direction 58, generally perpendicular to the direction 56, for passing the drilling fluid back to a fluid pit or pits located at the well drilling site generally near the drilling operations. The drilling fluid commonly is referred to in the industry as drilling mud.
The kelly 54 is rotating during the drilling operations and the kelly 54 generally has a non-circular shaped cross section. The rotating head 10 sealingly engages the rotating kelly 54 to prevent the drilling fluid from being passed upwardly through the rotating head 10 and onto the drilling platform floor or onto another portion of the drilling rig, the rotating head 10 functioning to divert the received drilling fluid for passing the drilling fluid back to the mud pit to pits.
The inner barrel 22 generally is cylinderically shaped and has a support flange 60 formed on the outer peripheral surface of the inner barrel 22. The support flange 60 is disposed generally midway between the upper end 24 and the lower end 26 of the inner barrel 22 and the support flange 60 extends circumferentially about the outer peripheral surface of the inner barrel 22. The support flange 60 extends a distance radially from the outer peripheral surface of inner barrel 22 thereby providing an upwardly facing support surface 62 which extends circumferentially about the outer peripheral surface of the inner barrel 22 and which is spaced a distance radially from the upper end 24 of the inner barrel 22, and a downwardly facing support surface 62 which extends circumferentially about the outer peripheral surface of the inner barrel 22 and which is spaced a distance axially from the lower end 26 of the inner barrel 22, the support surface 62 also being spaced a distance axially from the support surface 64.
A recess 66 is formed in the upper end 24 portion of the inner barrel 22 and a recess 68 is formed in the lower end 26 portion of the inner barrel 22. An upper sleeve 70 is disposed and secured in the recess 66 and a lower sleeve 72 is disposed and secured in the recess 68, the sleeves 70 and 72 preferably being constructed of chrome steel.
The inner barrel 22 is disposed in the outer barrel 18 and positioned such that the upper end 24 of the inner barrel 22 generally is coplanar with the upper end 14 of the outer barrel 12, the upper end 24 being in a plane slightly above the planar disposition of the upper end 14, as shown in the drawing, and such that the lower end 26 of the inner barrel 22 generally is coplanar with the lower end 16 of the outer barrel 12, the lower end 26 being in a plane slightly below the planar disposition of the lower end 16, as shown in the drawing.
The diameter of the inner barrel 22 formed by the outer peripheral surface of the support flange 60 is less than the inner diameter formed by the outer barrel bore 18, thereby providing a space between the outer peripheral surface of the inner barrel 22 and the support flange 60 and the inner peripheral surface of the outer barrel 12 formed by the outer barrel bore 18.
An upper cap 74 is connected to the upper end 14 of the outer barrel 12 and the upper cap 74 includes a portion of a bearing adjustment assembly 76. The upper cap 74 includes a base 77 and a flange 78 which extends a distance radially from the base 77, the flange 78 being disposed generally near the upper end of the base 77 of the upper cap 74.
In an assembled position, a portion of the base 77 extends into the outer barrel 18 and into the space between the inner peripheral surface formed by the outer barrel bore 18 and the outer peripheral surface of the inner barrel 22. In this position, the flange 78 engages the upper end 14 of the outer barrel 12 and a plurality of circumferentially spaced bolts 80 extend through the flange 78 and into the outer barrel 12 thereby securing the upper cap 74 to the outer barrel 12 (only two of the bolts 78 being shown in the drawing.
An opening 82 extends through a central portion of the upper cap 74, the upper end 24 portion of the inner barrel 22 being disposed within the opening 82 in the upper cap 74. A recess 83 is formed in the base 77 portion of the upper cap 74.
A portion of an upper seal assembly 84 is disposed in the recess 83 and the upper seal assembly 84 is adapted to sealingly engage the upper cap 74 and the outer peripheral surface of the inner barrel 22 or, more particularly, the upper sleeve 70, thereby cooperating to provide a fluid seal between the outer and the inner barrels 12 and 22. The upper seal assembly 84 forms a portion of the seal assembly 32.
A lower cap 86 is connected to the lower end 16 of the outer barrel 12. The lower cap 86 includes a base 88 and a flange 90 which extends a distance radially from the base 88, the flange 90 being disposed generally near the lower end of the base 88 of the lower cap 86.
In an assembled position, a portion of the base 88 extends into the outer barrel bore 18 and into the space between the inner peripheral surface formed by the outer barrel bore 18 and the outer peripheral surface of the inner barrel 22. In this position, the flange 90 engages the lower end 16 of the outer barrel 12 and a plurality of circumferentially spaced bolts 92 extend through the flange 90 and into the outer barrel 12 thereby securing the lower cap 86 to the outer barrel 12 (only two of the bolts 92 being shown in the drawing).
An opening 94 extends through a central portion of the lower cap 74, the lower end 26 portion of the inner barrel 22 being disposed through the opening 94 in the lower cap 74. A recess 96 is formed in the base 88 portion of the lower cap 86.
A portion of a lower seal assembly 98 is disposed in the recess 96 and the lower seal assembly 98 is adapted to sealingly engage the lower cap 86 and the outer peripheral surface of the inner barrel 22 or, more particularly, the lower sleeve 72, thereby cooperating to provide a fluid seal between the outer and the inner barrels 12 and 22. The lower seal assembly 98 forms a portion of the seal assembly 32.
It should be noted that, in a preferred embodiment, the upper and the lower sleeves 70 and 72 each are sized with respect to the upper and the lower seal assemblies 84 and 98 so that more surface area of the upper and the lower sleeves 70 and 72 is available for sealing engagement with the respective upper and lower seal assemblies 84 and 98 than indicated in the drawings. Initially, the upper and the lower seal assemblies 84 and 98 each are positioned in the repective recesses 83 and 96 so that the seal assemblies 84 and 98 engage respective portions of the sleeves 70 and 72 generally near the inner ends of the sleeves 70 and 72. In this manner, when the sleeve 70 and 72 wear as a result of the sealing engagement with the respective seal assemblies 84 and 98, the seal assemblies 94 and 98 can be pressed further into the respective recesses 83 and 96 to the positions shown in the drawing and, in this position, the seal assemblies 84 and 98 engage unworn portions of the respective sleeves 70 and 72. This reduces the costly replacement of the sleeves 70 and 72.
The rotating head 10 includes an upper bearing assembly 100 and a lower bearing assembly 102. The upper and the lower bearing assemblies 100 and 102 each engage a portion of the inner barrel 22 and a portion of the outer barrel 12, and the bearing assemblies 100 and 102 cooperate to rotatingly support the inner barrel 22 on the outer barrel 12 so the inner barrel 22 can rotate during the operation of the rotating head 10. The first and the second bearing assemblies 100 and 102 form a portion of the rotating support assembly 34.
The upper bearing assembly 100 includes a cone 104, a cup 106 and a plurality of rollers 108 (only two rollers 108 being shown in the drawing). The cone 104 has a plurality of openings and one of the rollers 108 is disposed in each of the openings in the cone 104. The cone 104 is disposed within the cup 106 and the rollers 108 rollingly or bearingly engage the cup 106. Tapered roller bearings such as generally described above with respect to the upper bearing assembly 100 are well known in the art and are commercially available from Timken Roller Bearing Company, for example.
As shown in the drawing, the upper end 24 portion of the inner barrel 22 extends through a central opening formed through the cone 104 of the upper bearing assembly 100 to a position wherein the cone 104 engages the support surface 62. In this position, the cup 106 portion of the upper bearing assembly 100 engages a portion of the upper cap 74 in a manner to be described in greater detail below.
The lower bearing assembly 102 is constructed exactly like the upper bearing assembly 100 in a preferred form and includes a cone 110, a cup 112 and a plurality of rollers 114 (only two rollers 114 being shown in the drawing). The cone 110 has a plurality of openings and one of the rollers 114 is disposed in each of the openings in the cone 110. The cone 110 is disposed within the cup 112 and the rollers 114 rollingly or bearingly engage the cup 112. Tapered roller bearings such as generally described above with respect to the lower bearing assembly 102 as well known in the art and are commercially available from Tinken Roller Bearing Company, for example.
As shown in the drawing, the lower end 26 portion of the inner barrel 22 extends through a central opening formed through the cone 110 of the lower bearing assembly 102 to a position wherein the cone 110 engages the support surface 64. In this position, the cup 112 portion of the lower bearing assembly 102 engages a portion of the lower cap 86.
The engagement of the inner and the outer barrels 22 and 12 with the upper and the bearing assemblies 100 and 102 secures the bearing assemblies 100 and 102 in position for rotatingly supporting the inner barrel 22 on the outer barrel 12. It is important that the cones 104 and 110 fit with the respective cups 106 and 108 in an aligned manner, or in other words, so that one is not cocked at an angle with respect to the other (referred to herein simply as being in bearing alignment). If the cones 104 and 110 are not in bearing alignment with the respective cups 106 and 108, increased friction or binding results thereby substantially reducing the ability of the inner barrel 22 to rotate during the operation of the rotating head 10.
The upper cap 74 portion of the outer barrel 12 includes a plurality of circumferentially spaced openings 116 extending therethrough intersecting the upper and the lower ends of the upper cap 74 (only two of the openings 116 being shown in the drawing). The openings 116 are aligned with the cup 106 portion of the upper bearing assembly 100, generally at a position near the outer peripheral surface of the cup 106.
The bearing adjustment assembly 76 includes a plurality of adjustment screws 118, each adjustment screw 118 threadedly extending through one of the openings 116 in the upper cap 74. Each of the adjustment screws 118 extends through one of the openings 116 to a position wherein one end of each of the adjustment screws 118 engages the cup 106. The bearing alignment of the upper bearing assembly 100 is adjustable by adjusting the engagement between the adjustment screws 118 and the cup 106. The bearing alignment accomplished on the upper bearing assembly 100 utilizing the adjustment screws 118 also has the effect of adjusting the bearing alignment of the lower bearing assembly 102.
In addition of the adjustment of bearing alignment accomplished via the adjustment screws 118, it also is important that, in an assembled position, the support surface 64 be substantially coplanar with the upper end of the lower cap 86 which engages the lower bearing assembly 102 since any deviation in this coplanar relationship would contribute to bearing misalignment in the lower bearing assembly 102 thereby reducing the ability of the inner barrel 22 to rotate during the operation of the rotating head 10. Further, in this regard, the support surface 62 should be substantially coplanar with the since any deviation in this coplanar relationship would tend to reduce the effect of the adjustment screws 118 to simultaneously adjust the bearing alignment of the lower bearing assembly 102 while directly affecting the upper bearing assembly 100.
It should be noted that the adjustment screws 118 are positioned so that access to such adjustment screws 118 is readily available in an assembled position of the rotating head 10 without the necessity of disassembling any portion of the rotating head 10. Thus, the bearing alignment of the upper and the lower bearing assemblies 100 and 102 can be readily adjusted in the field in an assembled position of the rotating head 10.
The lower end 26 of the inner barrel 22 is disposed in a plane spaced a distance generally below the planar disposition of the lower end 16 of the outer barrel 12. A generally circularly shaped adapter plate 120 is secured to the lower end 26 of the inner barrel 22 via a plurality of bolts 122 (only two of the bolts 122 being shown in the drawing). The adapter plate 120 has an opening 124 extending through a central portion thereof and, in an assembled position, the opening 124 in the adapter plate 120 is axially aligned with the inner barrel bore 28.
The rotary drive member 36 is connected to the adapter plate 120 by a plurality of circumferentially spaced bolts 126 (only two bolts 126 being shown in the drawing). The rotary drive member 26 includes an elastomeric member 128 and a reinforcing plate 130. The elastomeric member 128 has an upper end which forms the upper end 38 of the rotary drive member 36, a lower end which forms the lower end 40 of the rotary drive member 36 and an opening extending therethrough intersecting the upper and the lower ends 38 and 40, the opening through the elastomeric member 128 being the drive bore 42 formed through the rotary drive member 36. The upper end 38 portion of the elastomeric member 128 is bonded or otherwise securedly attached to the plate 130 and the plate 130 is connected to the adapter plate 120 by the bolts 126, thereby connecting the elastomeric member 128 and the plate 130 (the rotary drive member 36) to the lower end 16 of the inner barrel 22 via the adapter plate 120 portion of the rotary drive member 36.
In an assembled position the drive bore 42 through the rotary drive member 36 is axially aligned with the opening 124 in the adapter plate 120 and the inner barrel bore 28. The drive bore 42 through the rotary drive member 36, the opening 124 in the adapter plate 120 and the inner barrel bore 28 each are sized to receive the kelly 54 which extends through the axially aligned openings 136, 124 and 28 during the operation of the rotating head 10. More particularly, the opening 124 and the inner barrel bore 28 each have a diameter which is larger than the effective diameter of the kelly 54 so the kelly 54 can rotate freely within the opening 124 and the inner barrer bore 28 during the rotating head 10.
The drive bore 42 through the elastomeric member 128 preferrably has a generally circularly shaped cross section and the diameter of the opening 136 is less than the effective diameter of the kelly 54. Thus, the kelly 54 is forcibly inserted through the drive bore 42 in the elastomeric member 128 so the elastomeric member 128 grippingly and sealingly engages the portion of the kelly 54 extending through the drive bore 42.
It should be noted that the elastomeric member 128 could be constructed with a drive bore 42 having a non-circularly shaped cross section to mate with the non-circularly shaped cross section. However, it has been found that such non-circularly shaped openings in the elastomeric member 128 then must be aligned with the kelly 54 to effect a secure gripping and sealing between the elastomeric member 128 and the kelly 54 and, if not aligned, the gripping and sealing between the elastomeric member 128 and the kelly 54 is not as effective. The circularly shaped drive bore 42 provides an elastomeric shape which effectively grips and seals with the kelly 54 regardless of the rotational alignment of the kelly 54 with respect to the drive bore 42.
A clamp flange 138 is formed on the outer peripheral surface of the outer barrel 12 and the clamp flange 138 extends a distance radially from the outer peripheral surface of the outer barrel 12, thereby providing an upwardly facing clamp surface 140 and a downwardly facing surface 142. A recess 144 is formed in the clamp surface 140 and the recess 144 extends circumferentially about the clamp surface 140. The clamp flange 138 is disposed generally between the upper and the lower ends 14 and 16 of the outer barrel 12.
In an assembled position, the lower end 16 portion of the outer barrel 12 extends a distance into the bowl opening 50 generally near the upper end 46 of the bowl 44, to a position wherein the upper end 46 of the bowl 44 engages the downwardly facing surface 142. A groove 148 is formed in the upper end 46 of the bowl 44. A ring member 150 is formed on the downwardly facing surface 142 of the outer barrel 12, the ring member 150 extending a distance from the downwardly facing surface 142 and being alignable with the groove 148 in the upper end 46 of the bowl 44. The ring member 150 is disposed in the groove 148 and sealingly engages the upper end 46 of the bowl 44 in the assembled position, thereby forming a fluid seal between the bowl 44 and the outer barrel 12. The ring member 150 and the upper end 46 of the bowl 44 each are of a metal construction and, thus, there is a metal-to-metal seal between the bowl 44 and the outer barrel 12 in the assembled position.
The rotating head 10 includes a plurality of clamps 152 and each clamp 152 is connected to the upper end 46 portion of the bowl 44 and is removably connectable to a portion of the outer bowl 44 for removably connecting the bowl 44 to the outer barrel 12 (only two of the clamps 152 being shown in the drawing). The clamps 152 are identical in construction and each clamp 152 includes: a rod 154 having one end pivotally connected to the outer peripheral surface of the outer barrel 12, a bar 156 which is threadedly connected to the end of the rod 154, opposite the end of the rod 154 which is pivotally connected to the outer barrel 12 and a nut 158 which is threadedly connected to the rod 154 and which is engageable with the bar 156 (the rod 154, the bar 156 and the nut 158 being designated by reference numerals in the drawing only with respect to one of the clamps 152). When the outer barrel 12 has been positioned in the bowl opening 50 with the downwardly facing surface 142 of the clamp flange 138 engaging the upper end 46 of the bowl 44 (the ring member 150 being disposed therebetween), the rods 154 are pivoted in an upward direction to a position wherein the bars 156 extend generally over the clamp surface 140, a lip 160 on each bar 156 engaging the clamp surface 140 and extending into the recess 144. In this position, the nuts 158 are tightened down to secure the bars 156 in clamping engagement with the clamp flange 138, the clamps 152 also providing a means for tightening the engagement between the outer barrel 12 and the upper end 14 of the outer barrel 12 with the ring member 150 disposed therebetween thereby tighteningly securing the fluid seal between the outer barrel 12 and the bowl 44 provided by the ring member 150.
A discharge pipe 162 is connected to the outer peripheral surface of the bowl 44. The discharge pipe 162 has an opening extending therethrough and the opening in the discharge pipe 162 is aligned with the discharge opening 52 in the bowl 44.
As shown in the drawing, the rotating head 10 also includes a lid 164. The lid 164 includes a lid base 165 which is generally cylindrically shaped and which has a lid opening 166 extending therethrough intersecting the upper and the lower ends 167 and 168 of the lid base 165. A portion of the inner peripheral surface formed via the lid opening 166 is threaded and adapted to threadedly engage the threaded portion of the outer peripheral surface of the adapter plate 120, thereby threadedly connecting the lid 164 to the adapter plate 120. A lid flange 169 is formed on the lower end 168 of the lid base 165 and the lid flange 169 extends a distance radially inwardly into the lid opening 166.
In the connected position, the lid flange 169 extends a distance radially inwardly to a position wherein the outer-most end of the lid flange 169 is near, but does not abut the outer peripheral surface of the elastomeric member 128 (spaced a distance from the outer peripheral surface of the elastomeric member 128) and the lid flange 168 circumferentially encompasses a space 170, one end of each of the bolts 126 being disposed within the space 170. Further, in a connected position of the lid 164, the lid flange 168 preferrably abuts one end of each of the bolts 126, as shown in the drawing.
In a preferred embodiment, a plurality of set screws are threaded through the lid base 165, generally near the upper end 167, and into the adapter plate 120 for preventing rotation of the lid 164 which may result in unthreading the lid 164 from the adapter plate 120. Also, in a preferred form, the threads on the lid 164 and the mating threads on the adapter plate 120 each are formed of two spaced apart threaded portions with an unthreaded portion positioned generally between the two spaced apart threaded portions, the set screws extending through the unthreaded portions of the lid 164 and adapter plate 120 to prevent damage to the threads by the set screws.
Also, a portion of the outer peripheral surface generally near the connection of the lid flange 169 to the lid base 165 may be formed on a bevel, a preferred form of construction.
During the operation of a rotating head, it is possible for the bolts 126 to be inadvertently unthreaded and fall from the rotating head into the well borehole. The lid 164 retains any such bolts 126 and prevents such bolts 126 from falling into the well borehole.
The space 172 between the inner barrel 22 and the outer barrel 12 (the space between the inner peripheral wall formed by the outer barrel bore 18 and the outer peripheral surface of the inner barrel 22 and between the upper and the lower caps 74 and 86) is packed with grease to provide the necessary lubrication for the upper and the lower bearing assemblies 100 and 102. The rotating head 10 requires no external lubricating system.
During the operation, the kelly 54 extends through the inner barrel bore 28, the opening 124 in the adapter plate 120, the drive bore 42 in the elastomeric member 128 and through the bowl opening 50. Since the diameter of the drive bore 42 in the elastomeric member 128 is smaller than the effective diameter of the kelly 54, a portion of the drive bore 42, generally near the upper end 38, is tapered to guide the kelly 54 into the drive bore 42 and the kelly 54 is forced through the drive bore 42. The elastomeric member 136 grips and sealingly engages the kelly 54. The kelly 54 rotates and, due to the gripping engagement between the kelly 54 and the elastomeric member 128, the rotation of the kelly 54 causes the rotary drive member 36 to rotate following the rotation of the kelly 54. Since the rotary drive member 36 is connected to the inner barrel 22, the rotation of the rotary drive member 34 cause the inner barrel 22 to rotate, the inner barrel 22 being rotatingly supported on the outer barrel 12 via the rotating support assembly 34. The rotation of the inner barrel 22 and the rotary drive member 36 facilitates the maintaining of the sealing engagement between the kelly 54 and the elastomeric member 128 in a manner which substantially reduces the wearing of the elastomeric member 128. It is significant to note that the rotary drive member 36 provides the only means for rotating the inner barrel 22 and the rotating head 10 does not utilize and additional or other drive source for rotating the inner barrel 22 and the elastomeric member 128 connected thereto.
Drilling fluid enters the open lower end 48 of the bowl 44 in the direction 56 and the drilling fluid enters into the bowl opening 50, the bowl opening 50 forming and sometimes being referred to herein as a chamber. The sealing engagement between the elastomeric member 128 and the kelly 54 substantially prevents the drilling fluid from passing upwardly through the drive bore 42 in the elastomeric member 128 and through the inner barrel bore 28. The lower seal assembly 102 sealingly engages the outer peripheral surface of the inner barrel 22 and the outer barrel 12, thereby substantially preventing the drilling fluid from passing into and through the outer barrel bore 18 or, more particularly, through the space between the inner barrel 22 and the outer barrel 12. The sealing engagement between the outer barrel 12 and the bowl 44 provided by the sealing engagement of the ring member 150 substantially prevents the drilling fluid from passing through the connection between the outer barrel 12 and the bowl 44. Thus, the chamber or bowl opening 50 is sealed so the drilling fluid which enters through the open lower end 48 of the bowl 44 is diverted and passed in a direction 58 through the discharge opening 52 and through the discharge pipe 162 for passing such drilling fluid back to the mud pit, for example.
In a preferred form, the upper and the lower seal assemblies 84 and 98 are of the type commonly referred to in the art as Garlock seals, and such seals are commercially available.
In a preferred form, the elastomeric member 128 and the plate 130 connected thereto are of the type well known in the art and commercially available from such sources as Grant Oil Tool, for example.
Finally, it should be noted that the bowl 44 could be of a larger diameter construction with an upper flange adapted to accept an outer barrel 12 of a relatively much smaller diameter construction by supporting the clamps 152 on angle plates which are hinged to the bowl 44 and moveable to a position wherein the clamp 152 can clampingly engage the outer barrel 12. In this manner, the same smaller diameter bearing assemblies (outer barrel 12 with the inner barrel 22 and the bearing assemblies 100 and 102 assembled thereon) which permits the bearing assemblies to be assembled and lowered through the rotary table. This construction is useful when the size of the rotating head 10 or, more particularly, the bearing assemblies exceeds the size of the opening through the rotary table.
Changes may be made in the various elements and assemblies disclosed herein and the steps or the sequence of steps of the methods disclosed herein without departing from the spirit and the scope of the invention as defined in the claims.
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An improved rotating head having an inner barrel disposed within and rotatingly supported on an outer barrel wherein an elastomeric member is connected to the inner barrel via bolts and a kelly is extendable through the inner barrel and through the elastomeric member, the elastomeric member sealingly engaging the kelly, and wherein a lid is connected to the elastomeric member encompassing the bolts connecting the elastomeric member to the inner barrel for retaining said bolts in the event any of said bolts become inadvertently unthreaded.
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This a division of application Ser. No. 37,303 filed May 8, 1979 now U.S. Pat. No. 4,287,241 which in turn is a division of application Ser. No. 795,888, filed May 11, 1977 now U.S. Pat. No. 4,160,346.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the construction of buildings and is specially concerned with building elements subjected to weather, for example, roofs and walls, and with components of these elements, for instance, coatings.
A specific utility of the invention is in providing an improved form of Bermuda roof. This type of roof will, therefore, serve as a convenient starting point for the understanding of the invention, although it must be understood that the invention is not limited to this use. The Bermuda roof has a sloping deck clad with a plurality of limestone slabs over-lapped to provide a stepped or contoured surface which is covered with paint or a cement wash to render it waterproof. This roof has a characteristic appearance as will be readily recognized by anybody who has visited Bermuda.
Applying the invention to the construction of a Bermuda roof, the stone slabs are replaced by wedge-shaped interfitting insulating shingles of substantially impervious synthetic resin closed cell foam firmly secured to the deck, to form a continuous insulating blanket. The blanket is covered by a load-bearing impact-resistant weather impervious sheath. The sheath is made up of a hard, essentially reinforced concrete shell adhering tenaciously to the top surface of the shingles and an essentially rubbery-textured membrane covering the shell and adhering tenaciously to it. Critical characteristics of the sheath materials and advantageous detailed features of construction which may be accomplished by their use will be described as this disclosure progresses.
2. Description of the Prior Art
The general prior art of constructing roofs and walls is replete in the use of synthetic resin foam in combination with other structural and coating material. For example, one patent, which, at first glance, might be considered analogous to the applicant's development, is directed to cladding a flat surfaced wall or roof, employing a plurality of resilient thermo-insulating cellular polystyrene plates to form an insulating layer covering the wall or roof support. Over the insulating layer there is applied a continuous intermediate layer consisting essentially of a synthetic resin having a reinforcing glass fabric embedded in it. The patentee describes the intermediate layer as being of polyvinyl chloride or a butadiene styrene copolymer, having quartz powder distributed throughout and a propionic acid binder which he says may be mixed with an equal amount of Portland cement. On the free outer face is formed a continuous plaster coating, consisting essentially of a mixture of quartz and synthetic resin cementitious material, which the patentee suggests may be formed of propionic acid ester.
This prior art has the following characteristics. Polyvinyl chloride deteriorates on ultraviolet exposure and gives off corrosive hydrogen chloride. Polyvinyl chloride film blackens and brittles and requires plasticizers for usable flexibility. Butadiene styrene polymers oxidize in ultraviolet light with severe yellowing and embrittlement due to cross-linking. They require the use of antioxidants. Propionic acid esters and polyvinyl acetates hydrolize in the presence of moisture and alkali.
SUMMARY OF THE INVENTION
The applicant's construction contrasts with the teachings of this and other prior art patents by its special protective load-bearing and weatherproof sheath in which there are married together a hard essentially reinforced concrete shell covering the insulating blanket and a soft essentially rubbery-textured plastic membrane covering the shell, the nature and advantages of which will be apparent from the detailed description to follow. A feature of the sheath is that the components may be applied at once at essentially their ultimate thickness. Both the cement mixture to form the concrete shell and the extended resinous mixture for forming the membrane are material in a flowable plastic state which can be spread on a flat or uneven surface. The materials and construction specified by the patentee endow the structure with important properties lacking in materials suggested in earlier proposals.
A preferred sheath is made up as follows. It includes a continuous hard tough shell from about 1.5 mm. to about 5.0 mm. thick of reinforced concrete made with hydraulic cement modified with from about 5% to 20% on a solids weight basis of the total of a synthetic resin latex modifier and desirably reinforced with glass fibers. This shell adheres tenaciously to the surface of the insulating blanket. Adhering tenaciously to the shell is a soft rubbery membrane from about 0.75 mm. to about 3 mm. thick based on a binder matrix of a non-plasticized latex of an acrylic elastomeric-type polymer having a T g within the range from about -35° C. to about -45° C. containing from about 50% to about 60% by weight of finely divided extender. The membrane and shell are married together as an essentially integral unit with the shell providing load-bearing strength and the membrane sealing the shell from the outside and preserving properties of the relatively thin concrete which could be otherwise deteriorated by exposure to the elements. Because of interaction between the setting membrane material and the concrete, the interface between the membrane and the shell is free of moisture-escape blisters which often occur between latex-deposited films and substrates. This is because the membrane is formed with an emulsion (or latex) in which the discrete copolymer (acrylic) particles are dispersed and which permits the formation of a film with minute capillary openings which permit moisture vapor trapped in a building to escape without causing blistering of the membrane as would occur with a membrane formed with a solution polymer binder (continuous solid film as taught in the prior art patent mentioned).
BRIEF DESCRIPTION OF THE DRAWING
Having thus generally described the invention, it will be referred to in more detail by reference to the attached drawing by illustrating preferred embodiments and in which:
FIG. 1 is a fragmentary perspective view of a building having a roof constructed, according to the invention, with parts removed to show the construction:
FIG. 2 is a top plan view of a preferred form of insulating shingle used to form the insulating blanket;
FIG. 3 is an enlarged fragmentary perspective view of one end of the shingle shown in FIG. 2;
FIG. 4 is a fragmentary perspective view of the other end of the shingle shown in FIG. 2;
FIG. 5 is a cross-section along the line 5--5 of FIG. 2;
FIG. 6 is an enlarged fragmentary cross-section along the line 6--6 of FIG. 1 through the eaves part of the roof;
FIG. 7 is an enlarged fragmentary cross-section along the line 7--7 of FIG. 1 through the verge of the roof; and
FIG. 8 is an enlarged fragmentary cross-section illustrating the application of the invention to another type of roof.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring more particularly to the drawings, there is shown a building having a wall A made up of a number of building blocks 15. A roof B is carried by the wall A through an end beam 16, side beams 17 and 18 enclosing a concrete belt course 19 having a reinforcing rod 20, and a ridge beam 21. Rafters 22 extend between the ridge beam and the beam 18 and a rafter foot 23 protrudes from each rafter 22 through the belt course 19 and through a notch in the beam 17.
A roof deck C is made up of sheets 25 of plywood butted together edgewise, with fissures 26 intervening them. The undersurface of the plywood 25 is preferably covered with a layer of plaster 25a prior to erection. A preferred material for this purpose is sold as "Sunny Plaster SP" by Coatings International Limited, Hamilton, Bermuda. Preferably the fissures 26 are caulked with a caulking composition. The roof deck C slopes at an angle to provide drainage and an aesthetic appearance in the roof above it.
On top of the deck C is laid an insulating blanket D made up of a number of interfitting synthetic resin foam shingles 30. The shingles are preferably held to the deck by adhesive 31 although they may be secured by nailing or otherwise. A preferred adhesive is a water-based foam and tile adhesive sold under the trade mark "Nova 96" by Coatings International Limited of Hamilton, Bermuda.
In the example roof, the shingles 30 are of the form shown in FIGS. 3 to 5. Each shingle is tapered and has an undersurface 32 and a merging upper surface 33. Each shingle has a stepped leading end with off-set surfaces 34 and 35 with an intervening shoulder 36 providing a receiving recess (for the thin end of the adjacent shingle higher on the roof) and a thin end 37. One side of each shingle is stepped to provide a side surface 38 and a projecting flange 39. The other side is stepped to provide a side surface 40 and an inwardly stepped narrow surface 41 and shoulder 42 providing a recess for receiving the flange 39 of the adjacent shingle. The shingles are laid in interlocking relationship with those in one row staggered relative to those in the next, as will be readily apparent from FIG. 1 considered in conjunction with the construction of the shingles in FIGS. 2 to 5. Together the shingles form a continuous (apart from the fissures between the shingles) blanket having a stepped or contoured surface covering the deck c. The use of relatively short shingles instead of an elongated strip minimizes the overall expansion and contraction across the roof with temperature changes.
The synthetic insulating foam material of the shingles, because of its voids provide good insulation of the deck C against heat and cold. However, the material lacks structural strength and impermeability to moisture and other influences and requires protection in these respects. To this end, the entire surface of the insulating blanket D is protected, according to the invention, by the adhesive load-carrying sheath made up of a hard, essentially reinforced concrete shell E covered by the soft essentially rubbery textured plastic membrane F, applied as follows.
The hard shell E is preferably formed by spreading over the continuous surface of the roof B a coating of spreadable hydraulic cement-aggregate mix reinforced with finely divided inert material and short glass fibers. The coating is allowed to set to form the thin continuous hard concrete layer E having a thickness from about 1.5 mm. to about 5 mm. conforming to the surface of the insulating layer D and adhering tenaciously to it.
The soft rubbery membrane F is formed by spreading, over the concrete shell E, a matrix-forming composition containing major amounts of finely divided extender and a synthetic resin aqueous emulsion binder. The coating solidifies to form the rubbery membrane, adhering strongly to the shell. It conforms to the surface contours of the insulating layer D and accommodates its expansion and contraction while adhering tenaciously to its surface.
As shown in FIG. 6, the leading edges of the shingles at the lower edge or eaves of the roof extend beyond the edge of the deck 25 and are supported by an overall rectangular eaves-finishing strip 42. The strip 42 has an upper face 43 juxtaposed to the undersurface 32 of the shingles 30, a recess 44 receiving the edge of the deck plywood sheets 25, an outer face 45, and an undersurface 46 which is provided with a longitudinal groove 47 to intercept water blown inward along its surface. The surfaces 36 and 35 of the shingles form with the surface 45 of the strip a pocket to receive a concrete fillet. In accordance with the invention, the shell E continues from the upper surface 33 of the eaves shingles down their leading face 34 and into the pocket to provide a massive anchoring fillet P which adheres tenaciously to the undersurfaces of the shingles 34 and to the surface 45 of the strip 42.
The membrane F also continues over the edge of the roof, covering the parts of the shell in that zone. The membrane extends beyond the shell along the undersurface 46 and into the surface of the groove 47, adhering tenaciously to these surfaces. The shell E is thus anchored to the edge of the roof and acts to protect and retain the edges of the eaves shingles 30. The membrane F completes the job by enveloping the entire edge of the roof in what amounts to a bonnet having a girdle extending down from the top surface and then inwards, sealing the roof against ingress of moisture and further anchoring to the roof deck the shingles of the insulating blanket D and the entire sheath made up of the shell E and the member F.
At the end of the roof there is a verge-finishing strip 50 like the eaves-finishing strip 42. This is overlapped by the shingles 30, the undersurfaces of which are adhesively secured to the strip by adhesive 31.
The skirt of the shell E extends down the verge to the bottom of the side of strip 50. The membrane F extends over the verge covering the shell E and across the undersurface of the strip 50 as far as its groove 51.
FIG. 8 shows the corner of another building employing certain teachings of the invention. The top of a concrete wall 55 supports a steel deck 56 which, in turn, supports a concrete slab 57. Anchored by bolts 58 to the concrete slab is a plywood strip 59. In accordance with the invention this corner structure is covered with a thick fillet 60 of a glass fiber-filled coating composition of the type used to form the membrane F. A continuous membrane 61 is also applied to adhere tenaciously to the surface of the slab 57, the fillet 60, and the strip 59 to extend underneath the plywood strip in a flange 62.
VARIATIONS IN MATERIALS
While the preferred material for the supporting deck A of the structure shown in FIGS. 1 to 8 has been shown as sheets 25 of plywood, other structural materials can be employed, for example, tongue-and-groove timber, corrugated iron, or concrete.
The insulating blanket D is preferably of a synthetic resin foam material capable to being worked, for example, by sawing from a block or sheet or by molding, to provide shingles 30 as described which can be fitted together to provide a continuous covering apart from the fissures at the interface between the respective shingles 30. A preferred material is a closed cell polystyrene foam of a density from about 1 to about 3 pounds, preferably approximately 2 pounds, per cubic foot. One good material is sold under the trade mark "Styrofoam" as described, for example, in the booklet "AMSPEC Full Sidewall Insulation and Wood Frame Construction with Styrofoam Brand Plastic Foam", Amspec Inc., September 1972, Columbus, Ohio, the disclosure of which is incorporated by reference.
SHELL
The shell E is essentially a continuous hard tough load-carrying sheet of reinforced concrete having a thickness within the range from about 1.5 mm. to about 5 mm. which armor-plates the blanket D and adheres tenaciously to it. Preferably this concrete is made with hydraulic cement, fine aggregate and reinforcing material, preferably glass fiber, modified by the use of from about 5% to about 20% of a synthetic resin latex cement modifier to provide it with high impact strength (at least 6 to 16 inch pounds), high flexural strength, thin section strength, high tensile strength (greater than 100 pounds per square inch), shear bond adhesion (at least ten times that of unmodified concrete made with Portland cement) and the capacity of adhering tenaciously to the substrate and other properties. In certain cases, for example, where the substrate is flat, scrim cloth may be used to reinforce the concrete. The resulting concrete also has a high tensile and flexural strength and adhesion necessary to resist freeze-thaw lifting and the durability to withstand weathering and ultraviolet degradation. The cement mix is curable under ambient conditions.
Preferred cement modifiers are aqueous acrylic emulsions as for example described in the article entitled "Acrylic Modifiers for Cement", "Resin Review", vol. 24, No. 2 (1974), hereby incorporated by reference. A preferred cement composition, according to the invention, contains from about 45% to about 60% Portland cement by weight on a dry solids basis and about 5% to about 20% of the acrylic cement mortar modifier resin emulsion "Rhoplex E-330" (trademark) (solids 47%±0.05%) described in the brochure "Rhoplex E-330 Cement Mortar Modifier", Rohm and Haas, August 1974, hereby incorporated by reference, or "Rhoplex MC-76" (solids 47%±0.5%). Less preferred concretes may be obtained by using other commercial latex cement modifiers, for example, containing butadiene styrene, vinylidene chloride, or polyvinyl acetate.
Preferred aggregate materials are fine silica sand within the size range from about 20 to about 100 microns, finely divided calcium carbonate of a size range from about 2 to about 20 microns, and quartz flour of a size range from about 10 to 100 microns. The quartz flour provides for a hard finish. The calcium carbonate gives spreading and working characteristics.
A preferred concrete is made by mixing together a first product including Portland cement, short glass fibers, silica sand, powdered limestone, wetting agents and defoamers with a second product including a liquid acrylic aggregate additive containing enough water for a concrete mix.
The cement mixture can be sprayed on or spread on with a trowel. If sprayed on it is subsequently troweled or brushed. The drying time for the concrete is two to three hours and the setting time about 12 hours. The modified concrete reaches about 90% of its ultimate strength in about 48 hours and cures after about seven days.
THE MEMBRANE
The membrane F is essentially a matrix of a rubbery material laid down from a creamy spreadable latex of elastomeric-type synthetic resin highly filled with a finely divided inert extender as a bodying agent. The membrane is a continuous layer tenaciously adhering to its substrate and having a thickness within the range from about 0.75 mm to about 3.0 mm. The extender should be present in an amount from about 50% to about 60% by weight of the total matrix plus filler. A preferred extender is preferably calcium carbonate, desirably being a blend of different sizes having a particle size within the range from about 2 to about 12 microns with the average from about 4 to about 12 microns. The mixed particle sizes improve packing of the system to the benefit of membrane continuity and physical properties. The membrane is resistant to fumes, chemicals, sea air, salt spray, it is freeze-resistant, non-brittle at low temperatures, non-runny at high temperatures, stable under prolonged exposure to ultraviolet light, has low dirt pick-up and is tenaciously adhesive to its substrate.
A preferred coating composition for the membrane is made by using as a binder composition an intimate mixture of "Rhoplex LC-67" (trademark) (T g about -40° C. to -45° C., pH between about 7 and 8) acrylic emulsion for plasticizer-free caulks and "Rhoplex AC-707" (trademark) (T g about +5° C., to about +15° C.) high solids acrylic emulsion vehicle in the proportions to provide a film having a T g within the range from about -35° C. to about -45° C. For some applications the AC-707 may be omitted allowing for high loading with extender or allowing at the same extender level for a lower T g down to about -45° C. For the significance of T g see the brochure "The Characterization of Polymers" by Rohm and Haas (CM-106 D/cd) and "Plastics in the Modern World" by Couzens and Yarsley, Penguin Books Ltd. (1968). pages 217 and 218., the disclosures of which are hereby incorporated by reference.
Preferred formulations are as follows, the percentages being given by weight:
______________________________________Total resin emulsion solids 44%Total filler and pigment 51%Miscellaneous constituents 5%______________________________________
The composition as manufactured should have a consistency within the range from about 5 to about 50 seconds as measured by the Semco running test referred to as follows in "Formulating Guide for Acrylic Latex Caulks" by Rohm and Haas, Philadelphia, 1975. A 6 oz. sample of the composition is loaded into a polyethylene cartridge and gunned under a pressure of 50 pounds per square inch through a Semco air-powered caulking gun fitted with a Semco nozzle with a 1/8th inch diameter orifice. The time, in seconds, required to gun the caulk sample is the figure used to define the consistency. For example, if it takes 25 seconds to gun the sample, the composition is said to have a consistency of 25. The consistency may be adjusted with water or a glycol for spray or brush application and open time.
The membrane material can be brushed on, troweled on, or sprayed on and brushed. A second and third coat, depending on thickness, can be applied in a minimum of about two hours and a maximum of about 12 hours depending on weather conditions. The membrane should not be applied till 4 or 5 hours at the earliest, preferably about 12 hours after the concrete is applied.
In more detail "Rhoplex LC-67" (trademark) is described in the brochure of Rohm & Haas entitled "Rhoplex LC-67 Acrylic Emulsion for Plasticizer-Free Latex Caulks" (1976), the disclosure of which is hereby incorporated by reference. As described in this literature, this binder has the following characteristics, in terms of its use in caulks. By its use, as a binder, a high quality caulk may be made which is not subject to plasticizer migration problems such as glossing and tackifying of paints with accompanying dirt pick-up, mildew growth, and loss of caulk flexibility on exterior exposure. Caulks using this binder retain the performance advantage of current commercial caulk emulsions over conventional latex caulks in terms of low shrinkage, initial low temperature flexibility, resistance to discoloration on aging or ultra-violet exposure, and dry and wet adhesion to alkyd paints, glass, glazed ceramic and concrete substrates. Using formulations embodying this binder, a latex caulk can be manufactured which exhibits superior adhesion properties and superior elongation with satisfactory tensile and recovery properties.
According to the manufacturer's literature, this aqueous acrylic emulsion polymer binder has the following typical properties:
______________________________________Appearance Milky white liquidSolids content, % 64.5 to 65.5pH, as packed 4.8 to 5.4Specific gravity 1.04Density, lbs./U.S. gal. 8.66Minimum film-formation less then 0temperature, °C.Glass transition temperature approximately -50(T.sub.g), °C.Tukon hardness (KHN) less than 1Storage stability protect from freezing______________________________________
To further characterize this binder, it should be noted that typical caulk formulations using it contain along with it major amounts of a primary extender or filler to provide good caulk performance in terms of caulk rheological and application properties and in minor amounts a drying retarder to provide working times for applying the caulk, defoamer to eliminate gas, a wetting agent and emulsifier which tends to stabilize the binder emulsion and improve the caulk mechanical stability and lowers the caulk consistency and enhances its package or self-stability, a primary pigment dispersion which contributes to forming a stable homogeneous and creamy low consistency caulk, a secondary pigment dispersion which is essential to form a stable, homogeneous caulk with good package stability, and an organic liquid which provides freeze-thaw stability.
Caulk formulations of the type described to characterize the binder are described to explain the nature of the formulation to which the compositions of the present invention belong. The caulk formulations do not, themselves, normally have the consistency required for application by normal coating methods and where laid down in a coating layer do not have adequate coating characteristics.
"Rhoplex AC-707" (trademark) is described in the Rohm and Haas booklet "Rhoplex AC-707" High Solids Acrylic Emulsion Vehicles for Exterior and Interior Latex Paints" (July 1974), the disclosure of which is hereby incorporated by reference.
This literature describes the binder as a high solids acrylic emulsion polymer having the following typical properties:
______________________________________Solids content, % 65.0 ± 0.5pH 9.0 to 9.7Viscosity, cps.Brookfield No. 3 spindle - 60 RPM 300 to 700Minimum film formation +10° C. to +12° C.temperature, °C.Tukon hardness, KHN <1Weight per gallon, lb. 8.97Bulking value, gal./lb. - wet 0.1115dry 0.107Mechanical stabilityWaring Blender - 5 cycles OKFreeze-thaw stability - 5 cycles OKCalcium ion stability OKOven stability - 10 days at 140° F. OKT.sub.g, approximately +10° C.______________________________________
Other qualities of the binder are that the stability of the emulsion formed with it is excellent and problems are not experienced with sedimentation or excessive skinning as might be expected from its high solids content. Usual precautions should be taken against the loss of water from the surface of the emulsion, when handled in bulk storage tanks and drums. A humidification system is recommended with bulk storage and lids should be replaced promptly on drums after use.
A preferred coating composition, according to the invention, includes, besides the two emulsion binders, and the extender pigment, auxiliary functional constituents as follows: "Varsol 138 (trade mark) a solvent type material which acts to retard skin formation and allow adequate time for working the coating: "Nopco NXZ" (trade mark) as a defoaming agent in an amount within the range from about 0.1% to 0.3%; "Triton X-405" (trade mark) a nonionic surfactant present in an amount from about 0.5% to about 0.8%; "Calgon T" (trade mark) a primary pigment dispersant present in an amount from about 0.5% to about 0.8%; "Oratan 850" (trade mark) a secondary pigment dispersant in an amount from 0.05% to about 0.15%; ethylene glycol, an anti-freeze and pigment resin extender in an amount from about 0.1% to about 0.3%; formaldehyde, as a package preservative in an amount from about 0.05% to about 0.15%; ammonia in an amount effective to adjust the pH to within the range from about 9 to about 11; rutile titanium dioxide or other pigments or equally finely ground material or materials in an amount within the range from 0.7% to about 2.0%. All these amounts are by weight on the total composition.
A caulk formulation, using the caulk forming binder alone, employs "Methocel 60HG" (trade mark) as a thickener which aids in attaining caulk slump resistance. For the purposes of the coatings of the invention such an agent is omitted. Likewise, a caulk formulation, using the caulk forming binder, employs "Silane Z-6040" (trade mark) to improve adhesion to certain substrates, in particular wet adhesion to glass and glazed ceramic tiles. Such material is omitted from the present compositions unless they are to be applied to glass or smooth ceramic substrates.
The mixing of the various materials to form the coating composition is relatively straightforward. Preferred apparatus for mixing or similar high shear, low mixing equipment is a Sigma Blade mixer. While the sequence of addition of the constituents is not critical, a preferred sequence is to mix the first and second binders together first. Half the defoamer may also be added at that time. Then, the extender is added slowly over a period of, typically, say a minute, and then there is added slowly the "Varsol", the surfactants and the dispersants. The mixture of the resin with the extenders is quite stiff and lumpy and the addition of the surfactants and dispersants makes it into a nice creamy mass. The total mixing time may run, typically, to about an hour and a half to form a smooth thick spreadable composition.
The inclusion of a fungicide, for example, formaldehyde, in addition to the adjustment of the pH well up into the alkaline range discourages bacteria growth and undesirable odor. Other fungicidal agents may also be included, for example, mercury compounds or "Skane M-8", trade mark for 2-n-octyl-4-isothazolyn-3-one in the carrier solvent propylene glycol.
It will be understood that the compositions of the invention are not necessarily limited to the auxiliary functional agents named or to the precise amounts given for the formation of plasticizer-free caulks and related types of composition to provide the total compositions of the invention with the auxiliary functional properties as described.
Compositions, according to the invention, may be applied by conventional methods, for example, by brushing, spraying or spreading with a spatula directly on the substrate to thicknesses within the range from about 1/8th of an inch to about 1/16 of an inch in one, two or three coats depending on weather conditions and desired coating thickness. A typical coating of the invention will generally "skin" in about half an hour, is rain-proof after about a couple of hours and fully cured within about a week. Once cured, such coating is resistant to weathering, mechanical stress, and abrasion. The coating material adheres strongly to the substrate and remains adhered thereto, after settling, despite expansion and contraction or other movements, because of the great elasticity of the coating. The coating may be laid down on a scrim of woven fiberglass which gives the coating further strength.
The coatings laid down from the coating materials of the invention are competitive cost-wise with other materials. For one example, a roof coating, according to the present invention, is competitive with a built-up tar and gravel roof.
A sheath made up of a membrane formed from the coating compositions described over a concrete shell has remarkable properties because of the inter-relationship between the concrete shell and the resin membrane. The shell being tenaciously adherent to the substrate, and when the latter is a plastic foam acts as a primer permitting bonding of the resin emulsion membrane to the foam surface to which it cannot effectively be bonded by direct contact. Compatability between the surface of the concrete shell and the resin emulsion membrane enables an effective bond between the shell and membrane so that the sheath is to all intents and purposes integral. This compatability is brought about partly by the resin modification of the concrete enabling it to take up moisture from the resin emulsion as it dries and partly by the properties of the resin emulsion whose capillary openings permit eventual escape of moisture from the membrane itself and from beneath it.
ACRYLIC EMULSIONS
The literature on the acrylic emulsions referred to above describes these emulsions as follows.
Rhoplex LC-67 (trademark) is a 65% solids, low Tg polymer emulsion binder that permits manufacture of plasticizer-free latex caulks. The elimination of plasticizer from latex caulk formulations by use of Rhoplex LC-67 (trademark) binder yields a high-quality caulk that is not subject to plasticizer migration problems such as glassing and tackifying of paints with accompanying dirt pickup, mildew growth and loss of caulk flexibility on exterior exposure.
Caulks based Rhoplex LC-67 (trademark) retain the performance advantages of current commercial caulk emulsions, Rhoplex LC-40 (trademark) and Rhoplex LC-45 (trademark), over conventional latex caulks in terms of low shrinkage, initial low temperature flexibility, resistance to discoloration on aging or on ultraviolet exposure, and dry and wet adhesion to alkyl paints, glass, glazed ceramic and concrete substrates. Utilizing our suggested starting point formulation, a latex caulk can be manufactured which exhibits superior adhesion properties and superior elongation with satisfactory tensile and recovery properties, even as compared to the standard 3:1 pigment to binder ratio of Rhoplex LC-40 (trademark) and Rhoplex LC-45 (trademark) based caulks.
Rhoplex LC-67 (trademark) is an aqueous emulsion polymer designed as an internally plasticized caulk vehicle with the following typical properties:
______________________________________Appearance Milky white liquidSolids content, % 64.5 to 65.5pH, as packed 4.8 to 5.4Specific gravity 1.04Density, lbs./U.S. gal. 8.66Minimum film-formulation Less than 0temperature, °C.Glass transition temperature Approximately -50(T.sub.g), °C.Tukon hardness (KHN) Less than 1Storage stability Protect from freezing______________________________________
Rhoplex AC-707 (trademark) is a high solids, acrylic emulsion polymer. Several formulating and manufacturing advantages are realized from utilizing a higher solids content emulsion. Less emulsion must be handled and stored to produce a paint at a given binder solids. More formulation latitude is available as a result of less water being present with high solids emulsion. For example, water included in lower solids emulsion could now be used to increase the grind volume. Higher volume solids paints can be formulated with satisfactory brushing properties while still offering improved film build and higher hiding.
These are typical properties of Rhoplex AC-707 (trademark), but should not be considered specifications:
______________________________________Solids content, % 65.0 ± 0.5pH 9.0 to 9.7Viscosity, cps. BrookfieldNo. 3 spindle - 60 RPM 300 to 700Minumum film formation 5 to 9temperature, °C.Tukon hardness, (KHN) <1Weight per gallon, lb. 8.97Bulking value, gal./lb. - wet 0.1115dry 0.107Mechanical stabilityWaring Blender - 5 cycles OKFreeze-thaw stability - 5 OKcyclesCalcium ion stability OKOven stability - 10 days OKat 140° C.______________________________________
Emulsion stability of Rhoplex AC-707 (trademark) is excellent and no problems have been experienced with sedimentation or excessive skinning as might be expected from the high solids content. However, the usual precautions should be taken against the loss of water from the surface when Rhoplex AC-707 (trademark) is handled in bulk storage tanks and drums. A humidification system is recommended with bulk storage of any Rhoplex (trademark) emulsion. Lids should be replaced promptly on drums after use.
Paints formulated from Phoplex AC-707 (trademark) have properties intermediate between Rhoplex AC-35 (trademark) and Rhoplex AC-388 (trademark) formulations. The flow of paints based on Rhoplex AC-707 (trademark) approaches that of Rhoplex AC-388 (trademark). The film build is slightly lower than Rhoplex AC-388 (trademark) but greater than Rhoplex AC-35 (trademark). Adhesion to chalk and gloss alkyl approach the performance of Rhoplex AC-35 (trademark). Although exterior exposure results are limited, we expect durability performance to be similar to Rhoplex AC-388 (trademark).
When Rhoplex AC-707 (trademark) is formulated into paints using our recommended formulations based on Rhoplex AC-388 (trademark), the spread rate averages up to about twenty percent higher than that of paints formulated with Rhoplex AC-388, (trademark).
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A roof having an insulating blanket of plastic foam covered by a protective sheath made up of a shell of reinforced concrete covered by a weather-impervious rubbery textured membrane. The membrane and the shell are married together in the sheath, the shell providing load bearing strength and the membrane protecting the shell and preserving its properties. The shell adheres tenaciously to the insulating blanket and the membrane to the shell. In a preferred construction, the sheath forms a protective bonnet having a girdle surrounding the eaves and verge further anchoring the roof covering to the superstructure of the building. Shingles of special construction preferably make up the insulating blanket. Special cement and latex binder compositions are disclosed for the shell and membrane respectively.
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CROSS REFERENCE TO RELATED APPLICATION
[0001] This is a Divisional application of U.S. patent application Ser. No. 13/871,094 filed Apr. 26, 2013 entitled ANKLE BRACE which is a Continuation-in-part of U.S. patent application Ser. No. 13/134,087, filed May 27, 2011 entitled ANKLE BRACE.
BACKGROUND OF THE INVENTION
[0002] Field of the Invention
[0003] This invention relates to an ankle brace and more particularly to an ankle brace including a tensioning system which functionally stabilizes the ankle as it reaches extreme ranges of motion.
[0004] Description of the Related Art
[0005] Conventional braces for protecting joints of the body do so by restricting or limiting motion of the joint to which it is applied to prevent a new injury or to protect a pre-existing injury. An ankle joint, just like all the joints in the human body, has a natural range of motion that it can move through without causing damage to itself. As it reaches the end of these ranges, the body has structure such as ligaments and tendons to create tension to end range of motion and protect the joint. Many of the prior art ankle braces do prevent the ankle from exceeding its extreme ranges of motion but do not provide the necessary flexibility to permit the athlete to function normally.
[0006] Applicant's ankle brace described and shown in the co-pending application represents an improvement in the ankle brace art. The instant invention represents a further improvement in the ankle brace art.
SUMMARY OF THE INVENTION
[0007] This Summary is provided to introduce a selection of concepts in a simplified form that are further described below in the Detailed Description. This Summary is not intended to identify key aspects or essential aspects of the claimed subject matter. Moreover, this Summary is not intended for use as an aid in determining the scope of the claimed subject matter.
[0008] An ankle brace is disclosed for use with a cleated athletic shoe having a sole with a lower surface, with cleats extending downwardly therefrom, a lateral side and a medial side, an upper part with an upper end, a lacing closure, with upper and lower ends, including a plurality of spaced-apart pairs of eyelets adapted to have a shoe lace threaded therein. The brace of this invention includes a flexible lateral portion having an upper end, a lower end, a forward end, a rearward end, an outer side and an inner side. The upper end of the lateral portion has a plurality of spaced-apart first eyelets formed therein at the forward end thereof. A first loop is secured to the outer side of the lateral portion adjacent the eyelets at the forward end thereof. A second loop is secured to the outer side of the lateral portion rearwardly of the first loop. A third loop is secured to the outer side of the lateral portion below the eyelets at the forward end of the lateral portion and below the first loop thereof. The lateral portion also has an eyelet formed therein rearwardly of the first eyelets. A patch or strip of hook fasteners secured to the outer surface of the lateral portion at the rearward end thereof. The lateral portion is removably positioned adjacent the lateral side of the upper part of the shoe with the lower end of the lateral portion extending beneath the sole of the shoe.
[0009] The ankle brace also includes a flexible medial portion having an upper end, a lower end, a forward end, a rearward end, an outer side and an inner side. The upper end of the medial portion has a plurality of spaced-apart first eyelets formed therein at the forward end thereof. A first loop is secured to the outer side of the medial portion adjacent the eyelets at the forward end thereof. A second loop is secured to the outer side of the medial portion rearwardly of the first loop. A third loop is secured to the outer side of the medial portion below the eyelets at the forward end of the medial portion and below the first loop thereof. The medial portion has an eyelet formed therein rearwardly of the first eyelets thereof.
[0010] The lower end of the medial portion extends beneath the sole of the shoe with the lower ends of the lateral and medial portions being joined together beneath the sole of the shoe. The rearward ends of the lateral and medial portions are spaced apart.
[0011] An elongated first strap having first and second ends and inner and outer surfaces is also provided. The first end of the first strap is secured to the medial portion at the rearward end thereof. The inner surface of the first strap has loop fasteners thereon. The rearward ends of the lateral and medial portions are spaced apart. The first strap is selectively adjustably secured to the patch of hook fasteners at the outer rearward side of the medial portion.
[0012] The ankle brace of this invention also includes a flexible and stretchable body member having upper and lower ends, a lateral side portion, a medial side portion, and a heel portion. The lower end of the lateral side portion of the body member is secured to the lateral portion. The lower end of the medial side portion of the body member is secured to the medial portion. The heel portion of the body member is secured to the spaced-apart rearward ends of the lateral and medial portions and extends therebetween. A second flexible and stretchable strap is provided having a first end, a second end, an upper end, a lower end, and inner and outer sides. The lower end of the second strap is secured to the upper end of the body member so that the first and second ends of the second strap extend forwardly from the body member. The outer side of the second strap has loop fasteners thereon at the first end thereof. The brace also includes a third flexible strap having a first end, a second end, an outer side and an inner side. The first end of the third strap is secured to the second end of the second strap. The inner side of the third strap has hook fasteners thereon for adjustable attachment to the loop fasteners on the second strap at the first end of the second strap. A fourth flexible non-stretchable strap is provided having first and second ends with the fourth strap being secured to the outer side of the second strap. The first end of the fourth strap has a pair of eyelets formed therein. The second end of the fourth strap has a pair of eyelets formed therein. A loop is secured to the fourth strap at the first end thereof and a loop is secured to the fourth strap at the second end thereof. A lace member adjustably extends through the eyelets on the first and second ends of the fourth strap.
[0013] The ankle brace of this invention includes a flexible and stretchable lateral tensioning cord having first and second ends. The first end of the lateral tensioning cord is secured to the fourth strap at the first end thereof. The lateral tensioning cord extends from its fixed first end downwardly and forwardly through the second loop on the lateral portion, thence forwardly through the first loop on the lateral portion, thence downwardly and rearwardly through the third loop on the lateral portion, thence upwardly and rearwardly through the second loop on the lateral portion, thence rearwardly through the loop at the first end of the fourth strap, thence downwardly therefrom. The second end of the lateral tensioning cord is secured to the lateral portion. A flexible and stretchable medial tensioning cord is also provided having first and second ends with the first end of the medial tensioning cord being secured to the fourth strap at the second end thereof. The medial tensioning cord extends from its fixed first end downwardly and forwardly through the second loop on the medial portion, thence forwardly through the first loop on the medial portion, thence downwardly and rearwardly through the third loop on the medial portion, thence upwardly and rearwardly through the second loop on the medial portion, thence rearwardly through the loop at the second end of the fourth strap, thence downwardly therefrom. The second end of the medial tensioning cord is secured to the medial portion.
[0014] The ankle brace also includes fifth and sixth straps having first and second ends. The first end of the fifth strap is secured to the lateral portion with the second end of the fifth strap being adjustably secured to the medial portion 92 . The sixth strap has its first end secured to the medial portion 92 and has its second end selectively adjustably secured to the lateral portion 36 . The ankle brace of this invention permits the wearers ankle to move through its normal range of motion and yieldably prevents the ankle from moving beyond its normal range motion thereby protecting the ankle.
[0015] It is therefore a principal object of the invention to provide an improved ankle brace.
[0016] A further object of the invention is to provide an ankle brace for use with a cleated athletic shoe which permits the wearer's ankle to move through its normal range of motion but which yieldably prevents the ankle from moving beyond its normal range of motion thereby protecting the ankle.
[0017] A further object of the invention is to provide an ankle brace of the type described which does not interfere with the normal movement of the person's ankle.
[0018] These and other objects will be apparent to those skilled in the art.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] Non-limiting and non-exhaustive embodiments of the present invention are described with reference to the following figures, wherein like reference numerals refer to like parts throughout the various views unless otherwise specified.
[0020] FIG. 1 is a perspective view of the ankle brace of this invention mounted on an athletic shoe;
[0021] FIG. 2 is a side view of the ankle brace of FIG. 1 ;
[0022] FIG. 3 is a side view of the ankle brace as seen from the medial side thereof;
[0023] FIG. 4 is a side view of the ankle brace as seen from the lateral side thereof;
[0024] FIG. 5 is a perspective view of the ankle brace of this invention; and
[0025] FIG. 6 is a bottom view of the athletic shoe having the ankle brace of this invention mounted thereon.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0026] Embodiments are described more fully below with reference to the accompanying figures, which form a part hereof and show, by way of illustration, specific exemplary embodiments. These embodiments are disclosed in sufficient detail to enable those skilled in the art to practice the invention. However, embodiments may be implemented in many different forms and should not be construed as being limited to the embodiments set forth herein. The following detailed description is, therefore, not to be taken in a limiting sense in that the scope of the present invention is defined only by the appended claims.
[0027] The ankle brace of this invention is referred to generally by the reference numeral 10 . Ankle brace 10 is designed to be attached to an athletic shoe 12 having a sole 14 with an underside 16 , and an upper part 18 . A plurality of cleats 19 extend downwardly from the underside 16 of sole 14 . Upper part 18 has a lacing closure structure 20 having a lower end 22 and an upper end 24 . Lacing closure has a plurality of eyelets, grommets or lace openings 26 designed to receive a shoelace 28 in conventional fashion. Shoe 14 will be described as having a lateral side 30 , a medial side 32 and a heel counter 34 .
[0028] Ankle brace 10 includes a lateral portion 36 having a forward end 38 , a rearward end 40 , an upper end 42 and a lower end 44 . Lower end 44 of lateral portion 36 extends partially below sole 14 as will be described in more detail hereinafter. Lateral portion 36 is comprised of a flexible, non-stretchable material such as polyester. The inner side of lateral portion 36 has a flexible, non-stretchable reinforcing or stiffening member 46 secured to the upper portion thereof by stitching or the like. Member 46 is preferably comprised of a plastic material. The upper forward end of lateral portion 36 has a plurality of spaced-apart grommets or eyelets 48 formed therein. Preferably, four eyelets 48 are formed in lateral portion 36 . A grommet 50 is formed in lateral portion 36 rearwardly of the rearward-most grommet 48 . A loop 52 is secured to the outer surface of lateral portion 36 between a pair of grommets 48 . A loop 54 is secured to the outer surface of lateral portion 30 adjacent the rearward-most grommet 48 . A loop 56 is secured to the outer surface of lateral portion 36 below loop 52 . The lower rearward end 44 of lateral portion 36 has a notch 58 formed therein. A notch 60 is also formed in the lower end 44 of lateral portion 36 forwardly of notch 58 .
[0029] Ankle brace 10 also includes a medial portion 62 having a forward end 64 , a rearward end 66 , an upper end 68 and a lower end 70 . Medial portion 62 is comprised of a flexible, non-stretchable material such as polyester. Lower end 70 of medial portion 62 extends partially below sole 14 and is secured to lower end 44 of lateral portion 36 . The inner side of medial portion 62 has a flexible, non-stretchable reinforcing or stiffening member 72 secured to the upper portion thereof by stitching or the like. Member 72 is preferably comprised of a plastic material. The upper forward end of medial portion 62 has a plurality of spaced-apart grommets or eyelets 74 formed therein, the number of which is equal to the number of grommets or eyelets 48 formed in lateral portion 36 . A grommet 76 is formed in medial portion 62 rearwardly of the rearward-most grommet 74 . A loop 78 is secured to the outer surface of medial portion 62 between a pair of the grommets 74 . A loop 80 is secured to the outer surface of medial portion 62 adjacent the rearward-most grommet 74 . A loop 82 is secured to the outer surface of medial portion 62 below loop 78 .
[0030] The lower end 70 of medial portion 62 has a notch 84 formed therein which registers with notch 58 in lateral portion 36 . The lower end 70 of medial portion 62 also has a notch 86 formed therein which registers with notch 60 of lateral portion 36 . The lower ends 44 and 70 of medial portion 62 and lateral portion 36 respectively are secured together by stitching 87 or the like.
[0031] As seen in the drawings, the rearward ends of lateral portion 36 and medial portion 62 are spaced-apart. The rearward end of medial portion 62 has a first strap 88 secured thereto which extends therefrom. The inner surface of strap 88 has loop fasteners thereon. The rearward end of lateral portion 36 has a patch 90 of hook fasteners to enable the strap 88 to be adjustably secured thereto.
[0032] The numeral 92 refers to a flexible and stretchable body member preferably comprised of neoprene or the like which is secured to lateral portion 36 and medial portion 62 as will now be described. Body member 92 includes a lateral side portion 94 , a medial side portion 96 and a heel portion 98 . The lower end of lateral side portion 94 of body member 92 is secured to the upper end of lateral portion 36 by stitching or the like. The lower end of medial side portion 96 is secured to the upper end of medial portion 62 by stitching or the like. Heel portion 98 is positioned between the rearward ends of lateral portion 36 and medial portion 62 and is secured thereto by stitching or the like.
[0033] The numeral 100 refers to an elongated second strap having ends 102 and 104 , an upper end 106 and a lower end 108 . The lower end 108 of strap 100 is secured to the upper end of flexible and stretchable body member 92 so that the ends 102 and 104 extend forwardly from the forward ends of flexible and stretchable body member 92 . The outer surface of strap 100 has loop fastener material thereon.
[0034] A short third strap 110 has one end secured to end 102 of strap 100 and extends therefrom. The inner side of strap 110 has hook fasteners thereon for adjustable connection to the loop fasteners on the outer side of end 104 of strap 100 .
[0035] A flexible and non-stretchable fourth strap 112 , having ends 114 and 116 , is secured to strap 100 at the outer side thereof by stitching or the like. A plastic reinforcing member 118 is secured to the inner side of strap 112 at end 114 . An elongated, flexible reinforcing or stiffening member 119 is positioned at the inner side of strap 112 . Grommets 120 and 122 are formed in the end 114 of strap 112 and reinforcing member 118 . At least one loop 124 is secured to and extends downwardly from end 114 of strap 112 and reinforcing member 118 .
[0036] End 126 of lateral tensioning cord 128 is secured to strap 112 and reinforcing member 118 adjacent end 114 of strap 112 . Tensioning cord 128 extends downwardly and forwardly from strap 112 and reinforcing member 118 , through loop 54 , thence through loop 52 , thence downwardly therefrom, thence rearwardly through loop 56 , thence upwardly and rearwardly through loop 54 , thence upwardly and rearwardly through loop 124 , and thence downwardly and rearwardly through grommet 50 for attachment to reinforcing member 46 at 129 .
[0037] One end of an elongated fifth strap 130 is slidably mounted on cord 128 between loops 54 and 56 . The inner surface of strap 130 is provided with loop fasteners thereon for adjustable attachment to a patch or strap of hook fasteners 131 secured to the outer side of medial portion 62 . A plastic reinforcing member 132 is secured to the inner side of strap 112 at end 116 . Grommets 134 and 136 are formed in end 116 of strap 112 and reinforcing member 132 . At least one loop 138 is secured to and extends downwardly from end 116 and reinforcing member 132 .
[0038] End 140 of tensioning cord 142 is secured to strap 112 and reinforcing member 132 adjacent end 116 of strap 112 . Tensioning cord 142 extends downwardly and forwardly from strap 112 and reinforcing member 132 , through loop 80 , thence through loop 78 , thence downwardly therefrom, thence rearwardly through loop 82 , thence upwardly and rearwardly through loop 80 , thence upwardly and rearwardly through loop 138 , and thence downwardly and rearwardly through grommet 76 for attachment to reinforcing member 72 .
[0039] One end of an elongated sixth strap 144 is slidably mounted on cord 142 between loops 78 and 80 . The inner surface of strap 144 is provided with loop fasteners thereon for adjustable attachment to a patch or strap of hook fasteners 146 secured to the outer side of lateral portion 36 .
[0040] In use, the brace 10 is positioned on the shoe 12 as generally seen in FIGS. 1-3 but the lace member 148 is not tied, the strap 88 is not secured to patch or strip 90 and the straps 130 and 144 are not secured to strips or patches 131 and 146 respectively. The shoe lace 28 is threaded through some of the lower lace openings or eyelets 26 and through at least some of the eyelets 48 of lateral portion 36 and through some of the eyelets 74 of medial portion 62 . The shoe lace 28 will then be threaded through the remaining eyelets 26 and tied at the upper end of the shoe 12 .
[0041] The lace member 148 is threaded through the eyelets 120 , 122 on end 114 of strap 112 and through eyelets 134 and 136 at end 116 of strap 112 . The lace member 148 is then tightened and tied. The strap 88 is then secured to patch 90 . Straps 130 and 144 are then adjustably tightened and secured as described hereinabove. As seen in FIG. 6 , some of the cleats 19 extend downwardly through the registering notches 58 and 84 and some of the cleats 19 extend downwardly through the registering notches 60 and 86 .
[0042] The ankle brace 10 permits the ankle of the person to move through its natural range of motion either laterally, medially, fore and aft. When the ankle moves towards the end of its normal range of motion, the tensioning cords 128 and 142 resist further motion to protect the ankle. Ankle support is also provided by the lateral and medial portions 36 and 62 and the reinforcing members associated therewith. Ankle support is also provided by the flexible and stretchable member 92 which enables the person's ankle to move through its normal range of motion.
[0043] Thus it can be seen that the invention accomplishes at least all of its stated objectives.
[0044] Although the invention has been described in language that is specific to certain structures and methodological steps, it is to be understood that the invention defined in the appended claims is not necessarily limited to the specific structures and/or steps described. Rather, the specific aspects and steps are described as forms of implementing the claimed invention. Since many embodiments of the invention can be practiced without departing from the spirit and scope of the invention, the invention resides in the claims hereinafter appended.
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An ankle brace which is positioned on an ankle of a person which incorporates a tensioning structure which permits full range of motion to the ankle joint but which prevents the ankle joint from moving past its normal range of motion to protect the ankle joint.
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FIELD OF THE INVENTION
Embodiments of the present invention are generally related to back flow preventors that interconnect to a water source. More particularly, devices that attach to a sill cock, or any other fluid source, to prevent back flow of fluids, that may contain contaminants into the fluid supply are provided.
BACKGROUND OF THE INVENTION
Almost all buildings include some type of exterior fluid delivery system. The most common outdoor fluid delivery system is comprised of a faucet with a handle for actuating a valve that initiates or ceases fluid flow from a fluid source through a sill cock of the faucet. In order to direct the exiting fluid, it is also well known to employ a hose that is threadingly interconnected to the sill cock. Fluid in the hose may, under certain conditions, enter the faucet and ultimately the fluid source. For example, if the fluid pressure in the hose is greater than the fluid supply pressure “back flow” will occur. Such back flow may be harmless. One skilled in the art will appreciate, however, that the fluid in the hose could be harmful and result in spoilage of the water supply or contamination of fluid dispensing apparatus often interconnected to the hose.
One source of contamination includes pesticides and/or fertilizers that are often associated with a delivery system that is interconnected to the open end of the hose. Fluid from the supply is used to dilute those harmful chemicals in the delivery system prior to being distributed. Most municipalities require that a one-way check valve be included in a fluid supply line that delivers water from a public water source to a dwelling so that contaminated water cannot enter the public water supply from the dwelling. Often, there is no requirement that dictates that similar precautions are taken with respect to an exterior fluid delivery system that is associated with a dwelling. It is entirely conceivable that contaminants entering a dwelling from an outside fluid source will affect individuals associated within the dwelling but not the public at large. Further, if the above-mentioned check valve is absent or malfunctioning contaminants could also enter the public water supply via the dwelling.
Another issue related to back flow is the harmful effects of freezing when supply pressure is reduced and/or flow is stopped wherein liquid accumulates within the faucet and/or related plumbing. When the ambient temperature drops, the trapped liquid may freeze potentially causing severe damage to the faucet interconnected check valve and/or associated plumbing. To address this freezing, draining features have been incorporated into prior art check valves, such as the A. W. Cash Valve Company Model VB-111, which includes a stem that must manually be actuated to allow drainage when a hose is not connected. This type of manually draining valve relies on an operator to drain the valve, and is thus not reliable. Self-draining check valves, however, are also known in the art and are disclosed in U.S. Pat. No. 4,712,575 to Lair (“Lair I”), which is incorporated by reference herein. Lair I discloses a self-draining, single valve back flow preventor. When a hose is detached, a spool succumbs to spring pressure and moves axially outwardly from the outlet end of the check valve. A valve, housed within the spool, is thus allowed to move axially from its sealing washer to permit drainage. When the hose is connected, the spool and the valve housed therein, are forced axially toward a sealing washer to create a seal that prevents back flow. Vent holes in the check valve prevent accumulation of back pressure within the valve. Sufficient water pressure during supply flow with the hose attached overcomes a spring used to seat the valve and deflects a vent sealing washer, thereby sealing the vent holes. One drawback of the Lair valve is that foreign material may lodge between the valve and the sealing washer, creating a passage through which back flow may occur.
One way to address the major drawback of Lair I is to provide a second check valve. U.S. Pat. No. 3,905,382 to Waterston (“Waterston”), which is incorporated herein, discloses a check valve with two normally closed spring biased valves, one inside an outlet, and the other located near an inlet. The central portion of the Waterston check valve has an externally-threaded vent outlet. When flow occurs, the supply pressure forces the inlet valve axially from its seat toward the outlet and seals the vent. As flow progresses to the outlet valve, the flow pressure compresses an outlet spring and fluid is free to flow from the check valve. When flow ceases and back flow pressure is sufficient to overcome the valve in the outlet, liquid accumulates in the sealed tube and is discharged through a vent.
The Waterston valve does not provide a draining feature that relieves accumulated liquid upstream from the check valve. In the event of freezing the accumulation of liquid upstream from the check valve can result in severe damage to the check valve and plumbing upstream of the check valve. In addition, contamination may collect in the internal portion of the check valve such that when a back flow condition occurs, the contamination trapped in the check valve may enter the fluid supply.
Another system that employs more than one check valve to prevent back flow of a liquid into a distribution system by eliminating pressure differentials that may occur between the faucet and interconnected hose, is the V-444 Valve (“V-444”) manufactured by A. W. Cash Valve Company. The V-444 is succinctly described in U.S. Pat. No. 5,228,470 to Lair et al. (“Lair II”). The V-444 employs three separate valves enclosed in a housing that allows drainage of the sill cock after the hose is removed and also prevents backflow into the structure. The V-444 includes an outer housing with an internally situated movable spool. The spool includes an o-ring positioned on an angled upper surface thereof that cooperates with an angled inner surface of the housing to define a first valve that selectively opens and closes an outer passage that allows trapped fluid in the sill cock to drain from a plurality of vent holes. The V-444 also includes an inlet check valve and an outlet valve that controls fluid through the valve and that prevents backflow.
In a first mode of use, wherein no hose is connected and supply pressure is absent, the V-444 is self-draining. A spring forces the spool downwardly to open a fluid path that drains fluid from the sill cock through the plurality of vent holes. Fluid trapped within the inlet and outlet check valves also drains from the outlet of the valve.
In a second mode of use, wherein the V-444 is exposed to supply pressure without a hose interconnected, the spring will force the spool downwardly, thereby creating a path for water to flow through the vents of the check valve. The supply pressure will also deflect the inlet check valve and the outlet check valve so that fluid will be able to exit the valve system.
In a third mode of operation, a hose is interconnected to the outlet portion of the V-444, but no supply pressure is provided. Any back pressure generated by fluid in the hose will force the outlet check valve to seat upon a surface provided by the spool. In this configuration, a hose forces the spool upward, thereby closing the first valve so that any fluid within the inlet check valve on the outlet valve can only travel out of the vents and not into the fluid supply.
In a fourth mode of operation, supply pressure is added to the V-444 with a blocked interconnected hose. Here, fluid from the fluid supply causes a seal to deflect, thereby blocking the vents. In addition, the outlet check valve is seated as described above, thereby preventing fluid from entering into the center of the V-444.
The V-444 includes a fifth mode of operation that is similar to the fourth mode wherein the hose is open to free flow. Again, since the hose is interconnected, the first valve is closed. Fluid pressure causes the inlet valve to transition downwardly to seat on the stem, thereby allowing fluid to flow through the center of the inlet check valve. The fluid pressure also pushes the outlet valve downwardly from its seat on the stem, which allows fluid to freely flow into the hose.
Among the major drawbacks of the V-444 are its size, weight, dimensions and inclusion of components that add to its complexity and expense, thereby rendering it unsuitable for use in various situations. More specifically, the V-444 check valve is approximately 2.2 inches in length and 1.9 inches in diameter and weighs about 200 grams. This size is attributed to the use of complex valving mechanisms and the provision of a first valve that includes a movable spool.
Other back flow preventors have been employed such as those similar to the backflow preventor shown and described in U.S. Pat. No. 7,013,910 to Tripp (“Tripp”), which is incorporated by reference herein. Tripp discloses an in-line backflow preventor that is used in fluid carbonation systems is interconnected between a fluid source and a mixing tank. The pressure in the mixing tank of these systems is often greater than the source pressure. Tripp is designed for either continuous down-steam pressure increases or intermittent down-stream pressure variations. Accordingly, Tripp does not have the capability of releasing pressure upstream of the valve outlet. Further, Tripp, due to its normally closed configuration, does not automatically drain or contain other similar features that are required for freeze prevention.
SUMMARY OF THE INVENTION
It is one aspect of the present invention to provide a double check valve for interconnection to a sill cock associated with an outside water source that prevents back flow into the water supply. Back flow can occur as a result of a siphon condition wherein a vacuum exists within the check valve, the sill cock or the water source that is apt to suction water in a hose, or in the interconnected check valve into the water supply. A back flow condition may also occur when the fluid pressure within the hose is greater than that of the water supply. For example, if the hose was taken to a roof of a building, the resulting head pressure may be greater than the supply pressure. In addition, a temporary loss or interruption in supply pressure may create a pressure differential that would create a back flow situation. The embodiments of the present invention also provide freeze protection wherein water inside the sill cock is allowed to freely drain from the double check valve after supply pressure is removed.
Embodiments of the present invention employ a valve body that includes an inlet check valve and an outlet check valve positioned within a valve body and a valve cap. The inlet check valve includes an inlet check seal and is biased from the outlet check valve via a spring (or other similar resiliently deflectable member). The inlet check seal cooperates with a main seal that is positioned between the valve body and the valve cap of the double check valve. The outlet check valve is comprised of an outlet check body with an outlet check seal that selectively engages a seat provided in the valve body. The outlet check body and the inlet check body are preferably selectively interconnected to each other, which will be described in further detail below. A hose plunger, which is adapted to selectively engage a hose, is preferably slidingly interconnected to the double check valve and is biased by a compressive member, such as a spring (or other similar resiliently deflectable member), that is associated with the seat of the valve body. The hose plunger includes a centralized hub that engages an outlet check spring (or other similar resiliently deflectable member) that is associated with the outlet check body. This combination of components is sufficient to prevent back flow and to provide self-draining (e.g. promote freeze resistance) without the need of a third check valve to control fluid flow through the vents. Detailed descriptions of the functionality of certain embodiments of the present invention will be provided below.
It is thus another aspect of the present invention to provide a check valve that omits or is devoid of components employed in prior art systems, thus rendering embodiments of the present invention easier and less expensive to manufacture, lighter, less complex, less prone to malfunction, and easier to repair. More specifically, embodiments of the present invention omit additional valves but continue to provide the same functionality of check valves of the prior art, such as the V-444 described above. That is, a system is provided that more effectively employs less than three valves and preferably two valves, thereby allowing size, weight and failure reduction. For example, it is contemplated that the double check valve of embodiments of the present invention are about ⅓ the size (preferably an about 70% reduction) of the V-444 check valve, which reduces bulk, weight and facilitates installation. Preferably, the check valve of one embodiment of the present invention is approximately 1.2 inches in length (an about 44% reduction) and approximately 1.4 inches in diameter (an about 26% reduction) and weighs about 130 grams (an about 35% reduction). In one embodiment, this reduction in size and weight is attributed to the omission of a spool and a stem that controls flow out of the vents of the V-444 check valve. To achieve this, embodiments of the present invention allow for drainage from a point other than through vents in a valve body, for example, drainage from the outlet of the double check valve as opposed to primarily through vents provided in a valve body, as is done by the V-444 check valve. In addition, the present invention employs a fixed inlet valve and a fixed outlet valve as opposed to the complicated valving scheme employed by the V-444, wherein a movable spool alters the configuration of the internal volume of the valve depending on flow condition.
It is still yet another aspect of the present invention to provide a check valve that meets the American Society of Safety Engineers (ASSE) regulations. More specifically the check valve of embodiments of the present invention meets the requirements of ASSE 1052.
It is another aspect of the present invention to provide a valving system that is dual use. More specifically, embodiments of the present invention possess the capabilities of an in-line valve as disclosed in Tripp and the ability to provide automatic self draining when a hose is disconnected from the valve. The double check valve, preferably, employs normally opened inlet and outlet check valves, which allows for complete and automatic drainage. When a hose is interconnected to the dual check valve, the inlet and outlet check valves close, and will open when the faucet is turned on, for example. Normally opened (present invention) and normally closed (in-line) valves are different and are regulated separate ASSE standards. Normally opened check valves are regulated by ASSE 1052 and in-line valves are regulated by ASSE 1022. ASSE 1022 concerns backflow prevention devices that protect potable water supplies that serve beverage dispensing equipment. ASSE 1022 requires that two independently acting check valves be used that are biased to a normally closed position. Conversely, ASSE 1052 concerns basic performance requirements and test procedures for backflow preventors that are designed to interconnect to a hose. ASSE 1052 valving systems are designed to protect against backflow due to back siphonage and low-head backpressure, under the high hazard conditions present at a hose threaded outlet. ASSE 1052 also requires that the inlet and outlet check valves be biased closed. Embodiments of the present invention comply with ASSE 1052 when a hose is interconnected thereto and provide needed automatic drainage when the hose is disconnected, a technological advancement over the prior art and an improvement over prior art devices similar to Tripp.
Accordingly, it is one aspect of the present invention to provide a back flow prevention device for interconnection to a sill cock that includes a valve body with threads that are adapted to receive a hose, the valve body also having an inlet volume and an outlet volume separated by an internally-disposed wall, a lower surface of the wall defining a valve seat, the valve body further including a vent that provides a flow path between the outside of the valve body and the inlet volume; a seal positioned with the valve body in a volume located adjacent to the inlet volume, the seal adapted to selectively block the vent; a valve cap interconnected to the valve body that is positioned within the volume that maintains the seal against the valve body, the valve cap having threads for interconnection to a sill cock of a faucet; an inlet check valve comprising: an inlet check spring positioned within the inlet volume, wherein the spring contacts an upper surface of the wall, an inlet check body positioned within the inlet check spring, an inlet check seal interconnected to the inlet check body that is adapted to selectively engage the seal, thereby opening and closing an aperture of the seal to control fluid flow from the valve cap into the inlet volume; a drain spring positioned within the outlet volume that contacts the seat and a plunger that is adapted to engage a hose; an outlet check valve comprising: an outlet check body positioned within the drain spring, an outlet check seal interconnected to the outlet check body that is adapted to selectively engage the seat to either open a flow path between the inlet volume and outlet volume, or isolate the outlet volume from the inlet volume, thereby preventing fluid from flowing from an interconnected hose into the sill cock; and an outlet check spring positioned about the outlet check body that contacts a portion of the outlet check body and a hub of the plunger.
More generally, it is an aspect of the present invention to provide a back flow prevention device, that includes a valve body with a fixed inlet volume and a fixed outlet volume, the valve body also having a vent for allowing fluid from inside the valve body to escape; a valve cap; a seal positioned between the valve cap and the valve body; an inlet check valve positioned within the inlet volume; and an outlet check valve positioned within the outlet volume.
In addition, it is an aspect of the present invention to provide a back flow prevention device including a body with a fixed inlet volume and a fixed outlet volume, the body also having an aperture; a cap; a primary means for sealing positioned between the cap and the body; an inlet means for selectively preventing flow of fluid positioned within the inlet volume; and an outlet means for selectively preventing flow of fluid positioned within the outlet volume.
Further, one of skill in the art will appreciate upon review of this disclosure that it is another aspect of the present invention to provide a water delivery system including a faucet associated with a water supply; a valve associated with the faucet that is adapted to selectively control the flow of fluid from the water supply through the faucet; and a double check valve associated with the faucet that prevents fluid from entering the water supply and that allows fluid within the faucet to drain therefrom when the valve is in the off position, the double check valve comprising: a valve body with a fixed inlet volume and a fixed outlet volume, the valve body also having a vent for allowing fluid from inside the valve body to escape, a valve cap, a seal positioned between the valve cap and the valve body, an inlet check valve positioned within the inlet volume, and an outlet check valve positioned with the outlet volume.
It is also an aspect of the present invention to provide a back flow prevention device that employs a housing having a passageway configured for the transport of a fluid therethrough, the housing having an inlet and an outlet, the passageway encompassing a valve system consisting essentially of: a first check valve disposed in the passageway that allows fluid to flow through the passageway in the direction from the inlet to the outlet; and a second check valve disposed in the passageway that allows fluid to flow through the passageway in the direction from the inlet to the outlet; a diaphragm disposed in the passageway adapted to engage at least one of the first check valve and the second check valve; a vent in fluid communication with the passageway and located between the first and second check valves, the vent selectively isolated from the passageway by the diaphragm, the vent adapted to permit fluid located between the first and second check valves to exit the housing through the vent, whereby the back flow prevention device permits substantially all fluid to drain completely from the device.
It is still yet an aspect of the present invention to provide a back flow prevention device that includes a housing having first and second ends and including a means for connecting to a fluid inlet line at the first end and for connecting a fluid outlet line to the second end; a central cavity within the housing; wherein the housing includes a valve system consisting essentially of first and second drain valves and is devoid of a third drain valve, the first drain valve located within the housing between the central cavity and the fluid inlet line to permit drainage of fluid from the fluid inlet line to the fluid outlet line end of the housing when the fluid outlet line is not connected thereto, and the second valve located within the housing between the central cavity and the fluid inlet line to control flow between the fluid inlet line and the central cavity, whereby the back flow prevention device permits substantially all fluid to drain completely from the device.
The Summary of the Invention is neither intended nor should it be construed as being representative of the full extent and scope of the present invention. The present invention is set forth in various levels of detail in the Summary of the Invention as well as in the attached drawings and the Detailed Description of the Invention and no limitation as to the scope of the present invention is intended by either the inclusion or non-inclusion of elements, components, etc. in this Summary of the Invention. Additional aspects of the present invention will become more readily apparent from the Detail Description, particularly when taken together with the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate embodiments of the invention and together with the general description of the invention given above and the detailed description of the drawings given below, serve to explain the principles of these inventions.
FIG. 1 is a perspective view of a double check valve of one embodiment of the present invention;
FIG. 1A is a partial cross-sectional view of the double check valve of one embodiment of the present invention associated with a faucet;
FIG. 2 is an exploded perspective view of the double check valve shown in FIG. 1 ;
FIG. 3 is a cross-sectional view of FIG. 2 ;
FIG. 4 is a cross-sectional view of FIG. 1 showing an open flow configuration wherein the double check valve is interconnected on one end to a sill cock and opened on the other end;
FIG. 5 is a cross-sectional view of FIG. 1 showing a no flow configuration wherein the double check valve is interconnected to a sill cock and a hose;
FIG. 6 is a cross-sectional view of FIG. 1 showing a closed flow configuration wherein the double check valve is interconnected to a sill cock and a hose;
FIG. 7 is a cross-sectional view of FIG. 1 showing a double check valve in a siphon condition;
FIG. 8 is a cross-sectional view of FIG. 1 showing the double check valve exposed to back siphonage;
FIG. 9 is a cross-sectional view of FIG. 1 showing the double check valve subsequent to hose removal;
FIG. 10 is a cross-sectional view of FIG. 1 showing the double check valve during testing;
FIG. 11 is a valve cap of an alternate embodiment of the present invention; and
FIG. 12 is a valve cap of an alternate embodiment of the present invention.
To assist in the understanding of the present invention the following list of components and associated numbering found in the drawings is provided herein:
#
Components
2
Double check valve
4
Hose
6
Inlet check valve
10
Outlet check valve
14
Valve body
18
Valve cap
22
Vent
26
Outlet
30
Inlet
34
Main seal
38
Inlet check seal
42
Threads
46
Knurls
50
Hose plunger
51
Faucet
52
Valve
54
O-ring
58
Wrench flats
62
Annular jut
66
Inlet check body
70
Hooked surface
74
Inlet check spring
78
Seat
80
Passage
82
Drain spring
86
Outlet check body
90
Hollow portion
94
Slot
98
Stop
102
Outlet check seal
104
Outlet check spring
108
Cylindrical portion
112
Protrusion
116
Hub
118
Upper surface
120
Lip
124
Stop
128
Thumb screw hole
132
Hose washer
134
Fluid
136
Ring
140
Groove
It should be understood that the drawings are not necessarily to scale, although particular perspective dimensions may be relied upon to define the present invention. In certain instances, details that are not necessary for an understanding of the invention or that render other details difficult to perceive may have been omitted. It should be understood, of course, that the invention is not necessarily limited to the particular embodiments illustrated herein.
DETAILED DESCRIPTION
Referring now to FIGS. 1-12 , a double check valve 2 is provided that includes an inlet check valve 6 and an outlet check valve 10 positioned in a valve body 14 . The valve body 14 receives a valve cap 18 that is adapted for interconnection to a sill cock of a faucet, for example. The valve body 14 also includes a plurality of vents 22 that allow for drainage of fluids from the sill cock, the inlet check valve 6 and/or outlet check valve 10 depending on the pressure gradient within the double check valve 2 . Embodiments of the present invention thus allow fluid within the sill cock to drain from the double check valve to prevent freezing. Back flow is prevented such that when pressure at an outlet 26 of the double check valve is greater than the pressure at the inlet 30 , which is in communication with a fluid supply, a main seal 34 (or diaphragm) will cooperate with an inlet check seal 38 to prevent back flow from entering the fluid supply. Excess water then will be trapped within the inlet check valve 6 or outlet check valve 10 (when a hose is interconnected to the check valve), or be drained from the vents 22 . If no hose is interconnected, trapped fluid is able to drain from the inlet and outlet valves as well.
Referring now to FIGS. 1 and 1A , a double check valve 2 of one embodiment of the present invention is shown. Preferably, the components of double check valve 2 , which will be described in further detail below, are constructed of a rigid material commonly used in the plumbing arts, such as brass. However, one skilled in the art will appreciate other suitable materials may be utilized without deviating from the scope of the invention. The double check valve 2 includes a valve body 14 that is interconnected to a valve cap 18 . The valve cap 18 is the inlet 30 of the double check valve 2 and employs a plurality of threads 42 (or a bayonet fitting), positioned on its outer and/or inner surface thereof, for interconnection to a sill cock of a faucet. The valve body 14 is preferably a cylindrical member that may include a knurled 46 outer surface that aids in the interconnection of the double check valve 2 to a fluid source. The double check valve 2 also includes a plurality of vents 22 that allow fluid and/or air to escape from the internal volume thereof. The valve body 14 also includes a plurality of threads 42 positioned about an outlet 26 of the double check valve 2 . A hose plunger 50 is selectively interconnected to the valve body 14 and is designed to coincide with the outlet 26 of the double check valve 2 when a hose 4 is interconnected thereto. FIG. 1A illustrates an embodiment of the double check valve 2 in association with a faucet 51 , also referred to as a sill cock. The faucet 51 employs a valve 52 to control the flow of water.
Referring now to FIGS. 2 and 3 , exploded views of one embodiment of the present invention are provided. An o-ring 54 is positioned within the valve cap 18 . One of skill in the art will appreciate the sealing function provided by the o-ring 54 may be performed by a flat seal or any other sealing member, or combination thereof, without departing from the scope of the invention. The valve cap 18 may also include a plurality of wrench flats 58 for securely interconnecting the double check valve 2 to a sill cock, for example. The valve cap 18 also includes an annular jut 62 that interfaces with the main seal 34 of the double check valve 2 . Between the main seal 34 and the valve body 14 resides an inlet check body 66 that includes a lower end with a protruding, or hooked surface 70 . The inlet check body 66 receives the inlet check seal 38 on one end and an inlet check spring 74 on the other end. The inlet check spring 74 rests on an internal wall, or seat 78 , provided within the valve body 14 . Alternatively, the inlet check spring 74 may contact and outlet check body 86 . The seat 78 defines a passage 80 that allows fluid to flow from the inlet check valve 6 to the outlet check valve 10 . The valve body 14 also includes threads 42 that receive a hose.
The seat 78 is also associated with a drain spring 82 that is positioned about the outlet check body 86 . The outlet check body 86 includes a hollow portion 90 having a slot 94 bounded by a stop 98 . The stop 98 cooperates with the hooked surface 70 of the inlet check body 66 , thereby operably interconnecting the inlet check body 66 and the outlet check body 86 . The outlet check body 86 includes an outlet check seal 102 and an outlet check spring 104 positioned about a cylindrical portion 108 thereof. Finally, the outlet check body 86 includes a lower protrusion 112 that is snap fit within a hub 116 of the hose plunger 50 .
An upper surface 118 of the hose plunger 50 is engaged to the drain spring 82 wherein its lower portion is adapted to contact a hose. The hose plunger 50 also includes a lip that engages an inner surface of the valve body 14 when a hose is interconnected thereto that prevents further insertion of the hose plunger 50 into the double check valve when the hose is interconnected. The hose plunger 50 of one embodiment of the present invention is a snap fit within the valve body 14 such that the lip 120 of the hose plunger 50 engages a stop 124 provided adjacent to the outlet of the valve body 14 when a hose is not interconnected to the valve body 14 .
Referring now to FIG. 4 , the double check valve 2 of one embodiment is shown during an open flow condition. Here, the valve cap 18 is shown interconnected to the valve body 14 . The valve cap 18 may include a thumbscrew aperture 128 to receive a thumbscrew that allows a user to tightly (an often permanently) affix the double check valve 2 onto a sill cock. A main seal 34 is positioned between the annular jut 62 of the valve cap 18 and the valve body 14 . Embodiments of the present invention interference fit the valve cap 18 onto the valve body 14 . One skilled in the art, however, will appreciate that the valve cap 18 may be screwed, welded or otherwise interconnected to the valve body 14 . An o-ring 54 resides within the valve cap 18 and is adapted to provide a seal between the sill cock and the valve cap 18 .
FIG. 4 shows an open flow condition wherein the supply pressure exists but no hose is interconnected to the double check valve 2 . The hose plunger 50 is biased by the drain spring 82 such that the lip 120 of the hose plunger 50 contacts the stop 124 of the valve body 14 . Supply pressure forces the main seal 34 to deflect downwardly, which blocks fluid flow through the vents 22 . This configuration is substantially different from the V-444 configuration described above. During an open flow condition with no interconnected hose, the V-444 valve will allow fluid to escape out of the vents that wastes water. Supply pressure also forces the inlet check body 66 downwardly, which compresses the inlet check spring 74 . The supply pressure in this configuration is sufficient enough to transition the outlet check seal 102 downwardly and to compress the outlet check spring 104 to separate the outlet check seal 102 and seat 78 .
Referring now to FIG. 5 , the double check valve 2 is shown with the hose 4 interconnected during a non-flow condition. In this configuration, connection of the hose 4 , which includes a hose washer 132 , forces the hose plunger 50 , and thus the hub 116 thereof, axially upward. The upward motion of the hose plunger 50 compresses the outlet check spring 104 , which forces the outlet check body 86 upwardly such that the outlet check seal 102 engages the seat 78 . Thus, interconnection of the hose 4 completely isolates the outlet check valve 10 from the inlet check valve 6 . If any back flow causing pressure rise in the hose 4 occurs, the seal between the outlet check seal 102 and its seat 78 will prevent fluid from entering the fluid source, unless those components have failed (for example, debris lodged between the outlet check seal 102 and the seat 7 that allows for fluid infiltration). Since there is no flow from the fluid supply, the inlet check spring 74 and the inlet check body 66 will be positioned upwardly so that the inlet check seal 38 is engaged to the main seal 34 . Thus, the inlet check valve 6 is isolated from the valve cap 18 that is interconnected to the fluid source. The inlet check valve 6 is, however, in fluidic communication with the vents 22 wherein any fluid pressurized by the transitioning outlet check body 86 will exit therethrough.
Referring now to FIG. 6 , a closed flow condition is shown wherein the hose (not shown) is interconnected to the valve body 14 and the fluid supply has been opened. Here, supply pressure deflects the inner diameter of the main seal 34 downwardly such that the main seal 34 blocks the vents 22 . Supply pressure also acts on the inlet check seal 38 to force it downwardly which compresses the inlet check spring 74 . As described above, since the hose is interconnected to the valve body 14 , the hose plunger and the outlet check body 86 will be shifted upwardly. The inlet check body, however, will contact the outlet check body 86 and force it downwardly, thereby counteracting the outlet check seal and opening the passage 80 between the inlet check valve 6 and the outlet check valve 10 .
Referring now to FIG. 7 , a non-flow configuration wherein a siphon has occurred is shown subsequent to the removal of supply pressure with the hose (not shown) interconnected to the valve body 14 . A siphon condition may be caused when gravity-induced flow of the water in the hose pulls a vacuum after the supply pressure has been shut off. The vacuum within the inlet check valve 6 and the outlet check valve causes the main seal 34 and the outlet check body 86 to deflect towards the outlet of the double check valve 2 . The outlet check body 86 translates downwardly until it contacts the hub 116 of the hose plunger 50 . The inlet check spring 74 pushes the inlet check body 66 upwardly. However, the hooked surface 70 of the inlet check body 66 will engage with the stop 98 of the outlet check body 86 , thereby limiting the range of motion of the inlet check body 66 and preventing the inlet check seal 38 from closing the main seal 34 . That is, during a siphoning condition, the inlet check seal 38 will not be able to fully flatten the main seal 34 . As a result, the deflected main seal 34 will be prevented from completely blocking the vents 22 . A path between the inlet check seal 38 and the internal surface of the inlet check valve 6 will allow air from the outside of the double check valve 2 to enter through the vents 22 to break the vacuum which allows the outlet check spring 104 to relax and engage the outlet check valve 10 on the seat 78 . This in turn will allow the inlet check body 66 to transition upwardly to engage the inlet check seal 38 onto the main seal 34 to isolate the inlet check valve 6 and the outlet check valve 10 from the valve cap 18 as shown in FIG. 5 .
Referring now to FIG. 8 , a back siphonage situation is shown. Here, the hose (not shown) is interconnected to the valve body 14 and a vacuum has occurred at fluid supply that could cause contaminated fluid from the hose or double check valve 2 to enter the fluid supply. In operation, the hose forces the hose plunger 50 upwardly that compresses the drain spring 82 . The hub 116 of the hose plunger 50 also moves upwardly and forces, via the outlet check spring 104 , the outlet valve check body 86 to move upwardly so that outlet check seal 102 engages the seat 78 . The vacuum in the valve cap 18 pulls the inlet check seal upwardly to engage the main seal 34 . Thus the outlet check valve 10 is isolated from the inlet check valve 6 and the inlet check valve 6 is isolated from the cap valve 18 which is interconnected to the fluid supply, and no fluid from the hose and/or the double check valve can enter the fluid supply.
Referring now to FIG. 9 , draining of the double check valve 2 is illustrated. After the hose is removed, the drain spring 82 expands and forces the hose plunger 50 downwardly such that the lip 120 of the hose plunger 50 contacts the stop 124 of the valve body 14 . The hub 116 of the hose plunger 50 will also contact the protrusion 112 of the outlet check body 86 and pull the outlet valve body 86 downwardly, which removes the outlet check seal 102 from the outlet check seat 78 . The stop 98 of the outlet check body 86 will contact the hooked surface 70 of the inlet check body 66 and pull the inlet check seal 38 from the main seal 34 . Thus, a free flow path from the inlet check valve 6 into the outlet check valve 10 and out of the hose plunger 50 is provided. Water in the sill cock will also be able to flow through the valve cap 18 and through the inlet check valve 6 , the outlet check valve 10 and out of the hose plunger 50 . Fluid may also drain through the plurality of vents provided.
Referring now to FIG. 10 , the double check valve 2 is shown during a test. More specifically, it is one aspect of the present invention that the double check valve 2 of embodiments of the present invention can be easily tested in the field to ensure that it is in proper working condition. Here, the hose (not shown) is interconnected to the threads 42 of the valve body 14 that forces the hose plunger 50 upwardly and compresses the drain spring 82 . The hub 116 is also forced upwardly which compresses the outlet check spring 104 and forces the outlet check seal 102 against seat 78 . If the double check valve 2 is working properly the outlet check valve 10 should be isolated from the vents 22 . Fluid 134 is then added via the hose and into the outlet 26 of the double check valve 2 . If the integrity of the outlet check valve 102 and the seat 78 are adequate, no fluid will enter the inlet check valve 6 . Conversely, if the integrity between the outlet check seal 102 and the seat 78 is broken, fluid 134 will fill the inlet check valve 6 , and will exit from the plurality of vents 22 . The inlet check spring 74 will force the inlet check body 66 upwardly to place the inlet check seal 38 in contact with the main seal 34 to prevent any fluid from entering the water source during this test.
Referring now to FIGS. 11 and 12 , valve caps 18 of alternate embodiments of the present invention are provided. Here, the annular jut 62 , which interfaces with the main seal 34 and ring 136 , which interfaces with a groove 140 provided on the valve body 14 are substantially the same as those described above. However, the inlet portion 30 of the valve cap 18 includes a plurality of exterior threads 42 for threading onto sill cocks and have inwardly threads 42 . Inspection of FIGS. 11 and 12 will show that the inlets 30 of these valve caps 18 are of different diameters, thereby succinctly illustrating the scalability of the present invention.
One of skill in the art will appreciate that the valve described and shown herein may be interconnected to the sill cock via a bendable or telescoping member to provide the ability to selectively locate the valve. Alternatively, or in addition, valves as described may possess telescoping functionality as shown in U.S. Design Pat. No. D491,253 to Hansle. The valve may also employ a timer, flow regulation capabilities, etc. to control the flow of fluid therefrom. The valve may employ more than one outlet, which each may include valving as described, and may employ a combination of materials as described in Tripp. Further, the valve may be directly integrated into the sill cock instead of interconnected thereto. The system described herein may include a visual or audible alarm to notify the instance of a valve failure.
While various embodiments of the present invention have been described in detail, it will be apparent that modifications and alterations of those embodiments are also intended to be encompassed by this description. However, it is to be expressly understood that such modifications and alterations are within the scope and spirit of the present invention, as set forth in the following claims. For example, aspects of inventions disclosed in U.S. patent and Published Patent Application Nos. U.S. Pat. Nos. 5,632,303, 5,590,679, 7,100,637, 5,813,428, and 20060196561, all of which are incorporated herein by this reference, which generally concern back flow prevention, may be incorporated into embodiments of the present invention. Aspects of inventions disclosed in U.S. Pat. Nos. 5,701,925 and 5,246,028, all of which are incorporated herein by this reference, which generally concern sanitary hydrants, may be incorporated into embodiments of the present invention. Aspects of inventions disclosed in U.S. Pat. Nos. 6,532,986, 6,805,154, 6,135,359, 6,769,446, 6,830,063, RE39235, 6,206,039, 6,883,534, 6,857,442 and 6,142,172, all of which are incorporated herein by this reference, which generally concern freeze-proof hydrants, may be incorporated into embodiments of the present invention. Aspects of inventions disclosed in U.S. patent and Published Patent Application Nos. D521,113, D470,915, U.S. Pat. Nos. 7,234,732, 7,059,937, 6,679,473, 6,431,204, 7,111,875, D482,431, 6,631,623, 6,948,518, 6,948,509, 20070044840, 20070044838, 20070039649, 20060254647 and 20060108804, all of which are incorporated herein by this reference, which generally concern general hydrant technology, may be incorporated into embodiments of the present invention.
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A double check valve is provided that includes an in-line inlet check valve and an outlet check valve that cooperate to prevent back flow of fluid through the valve. The check valve also includes at least one vent that allows for fluid trapped within the check valve to drain, thereby preventing freezing of the check valve and hydrant to which it is interconnected. The check valve provided omits many superfluous components and thus is smaller and easier to install than check valves of the prior art.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the recovery of ethylene gylcol and dimethylterephthalate from scrap polyethylene terephthalate polyesters. More particularly, it relates to a simplified method of obtaining the constituent monomers of polyethylene terephthalate from scrap wherein the process is practiced under atmospheric conditions without deterioration of the yields.
2. Description of Related Art
Various methods have been disclosed heretofore for the recovery of ethylene glycol and terephthalic acid or derivatives thereof.
U.S. Pat. No 3,776,945 teaches a process of depolymerizing polyethylene terephthalate waste to obtain dimethylterephthalate and ethylene glycol by subdividing the waste into dimensions between 4 and 35 mesh and treating at a temperature of 100° C. to 300° C. and a pressure from 1 to 150 atmospheres with methanol in a quantity that the proportion of methanol to waste is between 1:1 and 10:1 by weight in the presence of acid catalysts.
U.S. Pat. No. 3,321,510 relates to a process of decomposing polyethyleneterephthalate by first treating with steam at a temperature of from about 200° C. to 450° C. and then reducing the steam-treated polyethyleneterephthalate in the form of a brittle solid product to a powder having a mean particles size of from about 0.0005 to 0.002 millimeters and subsequently atomizing the fine powder with a gaseous substance including inert gas and methanol vapor to form an aerosol which is conducted through a reaction zone at a temperature of 250° C. to 300° C. in the presence of excess methanol vapors.
U.S. Pat. No. 3,037,050 relates to the recovery of terephthalate acid dimethyl ester by treating polyethyleneterephthalate in the form of bulky or lumpy solid masses with super-heated methanol vapor in the presence of any suitable esterification catalyst substantially at atmospheric pressure.
U.S. Pat. No. 4,578,502 relates to a procedure for recovering monomeric polycarboxylic acids and polyols from solid scrap polyesters by granulating the scrap resin, slurring the resin with sufficient solvents such as water or methanol, depolymerizing the slurried resin by the application of heat and pressure for a time sufficient to convert substantially all of the resin into its monomeric components, crystallizing the monomeric polycarboxylic acid present by flash crystallization and recovering the polycarboxylic acid and then the polyol by distillation.
U.S Pat. No. 4,163,860 relates to a process for converting a bis-(diol) terephthalate to dimethylterephthalate by interchange in a substantially anhydrous methanol medium in the presence of a magnesium methylate catalyst.
U.S. Pat. No. 3,701,741 relates to a method of recovering substantially pure poly(ethyleneterephthalate) from scrape poly(ethyleneterephthalate) contaminated with impurities by dissolving the contaminated material at elevated temperatures and super-atmospheric pressure in a volatile solvent. This patent does not relate to the recovery of the monomeric ingredients that comprise the polymer.
U.S. Pat. No. 3,488,298 relates to a process for recovering dimethylterephthalate and ethylene glycol from poly(ethyleneterephthalate) scrap by forming a mixture comprising the poly(ethyleneterephthalate) scrape, catalyst and methanol, heating the mixture to approach equilibrium, treating the partially hydrolyzed mixture with an excess of phosphorus-containing compound, heating the treated mixture to fractionate the constituents and recovering methanol, ethylene glycol and dimethylterephthalate.
It can be seen from the above-recited art that many different techniques have been employed in the recovery of the monomeric constituents from poly(ethyleneterephthalate) resins.
These resins have found wide spread use in many and varied applications. For example, poly(ethyleneterephthalate) polyester resins find applications in the preparation of many types of films, including photographic film base, in fibers and in the preparation of food containers such as bottles and the like. Thus, there is a widespread need for a simple and economical method of treating such polyesters to recover the initial ingredients utilized in the preparation of the polyester polymers.
SUMMARY OF THE INVENTION
The invention provides an improved atmospheric pressure method of recovering ethylene glycol and dimethylterephthalate from polyethyleneterephthalate scrap resins by dissolving the scrap polyester resin oligomers of the same monomers as present in the scrap, passing super-heated methanol through the solution and recovering the ethylene glycol and dimethylterephthalate. The process is also advantageous in that the recovered dimethylterephthalate and ethylene glycol is freed of impurities by this method. Thus, the make up of the scrap polyester from which the constituents are recovered need not be considered prior to the recovery procedure and the inventive method is very satisfactory. For example, the following scrap sources are available even if they contain large amounts of impurities:
(1) ground bottle scrap including all the components present, such as, bottle contents, bottle caps, labels and polyethylene bottom cups;
(2) subbed film scrap;
(3) photographic film;
(4) washed film scrap;
(5) still dregs from polyester recovery plant; and
(6) scrap polyester containing polymers including acetate resins, polyvinyl chloride and the like. By oligomers of the same monomers is meant, that the monomers which form constituent parts of the oligomer are the same as that of the polymer, i.e., ethylene gylcol and terephthalic acid or dimethylterephthalate. In accordance with Grant and Hacks Chemical Dictionary, Fifth Edition, published by MaGraw-Hill Book Company, an oligomer is "a polymer whose properties change with the addition or removal of one or a few repeating units. The properties of a true polymer do not change markedly with such modification". In accordance with this invention an oligomer is any low molecular weight polyester polymer of the same constituency as that of the scrap material being employed as the starting component wherein the scrap polymer will dissolve in the low molecular weight oligomer. The constituent units of the oligomer used in accordance with this invention will repeat "n" times wherein the "n" will vary between 2 and 100 and a molecular range of between 384 and 19200. In this oligomer composition, many polymer units of varying chain links is present. Values of n as low as 2 to 5 or as high as 50 to 100 are suitable in accordance with this invention.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a schematic flow diagram illustrating an apparatus suitable for use in practicing the process of this invention.
DESCRIPTION OF PREFERRED EMBODIMENTS
FIG. 1 illustrates in diagrammatic fashion a flow chart for practicing the process in accordance with this invention. Reactor 11 is equipped with an agitator 13 driven by a motor (not shown), a temperature sensing means (now shown), a sparging means 15 for introducing a gas into the reactor 11and a scrap introduction means 17 made up of hopper 19, barrel 21 and auger23. The auger is provided with a motor means (not shown) for rotating the auger 23 within barrel 21. The reactor 11 is provided with a means for controlling the temperature of the contents thereof. While any suitable control means may be employed, FIG. 1 depicts a container 25 having contents 27 which can be maintained at a suitable constant temperature by an external heating means (not shown). The contents 27 may be a salt bath for example. Container 25 is provided with a means (not shown) for raisingand lowering in order that reactor 11 can be positioned relative with respect to the contents 27 of container 25. A reservoir 29 is connected bymeans of conduit 31 with sparging means 15. Conduit 31 has disposed thereinpump 33 for delivering the contents of reservoir 29 to sparging means 15 via conduit 31. Conduit 31 has associated therewith a heating means which in the case as shown is a length of conduit 31 doubled upon itself and disposed within heating medium 27 in container 25. Reactor 11 is further provided with outlet means 35 connected to first distillation device 37 byconduit 39. Conduit 41 is provided to return the overheads from distillation device 37 to reservoir 29. Conduit 43 conveys the higher boilers to second distillation device 45.
In operation, oligomers of dimethylterephthalate and ethylene glycol are introduced into reactor 11 to at least approximately 50% of the volume of the reactor 11 and agitator 13 and heating means depicted as container 25 and contents thereof 27 actuated to bring the temperature of the oligomersto from about 220° C. to about 270° C. Scrap feeding means 17loaded with polyethyleneterephthalate scrap resin is actuated to deliver scrap resin to the contents of reactor 11. Pump 33 is actuated to deliver methanol from reservoir 29 through conduit 31 wherein the methanol is super-heated and delivered through sparging means 15 into the contents of reactor 11 as a vapor which passes through the solution of the polyethyleneterephthalate and the oligomer thereof. The methanol is recovered by passing out through outlet 35 through conduit 39 and distillation device 37 back through conduit 41 to the methanol reservoir 29. The recovered dimethylterephthalate and ethylene glycol also exits viaoutlet 35 through conduit 39, are separated from the methanol in distillingdevice 37 and past via conduit 43 to second distillation device 45 where the ethylene glycol is collected overhead while the dimethylterephthalate is removed below. It may be desirable for conduit 39 to be provided with aheating means in order to prevent the condensation of any of the three components exiting from reactor 11.
It is, of course, to be understood while the process described above is semi-continuous in nature, that the method in accordance with this invention may be carried out as a batch, a semi-continuous or continuous method. In the semi-continuous method depicted above, which involves the feeding of polyester scrap into the reactor at a rate substantially equivalent to product formation, impurities will accumulate in reactor 11 necessitating periodic clean out. In a continuous mode of operating the process in accordance with this invention for example, a small slip streamof the reactor contents would continuously be removed, the rate being basedon the rate of impurities being introduced into the reactor. An advantage associated with all of the three techniques, whether it be batch, semi-continuous or continuous, is that any catalyst employed in the preparation of the virgin poly(ethyleneterephthalate) resin will not enterthe product vapor stream but will be removed along with the impurities due to the low volatility of these catalysts.
The invention will be illustrated by the following examples in which parts are by weight unless otherwise specified:
EXAMPLE 1
A reactor 11 is charged with 2000 parts of polyethylene terephthalate oligomers containing a mixture having between 10 and 20 repeating units heated to about 250° C. to render the mass molten. Clean polyethylene terephthalate powder is fed by means 17 at the rate of 3.5 parts/minute and methanol is feed at the rate of 20 part by volume and sparged through the molten resin by means 15. The methanol is returned to reservoir 29 via distillation column 37 and conduit 41. The dimethyl terephthalate and ethylene glycol are recovered from distillation column 45.
EXAMPLE 2
A reactor similar to that of Example 1 is charged with about 630 parts of the oligomer mixture of Example 1 heated to about 225° C. to renderit molten. Methanol is feed to the sparging means 15 at a rate of 4 parts by volume/minute and ground scrap polyethylene terephthalate bottles including polyolefin bottom cups, aluminum bottle caps, labels and any adherents used for the labels and bottom caps are fed to the reactor at a rate of 2.5 parts/minute. As in Example 1 the methanol is returned to reservoir 29 and the ethylene glycol and dimethyl terephthalate recovered from distillation column 45. Crystalline dimethyl terephthalate with a light layer of polyolefins and aluminum collecting at the bottom of the melt are removed from the reactor.
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A method of recovering ethylene glycol and dimethyl terephthalate from scrap polyethylene terephthalate resins by dissolving the scrap in oligomers of the same monomers and passing methanol through the solution.
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BACKGROUND OF THE INVENTION
The present invention relates to methods and apparatus for stabilizing the idle speed of spark ignited internal combustion engine.
Prior U.S. Pat. application Ser. No. 044,328 filed May 31, 1979 discloses a method and apparatus for regulating idle speed of a spark ignited internal combustion engine by control of the ignition timing. In particular, the engine therein described is provided with a lean fuel-air mixture, to favorably influence the engine exhaust emission. The loss in the engine torque attributable to the lean mixture is recovered by providing a relatively high air throughout volume. The nominal ignition timing is relatively retarded, and the timing is advanced by a control circuit to stabillize the engine idling speed at a speed which approximates a desired value.
In German patent disclosure No. 2,221,354 there is described another method for stabilizing idle speed upon the occurrence of changes in engine load. In accordance with the disclosure, the ignition timing is advanced to compensate for increased engine load. Also, in order to compensate for the loss in output which results from a nominal retarded ignition timing, the volume of the mixture charge is increased.
German disclosure No. 2,725,460 discloses a governor wherein the volume of mixture provided to the engine is controlled in order to compensate for changes in engine load. A similar control is described in German disclosure No. 2,756,704. That document describes a system for control of air supply as a function of intake vacuum. Idling speed is increased during starting and warmup by an electrically generated control signal.
German disclosure No. 2,715,408 describes an idling speed governor wherein changes in load are compensated by changes in the volume of fuel supplied to the engine.
A characteristic of all of these prior art systems is that speed stabilization is obtained through variation of only a single engine control parameter. Consequently, the parameter must be varied over a range which is large enough to result in poor engine operation for some engine load conditions, or alternatively, full engine speed stabilization cannot be achieved. It is, therefore, an object of the present invention to provide a new and improved method and apparatus for controlling the idle speed of an internal combustion engine.
It is a further object of the invention to provide such an apparatus wherein such control parameter is varied over a predetermined selected range of values to ensure efficient and pollution free operation of the engine.
SUMMARY OF THE INVENTION
In accordance with the invention there is provided a method for operating a spark ignited internal combustion engine to stabilize the actual idle speed to be approximately eqyal to a desired idle speed. In accordance with the invention the engine is supplied with a lean fuel air mixture which has a high air ratio, exceeding the air-ratio corresponding to maximum mean indicated pressure. The ignition timing is controlled within a pair of selected timing limits to bring the actual idle speed toward the desired idle speed. The air ratio of the mixture is also controlled to bring the actual idle speed toward the desired idle speed.
In one embodiment, the air-ratio control is initiated only when the ignition timing reaches one of the limits. In another embodiment the air-ratio control is initiated after an extended time deviation of the actual idle speed from the desired idle speed.
According to the invention there is also provided an apparatus for stabilizing the idle speed of a spark ignited internal combustion engine having control signal operated adjustable ingition timing means and fuel metering means. The apparatus includes a first control device which responds to a first speed signal representing actual engine speed and a second speed signal representing desired engine speed. The first control device generates an ignition timing control signal for operation of the timing means, and for controlling the timing according to the difference between the first and second speed signals within the selected timing limits. There is also provided a second integrating control device, which responds to the timing control signal and the attainment of the timing limits for generating a fuel metering control signal for controlling the fuel metering means to change the air ratio of the mixture supplied to the engine.
In another embodiment the second integrating control device responds directly to the difference between the first and second speed signals, integrating the difference over time to generate a slowly changing fuel metering control signal.
In a preferred embodiment there may be provided a third control device, which responds to the output of the second control device for generating an air volume control signal, which regulates the volume of air supplied to the engine. It is possible to vary nominal values for engine speed, ignition timing, air ratio and air volume according to the actual operating temperature of the engine.
The method in accordance with the invention provides initially for a rapid regulation of the idling speed toward the nominal speed by modification of the ignition angle, i.e., in case of a sped decrease by adjusting the ignition in the direction toward an advance. In the event that the actual idling speed deviates from the desired speed over an extended period or, in the event that on modification of the ignition angle, the predetermined limit values thereof should be attained, a modification of the air ratio will occur for further stabilization of the idling speed. This modification of the air ratio may be subdivided, first, into a modification of the fuel quantity, and second a modification of the air volume supplied. The second "stage", modification of the air volume is initiated through the attainment of predetermined limit values for the modification of the delivered fuel quantity. A rapid response of the control is obtained due to the modification of the ignition angle which becomes effective very rapidly, namely, practically with the next-following ignition pulse. The modification of the air ratio becomes effective less rapidly and provides long-term stabilization so that variation of the ignition angle constituting the first stage remains available for regulating short-term and limited changes in the idling speed.
For a better understanding of the present invention, together with other and further objects, reference is made to the following description taken in conjunction with the accompanying drawings, and its scope will be pointed out in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a functional block diagram illustrating the apparatus of the present invention.
FIG. 2 is a functional block diagram of an alternate embodiment of the present invention.
FIGS. 3, 4 and 5 are graphs plotting mean indicated pressure as functions of air ratio, air volume, and ignition timing for various engine operating conditions.
DESCRIPTION OF THE INVENTION
Two examples of arrangements for carrying out the method in accordance with the invention will be described with reference to the functional block diagrams of FIGS. 1 and 2 and the graphs of FIGS. 3, 4 and 5. The diagrams in FIG. 3 refer to idling stabilization solely through adjustment of the ignition timing which is, the first state of the stabilization method of the present invention and which hereinafter is also designated as digital idling stabilization (DIS). FIG. 4 represents the corresponding diagrams for engine operation according to a method wherein, in addition to DIS there is provided, for speed stabilization, an adjustment of the air ratio through change of the fuel quantity delivered. This stage of adjustment is hereinafter designated as digital idling enrichment (die). In particular, air ratio adjustment serves to ensure, during cold start and warming up the engine an increased mean indicated pressure in the combustion chambers, which yields a higher torque. The higher torque is needed to overcome the higher friction of the engine under cold operating conditions. FIG. 5 contains similar graphs as FIGS. 3 and 4, for engine operation in which, in addition to the adjustment of the ignition timing and air ratio, there is also provided an adjustment of the air quantity delivered to the engine. This third stage of the method in accordane with the invention, on which the examples of embodiments illustrated are based, is designated hereinafter as digital airflow enhancement (DAE).
Referring to FIG. 1, there is shown a block diagram of a control circuit according to the present invention. In the FIG. 1 circuit signals representing the actual engine speed N a and the desired idle speed N d are provided to a comparison circuit 12, which provides an output representing the deviation of the actual idle speed N a from the desired idle speed N d . This deviation signal is provided to a first control device 11 which acts as linear-integrating circuit and provides an output representing ignition timing advance α z which is time-dependent. Thus, the first controller 11 converts the idling speed deviation or error signal into adjustment of the ignition timing within an ignition timing range which is defined by two ignition timing limit values α z max and α z min. These limit values are selected to have values which ensure that timing variation is not great enough to impair engine operation. Thus, they constitute ignition timing operating limits.
The starting value α zO of the ignition timing, which is a pre-selected nominal value, is within the timing range defined by the limit values so that it is possible to make adjustments to the ignition timing towards an advance and towards a delay.
The corresponding nominal values λ O and m LO for air ratio and air volume in the two further stages of the arrangement have been selected in accordance with these considerations.
The ignition timing starting value αz O is delivered to a combining circuit 13 which, depending on the output signals of the first controller 11 proper, delivers adjustment signals for setting the ignition timing α z needed to stabilize the idling speed, to an ignition timing adjusting device in the internal combustion engine 14. Devices of this kind are known in themselves and therefore need not be described here.
The output signals of the combining circuit 13 and the nominal value α zO of the timing advance are provided to the combining circuit 16 and the input of the second control device 15. At the input to second control device 15 there are connected in parallel, for improvement of the regulation dynamics, the three-state threshold circuit 26 with hysteresis characteristics and the delay element 17. Delay element 17 is connected as a feedback around theshold circuit 26 to form a pulse-width modulator.
Deviations from regulation of the idling speed are counteracted initially by adjustment of the ignition timing. Should this not be sufficient, that is, should such large adjustment of the ignition timing be required that the timing reaches one of the limit values, further control of the idling speed is achieved by adjustment of the fuel quantity delivered. In the FIG. 1 embodiment, the fuel quantity adjustment is obtained through changing the length t i of fuel injection pulses. Thereby there is delivered via the second control device 15, which in this case is designed for a selected characteristic of the reciprocal value 1/λ of the air ratio plotted against the time t, the prescribed value is supplied (in form of a correction value) to the succeeding air ratio control circuit 19. Here again a maximal and a minimal threshold value each are provided for the inverse air ratio. Moreover, a nominal value 1/λ for the inverse air ratio is supplied to combining circuit 18, which generates an error for the air ratio. The air ratio control circuit 19, to which this error signal is delivered, supplies a signal determining the injection time t i to the fuel metering device in the internal combustion engine 14. In the example of the embodiment described, the said metering device is the customary fuel injection means. As a matter of principle, it may, of course, also be a carburetor.
As indicated above, the air ratio range has selected values. In the event that further modification of the air ratio should become necessary, namely in the sense of an alternate regulation due to attainment of one of the limit values of the reciprocal value of the air ratio, the control device 20 is actuated by way of the combining circuit 21. Threshold circuit 22 and delay element 23, which operate similar to correponding circuit 16, 26 and 17. Control device 20 provide a control signal which adjusts the air volume m L , within a range defined by the limit values m L max and m L min, as a function of the set air ratio λ or its reciprocal value. The output signal for the air volume, which determines the air volume m L and which is obtained in the combining circuit 24 through comparison with the initial value m LO of the air volume, is delivered to a flap or a valve in the suction system of the internal combustion engine, for example, the throttle valve in the customary intake pipe, or an additional intake air valve.
Thus, as soon as due to an outside moment M w (resistance moment) during idling. There is a decrease of the actual value N a of the speed of the internal combustion engine, in accordance with its time behavior 25. The control apparatus of FIG. 1 will act in three stages of adjustment to cause an increase in the mean pressure p mi in the combustion spaces of the internal combustion engine, which will increase the torque M a produced by the engine to compensate for the disturbance moment M w .
In a preferred embodiment, engine temperature can be taken into account by selecting the values of nominal idle speed N d , nominal ignition timing α zo , nominal air ratio λ o and nominal air volume m LO .sub.. These values can be selected according to the sampled temperature of the engine oil or water from a programmed memory or the like. The combining circuits 12, 13, 16, 18, 21 and 24 are thus provided with temperature-dependent rather than constant nominal values, so that as a result, a speed-controlled warming-up system is obtained.
Analogous considerations also apply to the embodiment shown in FIG. 2. Here, again we find a control device 30, which, in this embodiment is a linear controller, and which is associated with a combining circuit 31 forming the difference between the nominal engine speed N d and the actual engine speed N a . This first control device 30 thus serves to deliver to the internal combustion engine 32 an error signal for adjustment of an ignition timing α z . Thus the control circuit responds to a lower engine speed caused by an addition moment M w by an increase in the ignition timing advance, which increases mean indicated pressure and output torque.
In the FIG. 2 embodiment, the idling speed error signal is delivered by way of the further combining circuit 33 to the second control device 34, which is an integral controller and becomes practically effective only after a given period of time has lapsed. Thus, there occurs here a partial overlap of the operation of the control devices 30 and 34. In the event that in spite of the (rapid) operation of the controller 30, the idle speed deviation should continue for an extended period of time, the (slower) second control circuit 34 becomes effective and causes a modification of the injection timing t i and thereby a corresponding modification of the fuel quantity delivered and the air ratio. As in the example of the embodiment shown in FIG. 1, the modification range of the air ratio and, respectively, its reciprocal value 1/λ is limited by predetermined limit values, and as soon as one of these limit values is attained, the control circuit containing the adjustment drive 35 in addition to the enabling circuit and delay elements becomes effective and brings about a change of the air throughout volume in a manner already described. Thus, a three-stage control is achieved by variation in succeeding the stages of the ignition timing, air ratio and air throughout volume.
For a further understanding of the functioning of the invention, reference is made to the graphs in FIGS. 3, 4 and 5. In each figure the diagram to the left shows the mean indicated pressure p mi in the combustion chambers of the internal combustion engine as a function of the air ratio λ. The middle diagram of each figure shows the dependence of the mean indicated pressure upon the air throughout m L . The diagram to the right in each figure shows the correlation between the mean indicated pressure and the ignition timing advance a z . I all cases idling is assumed.
The working point 1 of the engine shows the currenty customary idling adjustment with a rich mixture and relatively small air throughput. The disadvantage of such adjustments consists in high CO and HC emissions in the exhaust gas. For this reason, and also for reasons of control engineering, the method in accordance with the invention departs from a working point 2 of the internal combustion engine on the downward sloping branch of the air ratio diagram appearing on the left side in the figures, that is, from a lean mixture control. Because of the lean mixture the mean pressure p mi and thereby the torque delivered during idling by the engine drop, the air throughout m L must be increased so that the working point 3 in the diagrams is attained. Control difficulties now arise if the ignition timing setting is selected in the customary manner in accordance with point 3, as indicated in the right-hand diagrams. This ignition angle is so close to the maximum of the indicated mean pressure that an advance of the ignition point would hardly increase the mean pressure. Thus, in order to obtain an improved range of ignition timing control, the nominal setting of the ignition timing is moved to point 4, that is, the ignition is considerably retarded, and the loss in indicated mean pressure resulting therefrom is compensated by a further enlargement of the air throughput to point 5.
When the engine is warm, stabilization of the idling speed can be achieved by adjustment of the ignition timing within the range designated by points 5 and 6. This range is therefore characterized by "DIS" (digital idling stabilization).
FIG. 4 is based on FIG. 3 and concerns the case of creating a deviation of the idling speed due to low engine temperature, such as present during warming up. In this case, a wider margin from the lean operating limit must be ensured through enrichment of the mixture. Therefore, there is provided in addition to the speed control through change of the ignition angle DIS, an increase of the fuel quantity, that is, DIE (digital idling enrichment). The advantage of such a regulation in comparison with a general mixture enrichment during idling may be found in the fact that a mixture enrichment occurs only if a drop in speed actually signals a need for increased fuel delivery.
Whereas the starting point for a DIS is a change in the right-hand diagram of FIGS. 3, 4 and 5, an increase of the indicated mean pressure p mi occurs with DIE through decrease of the air ratio λ, so that each of the left diagrams forms the starting point. Thus the control characteristic of the DIS is enlarged to the hatched area in the diagrams of FIGS. 4 and 5.
FIG. 5 shows the effect of all three steps of the method in accordance with the invention, namely, idling stabilization (DIS) through modification of the ignition angle, idling enrichment (DIE) through modification of the fuel quantity supplied and addition of air (DAE=digital air enhancement), i.e., a change of the air ratio through modification of the air throughput volume m L . As becomes clear from FIG. 5, there is thus obtained a larger control range for influencing the indicated mean pressure p mi without the attainment by the manipulated variable, namely the ignition angle, air ratio and air throughput of any values which would impair the operation of the engine.
In FIG. 5, line 7 shows the required minimum value of the mean indicated pressure when the engine is warm, whereas line 8 shows the corresponding minimum value when the engine temperature is lower. It is clear that shifting the ignition point alone in the direction towards an advance will not be sufficient to cover the mean pressure needed when the internal combustion engine is cold. As already explained with reference to FIG. 1, there can be obtained selected nominal values not only for the ignition angle, but also for the air ratio and the air throughput as a function of temperature, for example, by way of a memory circuit .
The invention offers a method for regulating undesirable idling speed changes, which result from either a change in the engine temperature or from outside moments such as accessories, without the need for the operating parameters of the engine to assume values which are critical for its operation. Application of the method in accordance with the invention is capable of simplifying the automatic starting mechanism customary for vehicle engines.
Those skilled in the art of control circuits will recognize that the control functions herein described can be achieved using various specific circuits. One approach is to use analog circuitry which directly uses signals with voltage proportional to the quantities represented. Another approach is to convert measured quantities, such as engine speed into digital signals and generate the needed control signals digitally using either discrete control elements or a programmed microprocessor. Hybrid arrangements using a combination of digital and analog techniques are also possible.
While there have been described what are believed to be the preferred embodiments of the invention, those skilled in the art will recognize that other and further modifications may be made thereto without departing from the spirit of the invention and it is intended to claim all such embodiments as fall within the true scope o the invention.
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Engine idle speed is stabilized by a successive three stage control system which sequentially regulates ignition timing, fuel quantity and air throughput volume.
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FIELD OF THE INVENTION
This invention relates to a cutting bit for use in mining and construction operations. More particularly, this invention relates to a rotatable cutting bit including an extraction undercut to assist in the removal of the cutting bit from a bore in a cutting bit block.
BACKGROUND OF THE INVENTION
Various styles of rotatable cutting bits for use in mining and construction operations are well known. For example, one common style of rotatable cutting bit useful in mining and construction operations has a generally conical shape working head having secured to the apex of the head by brazing an axially disposed insert of cemented tungsten carbide. Depending from the conical shape working head is a shank which is inserted into a bore within a cutting bit block.
During mining and construction operations the cutting bit is generally utilized in a machine having a power driven cutter wheel. The power driven wheel is mounted on a horizontal shaft with the plane of the wheel disposed vertically. The wheel has on its periphery an array of cutting bits mounted in a plurality of permanent cutting bit blocks adapted to hold the carbide tipped cutting bits. The cutting bit blocks typically include a bore of a cylindrical shape having a substantially cylindrical opening. The cutting bits are mounted generally tangentially on the peripheral rim of the supporting wheel so that through the rotation of the wheel about its axis, the cutting bits may attack the material to be broken up by the horizontal reach of the cutting bits operating in a vertical plane.
Exemplary of a cutting bit block and a cutting bit for use on a construction machine is U.S. Pat. No. 4,201,421. U.S. Pat. No. 4,201,421 discloses a cutting bit including a spring sleeve of cylindrical form with a slot extending the full length of the spring sleeve along substantially all of the shank of the cutting bit. The cutting bit is inserted shank first into the bore of the cutting bit block such that the spring sleeve frictionally engages the inside wall of the bore keeping the cutting bit in a working position on the rim of the wheel. During operation of the construction machine the cutting bits impact against a material to be worked thereby breaking the material into small fragments. As the cutting bits repetitively impact against the material to be worked, some of the small material fragments may work between the cutting bits and corresponding cutting bit blocks thereby wedging the cutting bits into the bore of the cutting bit blocks and preventing free rotation of the cutting bits and subsequent removal of the cutting bits from the bit blocks as required. The effect of the small material fragments pressed between the bit blocks and the cutting bits is that the removal of the cutting bits from the bit blocks is difficult, if not impossible, thereby necessitating increased machine downtime and expense.
Previously, a removal tool having a wedge shaped tine was driven between the conical cutting head and the bit block to pry the bit from the block. However, because the loose fragments of material are packed so tightly around the conical cutting head and the bit block, insufficient clearance is provided between the cutting head and the bit block for the removal tool to enter between the conical cutting head and the block.
To alleviate the aforementioned problems, we have invented a conical flanged cutting bit having a working head and a supporting shank depending therefrom. Formed integral with the base of the working head is an undercut. The undercut allows for the free insertion of a cutting bit removal tool to assist in the removal of the cutting bit from the socket mount. In a preferred embodiment, the undercut comprises opposing triangular cutouts to provide a variable reaction surface upon insertion of the bit removal tool within the undercut between the cutting bit and the cutting bit block.
Accordingly, one aspect of the present invention is to provide a conical flanged cutting bit including an undercut at the base of the conical flange to receive a bit removal tool. Another aspect of the present invention is to provide a conical flanged cutting bit including an undercut at the base of the conical flange to receive a bit removal tool that is simple and economical to manufacture.
SUMMARY OF THE INVENTION
Briefly, according to this invention, there is provided a flanged conical cutting bit including at least one tapered undercut to receive a bit removal tool. The cutting bit includes a conical nose and an integral depending cylindrical shank. The conical nose includes a flange portion of a diameter greater than the shank positioned between the conical nose and the shank. The flange portion is of a circular circumference and has a planar underside including at least one undercut extending radially inward from the exterior surface of the flange portion.
In a preferred embodiment, the undercuts are spaced in an opposing paired relationship about the planar underside of the flange portion of the cutting bit. The undercuts extend radially inwardly from the exterior of the periphery of the circumference of the planar underside of the flange to form triangular shaped undercuts having a curved hypotenuse equivalent to the curvature of the circumference of the flange.
In a preferred embodiment, the undercuts taper upwardly from the underside surface of the flange toward the conical nose of the cutting bit. The undercuts taper upwardly at an angle of approximately 15 degrees from a line extending transversely from a longitudinal axis of the cutting bit.
The present invention also contemplates, in combination, the cutting bit as previously described and a bit block for rotatably holding the cutting bit. The undercut and face of the bit block cooperatively provide a variable opposing resistance surface between the undercut and face of the bit block to receive a tine of a cutting bit removal tool.
BRIEF DESCRIPTION OF THE DRAWINGS
Further features and other aspects of this invention will become clear from the following detailed description made with reference to the drawings in which:
FIG. 1 is a partial fragmentary side view of a conical cutting bit in accordance with the present invention sealed within a cutting bit block;
FIG. 2 is an end view of the conical cutting bit of FIG. 1;
FIG. 3 is an isometric view of the conical cutting bit of FIG. 2; and
FIG. 4 is an isometric view of a conical cutting bit is accordance with another aspect of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to the drawings in which the reference characters refer to similar parts throughout the several views, FIG. 1 illustrates a rotatable flanged cutting bit 10 in accordance with the present invention secured within a bore 18 of a bit block 20 which may be attached to a rotating drum of a mining or construction machine of a type well known in the art. The rotatable flanged cutting bit 10 includes a working head having a generally conically shaped nose portion 12 and a depending shank portion 14 having a reduced diameter section which is adapted to receive a split annular spring retainer 16 of a type well known in the art.
The shank 14 of the cutting bit 10 is that portion which is inserted into the bore 18 formed within the bit block 20. The shank 14 is of a circular cross-section and is formed integral with and depends from the conically shaped nose portion 12. The shank 14 includes an annular recess 22 formed intermediate the rearward end of the cutting bit and the conically shaped nose portion 12. The split annular retainer 16 surrounds the annular recess and fits slidably within the bore 18 of the bit block 20.
As shown in FIG. 1, the cutting bit 10 and spring retainer 16 are fully inserted in the bore 18 of the bit block 20 and the cutting bit is ready to be used for the desired function. The spring sleeve retainer 16 loosely embraces the shank 14 of the cutting bit 10 thereby maintaining the underside of the cutting bit flush with a flat bearing surface of the bit block 20. The spring sleeve retainer 16 exerts a strong hold on the inner surface of the bore 18 to resist axial movement of the cutting bit 10 as the cutter wheel previously described herein rotates.
The split spring retainer 16 is longitudinally slotted and is preferably made of a resilient metal such as AISI 1050 spring steel heat treated to Rockwell C 45-50. The split spring retainer should have sufficient resilience when it is contracted to produce an adequate holding force for retaining the spring retainer in position when disposed around the cutting bit within the bore 18.
As shown in FIGS. 1-4, the conical nose portion 12 of the cutting bit 10 includes a flange 24 and tip 26. The conical nose portion 12 of the cutting bit 10 diverges from the tip 26 of the cutting bit rearwardly to the flange 24 positioned intermediate the tip of the conical nose portion and the shank 14 of the cutting bit. Secured within the tip 26 of the cutting bit 10 is an insert 28. The insert 28 is preferably made of a cemented metal carbide such as cobalt tungsten carbide but may be made of any other material suitable for the intended purpose of the cutting bit 10. The shape of the insert 28 may be as shown or of any other known insert shape or composition as exemplified by U.S. Pat. Nos. 4,725,098; 4,497,520; 4,859,543.
The flange 24 of the cutting bit 10 is of a generally truncated frustoconical shape extending radially outward beyond the tip 26 of the conical nose portion 12 and terminating in a planar underside 30. It will be appreciated that the flange 24 of the cutting bit 10 protects the face 32 of the bit block 20 against premature wear from abrasion with the work surface. Formed within the planar underside 30 of the flange 24 are undercuts or recesses 34 to receive the tines of a bifurcated fork removing tool of a type well known in the art.
Although the present invention is illustrated in connection with a flanged cutting bit 10 having a split retainer 16, it will be appreciated that the present invention may be applied with equal facility to other types of cutting bits employing different retainer systems. For example, the teachings of the present invention may also be utilized with a U94KHD cutting bit employing a short retainer as sold by Kennametal Inc. Accordingly, the style of retainer to secure the flanged cutting bit within the cutting bit block or the type of flanged cutting bit is not a limitation on the practice of the present invention.
The undercuts or recesses 34 may be of most any shape and size suitable to provide an opening between the planar underside 30 of the flanged cutting bit 10 and the face 32 of the bit block 20 when the cutting bit is seated within the bit block. As shown in FIGS. 1-3, the undercuts 34 extend radially inwardly from the exterior of the periphery of the circumference of the underside of the flange 24 to form triangular shaped undercuts in which the triangle hypotenuse 36 is also coincident with and follows the curvature of the circumference of the flange. The top surface 38 of the undercuts 34 taper upwardly from the underside planar surface 30 of the flange 24 toward the conical nose 12 of the cutting bit 10. The undercuts 34 may taper upwardly at an angle of approximately 15 degrees from the underside planar surface 30 of the cutting bit 10. The taper of the undercut 34 provides a variable opposing resistant surface between the undercut and the face 32 of the bit block 20 upon insertion of the tine of the removal tool within the opening formed between the bit block and the cutting bit.
In an alternative embodiment of the present invention as shown in FIG. 4, the undercut or recess 34 may be of a generally arcuate shape having a planar top surface 38.
The undercuts 34 are arranged circumferentially about the underside of the flange 24 to provide sufficient surface area to uniformly support the rotating cutting bit 10 upon the opposing flat face 32 of the bit block 20 as the bit cuts a work surface. As shown in FIGS. 3 and 4, the undercuts 34 are arranged in a spaced opposing paired relationship about the underside of the flange 24 of the cutting bit 10.
Upon insertion of the cutting bit 10 into the bore 18 of the bit block 20, the underside planar base of the flange 24 is firmly seated upon the opposing face 32 of the bit block. The undercuts 34 in cooperation with the face 32 of the bit block 20 provide an opening which allows for the free insertion of the tines of a bit removal to extract the bit from the bit block without damaging the socket mount or the head of the cutting bit.
The documents, patents and patent applications referred to herein are hereby incorporated by reference.
Having described presently preferred embodiments of the invention, it is to be understood that it may be otherwise embodied within the scope of the appended claims.
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A cutting bit including a conical nose and an integral depending cylindrical shank. The conical nose includes a tip having a hard wear resistant insert and a flange positioned between the tip and the shank and having a diameter greater than the shank. The flange has a planar underside including at least one undercut extending radially inward from the exterior peripheral surface of the flange to provide in cooperation with the face of a cutting bit block a resistance surface for insertion of a tine of a cutting bit removal tool.
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FIELD OF THE INVENTION AND RELATED ART
[0001] The present invention relates to a liquid container for storing liquid such as ink. In particular, it relates to a liquid container, a liquid container holder, and a recording head cartridge, for an ink jet recording apparatus which records letters, pictures, etc., on recording medium by ejecting ink.
[0002] There have been proposed various recording heads, for example, a wire dot recording head, a thermal recording head, a thermal transfer recording head, an ink jet recording head, etc., for a recording apparatus for recording images on recording medium, for example, paper, fabric, plastic sheet, OHP (overhead projector) sheet, etc.
[0003] Among the recording apparatuses which employ one of the above described recording heads, an ink jet recording apparatus (ink jet printer) has been used as an outputting means (printer) of an information processing system, more specifically, a copying machine, a facsimileing machine, an electric typewriter, a wordprocessor, a workstation, etc., or as a portable printer for a personal computer, a host computer, an optical disc apparatus, an video apparatus, etc.
[0004] An ink container for supplying a recording head with ink comprises: a container in which ink is held; an ink absorbing member which absorbs and holds ink, and a lid which keeps the container sealed.
[0005] There are two types of recording heads: a recording head integral with an ink container, and a recording head, to which an ink container is removably attachable.
[0006] In recent years, various ink jet recording apparatuses, which employ a recording head comprising an replaceable ink container, have come to be widely used, because they have been improved in reliability, and also, they are been reduced in operational cost. Some of them are usable for recording in color, and have a plurality of replaceable ink containers, for example, two replaceable ink containers, four replaceable ink containers, etc. In the case of an ink jet recording apparatus having two replaceable ink containers, one container contains black ink, and the other contains color inks (cyan, magenta, and yellow). In the case of an ink jet recording apparatus having four replaceable ink containers, the four ink containers contain four inks (black, cyan, magenta, and yellow inks), one for one.
[0007] In the case of a recording head cartridge employing a single of plurality of replaceable ink containers, it must be assured that ink is reliably supplied from the ink containers of the recording head cartridge to the recording head of the recording head cartridge. Thus, one of the most important prerequisites concerning recording quality is that the ink containers and recording head are accurately positioned relative to each other.
[0008] Thus, an ink container and an ink container holder are desired to be structured to assure that the ink container can be easily mounted into the ink container holder. More specifically, they are desired to be structured so that, in order to prevent the ink container and ink container holder from being damaged when mounting the former into the latter, it is made impossible for a user to incorrectly mount the ink container, or forcefully mount the ink container, into the ink container holder. Therefore, an ink container and an ink container holder, in accordance with the prior art (which hereinafter may be referred to as “conventional ink container and ink container holder”), are provided with guiding means for guiding the ink container into the ink container holder.
[0009] At this time, the structures of the ordinary conventional ink container and ink container holder (for example, those disclosed in Japanese Laid-open Patent Application 2001-25308) will be described will reference to the appended drawings. FIG. 9 is a side view of the conventional replaceable ink container 102 , and FIG. 10 is a bottom plan view of the ink container 102 .
[0010] As will be evident from FIGS. 9 and 10, the ink container 102 is provided with a pair of guiding projections 140 , which are on the side walls, one for one, of the ink container 102 , parallel to the direction in which the ink container 102 is mounted into the ink container holder 114 , and which engage with the guide rails of the ink container holder 114 , which will be described later. These guiding projections 140 project outward of the ink container 102 , in the direction perpendicular to the lateral walls 170 of the ink container 102 . The ink container 102 is also provided with a pair of outwardly projecting locking claws 142 , which are on the front wall of the ink container 102 , in terms of the direction in which the ink container 102 is mounted into the ink container holder 114 , being next to the bottom wall 176 of the ink container 102 . Further, the ink container 102 is provided with a latching lever 130 , which is on the rear wall 182 of the ink container 102 , in terms of the direction in which the ink container 102 is mounted into the ink container holder 114 . The latching lever 130 is provided with a latching claw, which engages with the ink container holder 114 , securing thereby the ink container 102 to the ink container holder 114 ; the latching claw is kept pressured outward, being thereby kept engaged with the ink container holder 114 , by the reactive force generated by the resiliency of the latching lever 130 as the lever 130 is pressed inward, that is, toward the rear wall of the ink container 102 . The ink container holder 114 will be described later.
[0011] The ink container 102 is also provided with a finger tab 144 , which is located at the rear end of the top wall of the ink container 102 , and which is to be grasped from the rear side of the ink container 102 when inserting the ink container into the ink container holder 114 , in order to insert the ink container 102 into the ink container holder 114 , from the front wall 172 side of the ink container 102 . Further, the ink container 102 is provided with three ink outlets 188 , one for each of the three different inks in the ink container 102 . The three ink outlets 188 are in the bottom wall 176 .
[0012] FIGS. 11 ( a ), 11 ( b ), and 11 ( c ) are phantom side views of the combination of the ink container 102 and ink container holder 114 , showing the steps for mounting the ink container 102 into the ink container holder 114 .
[0013] Referring to FIG. 11( a ), first, the ink container 102 is inserted into the ink container holder 114 , from the front wall 172 side. As the ink container 102 is inserted, the pair of guiding projections 140 engage with the pair of guiding rails of the ink container holder 114 , one for one. Then, the ink container 102 is horizontally guided by a pair of guiding rails 146 , toward the rear wall 166 of the ink container holder 114 . During this step, not only the guiding rails 146 horizontally guide the ink container 102 toward the rear wall 166 , but also toward the bottom wall 176 of the ink container holder 114 , that is, the vertical direction. As a result, the locking claw 142 of the ink container 102 is caught by the locking claw 148 of the rear wall 166 of the ink container holder 114 , as shown in FIG. 11( b ).
[0014] Next, the ink container 102 is pressed downward as indicated by an arrow mark X in FIG. 11( b ). As a result, the ink container 102 is pushed into the ink container holder 114 , while being rotated in such a manner that the rear end portion, that is, rear wall 182 portion, of the ink container 102 comes into contact with the bottom surface 168 of the ink container holder 114 . As the ink container 102 is pushed downward into the ink container holder 114 , the latching lever 130 is temporarily bent toward the rear wall 182 of the ink container 102 .
[0015] Then, at virtually the same moment as the rear end (wall 182 ) of the ink container 102 comes into contact with the bottom wall 168 of the ink container holder 114 , the latching claw 154 of the latching lever 130 engages into the latching level locking hole 150 of the ink container holder 114 , securing the ink container 102 to the ink container holder 114 while accurately positioning the ink container 102 relative to the ink container holder 114 , as shown in FIG. 11( c ).
[0016] Also referring to FIG. 11( c ), as the ink container 102 is properly mounted into the ink container holder 114 , the ink supply tube 136 presses on a porous member (unshown), as an ink holding member, in the ink container, making the portion of the porous member, in the adjacencies of the ink supply tube 136 , greater in capillarity. The portion of the porous member, which is greater in capillarity, draws ink toward the ink supply tube 136 so that the ink is supplied to a recording head (unshown) through the ink supply tubes 136 .
[0017] On the other hand, when removing the ink container 102 , the latching lever 130 is to be temporarily bent toward the rear wall 182 of the ink container 102 against the resiliency of the lever 130 in order to disengage the latching claw 154 from the latching lever locking hole 150 . Then, the ink container 102 is to be pulled upward by the finger tab 144 of the ink container 102 until the bottom rear end of the ink container 102 comes out of the ink container holder 114 . After the rear end of the ink container 102 comes out of the ink container holder 114 , the finger tab 144 of the ink container 102 is to be grasped and pulled in the direction opposite to the direction in which the ink container 102 is inserted into the ink container holder 114 , in order to pull the ink container 102 out of the ink container holder 114 . As the ink container 102 is pulled in the above described direction, the guiding projections 140 of the ink container 102 slide on the guiding rails 146 , one for one, raising thereby the ink container 102 away from the bottom wall 168 of the ink container holder 114 . As a result, the ink supply tubes 136 are moved out of the ink outlets 188 of the ink container 102 , being thereby prevented from interfering with the removal of the ink container 102 .
[0018] The above described conventional ink container and ink container holder, however, suffer from the following problems.
[0019] That is, the ink container and ink container holder for a portable printer need to be small, because a portable printer needs to be small in overall size. Therefore, they need to be structured so that they are smaller in the amount of the space required for mounting the ink container into the ink container holder, or removing the ink container therefrom.
[0020] In the case of an ink container holder such as the above described conventional one, however, the overall size of an ink container holder is substantially affected by the thickness of its walls of the ink container holder positioned in a manner to surround each of the ink container held by the holder, and also, by the width of its guiding rails; in other words, the thickness of the walls of the ink container holder and the width of the guiding rails of the ink container holder impose limits on the size reduction of a conventional ink container holder.
[0021] In addition, in the case of some of conventional ink container holders capable of accommodating multiple ink containers, a black ink container mountable therein is different from each of color ink containers mountable therein, in terms of the movement they make when they are mounted into an ink container holder. Thus, it is quite difficult to realize an ink container holder which is substantially smaller than a conventional ink container holder, and yet, is capable of preventing the problem that a recording head, etc., become damaged by being incorrectly mounted.
[0022] Further, an idea of modifying a conventional ink container in design so that the ink container will not come into contact with an ink container holder when it is mounted into the ink container holder has been taken into consideration, as a means to prevent an ink container holder, etc., from being damaged when an ink container is mounted into the ink container holder. However, this idea is problematic in that it reduces the internal volume, that is, ink capacity, of an ink container.
SUMMARY OF THE INVENTION
[0023] Thus, the primary object of the present invention is provide a liquid container, which is substantially smaller than a liquid container in accordance with the prior art, and which can be reliably mounted into an ink container holder, without being damaged, or damaging the ink container holder, even if it is incorrectly mounted into the ink container holder.
[0024] Another object of the present invention is to provide a liquid container, which is substantially smaller than a liquid container in accordance with the prior art, is compatible with a recording apparatus substantially smaller in size than a recording apparatus in accordance with the prior art, and yet, is not substantially smaller in liquid capacity than a liquid container in accordance with the prior art, can be reliably mounted into an ink container holder, and is reliable in liquid delivery.
[0025] According to the present invention made in order to accomplish the above described objects, a liquid container removably mountable in an ink container holder comprises a front locking portion and a rear locking portion, and a container proper for containing liquid. Only one of the lateral walls of the container proper, parallel to the direction in which the liquid container is inserted into the liquid container holder, is provided with a projection. When the liquid container is mounted into the liquid container holder, the liquid container rotates about the front locking portion thereof, with the projection being guided by the top edge of the guiding wall of the liquid container holder, whereas the other side of the liquid container, that is, the side opposite to where the projection is located, being regulated by the internal surface of the corresponding lateral wall of the liquid container holder.
[0026] When a liquid container structured as described above in accordance with the present invention is mounted into a liquid container holder structured as described above in accordance with the present invention, the projection on one of the lateral walls of the liquid container, parallel to the liquid container insertion direction, is guided by the top edge of the guiding wall of the liquid container holder, and the other lateral wall of the liquid container is regulated by the internal surface of the liquid container holder. Therefore, as the liquid container is mounted into the liquid container holder, it rotates about the front locking portion. Further, as the liquid container is mounted into the liquid container holder, the front and rear locking portions of the liquid container engage with the liquid container holder. In other words, according to the present invention, the space occupied by one of the pair of guiding projections on the two lateral walls, parallel to the liquid container insertion direction, of a liquid container in accordance with the prior art, can be eliminated. Therefore, not only is it possible to reduce the size of a liquid container while assuring that the liquid container is reliably mounted into a liquid container holder, but also to assure that even if the liquid container is incorrectly mounted into a liquid container holder, the liquid container holder, etc., are not damaged.
[0027] These and other objects, features, and advantages of the present invention will become more apparent upon consideration of the following description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0028] [0028]FIG. 1 is a perspective view of the ink jet recording head cartridge in the first embodiment of the present invention; (a) showing the ink container in the ink container holder, and (b) showing the ink container having been removed from the ink container holder.
[0029] [0029]FIG. 2 is a perspective view of the ink jet recording head cartridge shown in FIG. 1; (a) showing the ink container in the ink container holder, and (b) showing the ink container having been removed from the ink container holder.
[0030] [0030]FIG. 3 is a plan view of the ink jet recording head cartridge shown in FIG. 1.
[0031] [0031]FIG. 4 is a sectional view of the black ink container.
[0032] [0032]FIG. 5 is a sectional view of the color ink container.
[0033] [0033]FIG. 6 is a perspective view of the combination of the ink container and ink container holder, showing in sequence the steps for mounting the ink container into the ink container holder.
[0034] [0034]FIG. 7 is a perspective view of the ink jet recording head cartridge in the second embodiment of the present invention.
[0035] [0035]FIG. 8 is a plan view of the ink jet recording head cartridge shown in FIG. 7; (a) showing the ink container in the ink container holder, and (b) showing the ink container having been removed from the ink container holder.
[0036] [0036]FIG. 9 is a side view of an ink container in accordance with the prior art.
[0037] [0037]FIG. 10 is a bottom plan view of the ink container in accordance with the prior art.
[0038] [0038]FIG. 11 is a phantom side view of the combination of the ink container and ink container holder in accordance with the prior art, showing in sequence the steps for mounting the former into the latter; (a) showing the ink container which has just begun to be mounted into the ink container holder, (b) showing the ink container which is being mounted into the ink container holder, and (c) showing the ink container having just been completely mounted into the ink container holder.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0039] Hereinafter, the preferred embodiments of the present invention will be described with reference to the appended drawings.
[0040] (Embodiment 1)
[0041] [0041]FIGS. 1 and 2 are perspective views of the recording head cartridge in the first embodiment of the present invention. FIG. 1( a ) shows the recording head cartridge in the ink container holder, and FIG. 1( b ) shows the recording head cartridge, which is not in the ink container holder. FIG. 2 shows the recording head cartridge as seen from the side opposite to the side from which the cartridge is seen in FIG. 1. FIG. 3 is a plan view of the recording head cartridge.
[0042] As will be evident from FIGS. 1, 2, and 3 , the recording head cartridge 1 in this embodiment comprises: a recording head (unshown) for ejecting ink; a black ink container 3 for supplying the recording head with black ink; a color ink container 4 for supplying the recording head with color inks; and an ink container holder 5 into which the black ink container 3 and color ink container 4 are removably mountable.
[0043] The recording head, which is not shown, is attached to the ink container holder 5 , and has plural rows of nozzles for ejecting ink, and plural electrically resistant elements for generating the thermal energy for ejecting the ink supplied from an ink container. The plural rows of nozzles are different in the color of the ink they eject. The recording head forms an image by ejecting ink with the use of the thermal energy generated by the electrically resistant elements; the so-called film-boiling phenomenon is used to eject ink.
[0044] Obviously, the application of the present invention is not limited to the above described ink ejection mechanism. For example, it is also applicable to some of the well-known ink ejection mechanisms, in accordance with the prior art, such as an ink ejection mechanism which employs a piezoelectric ink ejection system, an ink ejection mechanism structured to use electrical charge, and the like ink ejection mechanism.
[0045] Referring to FIGS. 1 ( b ) and FIG. 2( b ), the ink containers 3 and 4 are provided with a container proper 31 and a lid 32 . The container proper 31 is in the form of a box, which cannot be open on the bottom side, and has a storage chamber in which ink is to be held. The lid 32 is for covering the opening (unshown) of the container proper 31 .
[0046] The lid 32 has through holes (unshown), and labyrinthine grooves (unshown). The through holes reach inward of the ink containers 3 and 4 from outside the lid 32 . The labyrinthine grooves are in the outward surface of the lid 32 , and extend from the through holes to the peripheries of the lid 32 . The labyrinthine grooves are covered with a sheet 40 so that they are exposed to the ambient air only at the peripheries of the lid 32 ; air vents are provided. With the provision of this structural arrangement, it is possible to minimize the amount by which the inks in the ink containers 3 and 4 evaporate from the air vents 42 ; virtually no inks in the ink containers 3 and 4 evaporate from the air vents 42 . The bottom wall of the container proper 31 is provided with a plurality of ink outlets 35 through which inks are supplied to the ink container holder 5 side.
[0047] The ink container holder 5 is provided with a plurality of ink delivery tubes 23 through which ink is taken in from the ink containers 3 and 4 . The ink delivery tubes 23 are in the bottom walls of the first and second ink container compartments 11 and 12 , which will be described later. Each ink delivery tube 23 is provided with a filter 23 , which is located at one end of the ink delivery tube 23 . It is in the formed of a chimney. As the ink container 3 ( 4 ) is mounted into the ink container holder 5 , the filter 24 of each ink delivery tube 23 of the ink container holder 5 is placed in contact with the ink retaining portion located inward of the corresponding ink outlet 33 of the ink container 3 ( 4 ), and the elastic members 25 attached to the ink container holder 5 so that they surround ink delivery tubes 23 , one for one, airtightly seal between the adjacencies of the ink outlets 33 and the adjacencies of the ink delivery tubes 23 , one for one, preventing ink from evaporating or leaking, and therefore, making it possible for ink to be desirably delivered to the recording head. In order to assure that the adjacencies of the ink outlets 33 and ink delivery tubes 23 are airtightly sealed, the elastic members 25 may be shaped so that their cross sections, parallel to the direction in which they are compressed, look like the cross section of the bell portion of a trumpet, parallel to its axial direction. Obviously, a piece of sealing tape or a rubber plug may be used instead of the elastic member 25 ; ink outlet is sealed with the sealing tape or rubber plug, which will be penetrated by the needle-tipped ink delivery tube of the ink container holder, when an ink container is mounted into the ink container holder. In other words, the elastic member 25 may be replaced with a component different in structure from the elastic member 25 , as long as the ink delivery (supply)-joint between the ink container and ink container holder 5 remains airtightly sealed.
[0048] Next, the structures of the black ink container 3 and color ink container 4 will be described in more detail with reference to the appended drawings.
[0049] [0049]FIG. 4 is a sectional view of the black ink container 3 , and FIG. 5 is a sectional view of the color ink container 4 . Incidentally, the internal structures of the black and color ink containers 3 and 4 in this embodiment, which will be described next, are not intended to limit the scope of the present invention.
[0050] First, the black ink container 3 for black ink will be described with reference to the drawings.
[0051] As shown in FIG. 4, the container proper 31 of the black ink container 3 contains an absorbent member 34 as an ink retaining member, and an ink delivery member 35 . This ink retaining member 34 absorbs and retains black ink. The ink delivery member 35 is positioned between the absorbent member 34 and ink outlet 33 , with its top surface being airtightly in contact with the absorbent member 34 so that ink outlet 33 is sealed at the inward end.
[0052] The absorbent member 34 and ink delivery member 35 are both capable of absorbing and retaining ink. In terms of the ink retainment property (capillarity), however, the ink delivery member 35 is made greater than the absorbent member 34 . With this setup, the ink retained in the absorbent member 34 is smoothly drawn into the ink delivery member 35 , improving thereby the efficiency with which the ink remained in the absorbent member 34 is consumed.
[0053] As the material for the absorbent member 34 and ink delivery member 35 , fiber formed of thermoplastic resin such as poly-olefin was used. More specifically, a certain number of pieces of web formed by arranging thermoplastic fibers virtually in parallel were layered, and compressed in the direction perpendicular to the webs. As the material for the absorbent member 34 , the fibrous material, which was roughly 6.7 [dtex] in the fiber thickness, was compressed to a density of roughly 0.09 μg/cm 3 was used. As for the material for the ink delivery member 35 , fibrous material, which was roughly 2.2 [dtex] in the fiber thickness, was compressed to a density of roughly 0.20[g/cm 3 ].
[0054] Incidentally, the container proper 31 and lid 32 of the ink container 3 ( 4 ) in this embodiment are formed of resinous material, in particular, poly-olefin, that is, the same material as the material for the absorbent member 34 and ink delivery member 35 , due to environmental concerns, more specifically, in order to drastically improve the amount by which the ink container 3 ( 4 ) can be recycled or reused.
[0055] The black ink container 3 is structured so that it can be removably mounted in the ink container holder 5 . More concretely, the black ink container 3 is provided with a locking claw 36 for preventing the black ink container 3 from dislodging from the ink container holder 5 after the mounting of the black ink container 3 into the ink container holder 5 . The locking claw 36 is an integral part of the black ink container 3 and projects from the bottom of the front wall of the black ink container 3 , in terms of the direction in which black ink container 3 is inserted into the ink container holder 5 . The locking claw 36 engages with the black ink container locking hole 26 of the ink container holder 5 , and keeps the black ink container 3 solidly secured to the ink container holder 5 .
[0056] The black ink container 3 is also provided with a latching lever 37 , which engages with the ink container holder 5 . The latching lever 37 is also an integral part of the black ink container 3 , being on the side opposite to where the locking claw 36 is present. It is elastically bendable in the direction indicated by an arrow mark a 1 in FIG. 4, and springs back into the original position in the direction indicated by an arrow mark a 2 in FIG. 4. It is attached to the bottom wall portion of the container proper 31 of the black ink container 3 by its base port-ion, and has a latching claw 38 , which is on the outward surface of the top portion of the latching lever 37 . The latching claw 38 engages with the ink container holder 5 .
[0057] The latching lever 37 projects at a predetermined angle from the bottom portion of the container proper 31 , so that the distance between the latching lever 37 and the container proper 31 gradually increases toward the top portion of the black ink container 3 . It is provided with a finger placement spot 39 by which the latching lever 37 is to be-pressed toward the container proper 31 in order to elastically deform the latching lever 37 when disengaging the latching claw 38 from the ink container holder 5 . The finger placement spot 39 is located at the tip of the latching lever 37 .
[0058] When the black ink container 3 is mounted into the ink container holder 5 , the latching lever 37 comes into contact with the rear lateral wall 21 of the ink container holder 5 , being thereby elastically bent by the wall 21 in the direction indicated by the arrow mark a 1 in FIG. 4, and the latching claw 38 of the latching lever 37 engages with the latching lever locking hole 27 of the ink container holder 5 , which will be described later.
[0059] Next, the color ink container 4 for the recording head 1 will be described. The structure of the color ink container 4 is basically the same as the above described structure of the black ink container 3 shown in FIGS. 1, 2, and 3 .
[0060] Referring to FIG. 5, the color ink container 4 in this embodiment comprises a container proper 31 , in the form of a topless box, in which three inks different color are held, and a lid 32 which covers the opening (unshown) of the container proper 31 .
[0061] The container proper 31 has three independent chambers which are separated by two parallel partitioning walls 41 , and in which three inks different in color are held one for one. The two parallel partitioning walls 41 are positioned perpendicular to the two parallel lateral walls of the color ink container 4 , by which the lateral movements of the color ink container 4 are controlled when the container 4 is mounted into the ink container holder 5 . Thus, the three chambers are parallel to each other, and overlap with each other in the lengthwise direction of the bottom wall of the container 4 .
[0062] The three chambers contain absorbent members 34 Y, 34 M, and 34 C, which absorb and retain yellow, magenta, and cyan inks, respectively. The bottom wall of the color ink container 4 has ink outlets 33 Y, 33 M, and 33 C, which lead to three chambers, one for one, and the openings of which are aligned in the lengthwise direction of the bottom wall.
[0063] The structures of the three chambers are the same as the above described structure of the black ink container 3 , and therefore, they will be not described here.
[0064] Also in the case of the color ink container 4 , fiber formed of thermoplastic resin such as poly-olefin is used as the material for the absorbent members 34 and ink delivery member 35 . More specifically, a certain number of pieces of web formed by arranging thermoplastic fibers virtually in parallel are layered, and compressed in the direction perpendicular to the webs. For the absorbent member 34 , the fibrous material, which was roughly 6.7 [dtex] in the fiber thickness, was compressed to a density of roughly 0.07-0.09[g/cm 3 ]. For the ink delivery member 35 , fibrous material, which was roughly 2.2 [dtex] in the fiber thickness, was compressed to the density of roughly 0.20[g/cm 3 ].
[0065] The lid 32 is also virtually the same as that for the black ink container 3 , except that the lid 32 of the color ink container 4 has three air vents 43 , one for each chamber, and that it is structured to hermetically separate the three chambers from each other. Therefore, it will be not described here.
[0066] The structure for removably securing the color ink container 4 to the ink container holder 5 is the same as the above described structure for the black ink container 3 ; it comprises a locking claw, and a latching lever with a latching claw as does that of the black ink container 3 . Referring to FIG. 1( b ), the ink outlets 33 Y, 33 M, and 33 C are aligned in the direction parallel to the plane which includes the center lines of the latching claw 38 and locking claw 36 , and which is perpendicular to the bottom wall of the color ink container 4 . Further, they are positioned closer to one of the lateral walls (walls parallel to ink container insertion direction) of the color ink container 4 than the other.
[0067] In other words, the ink outlets 33 , the presence of which are likely to weaken the mechanical strength of the areas of the bottom wall of the color ink container 4 , in which they are positioned, are positioned in the adjacencies of one of the ridges which the bottom wall and one of the lateral walls of the container proper 31 , that is, the portion of the container proper 31 which is relatively high in rigidity. Therefore, the amount by which the container proper 31 is reduced in mechanical strength by the presence of the ink outlets 33 is minimized. Moreover, the two portions (locking claw 36 and latching claw 38 ) for securing the black ink container 3 and color ink container 4 to the ink container holder 5 are also positioned in the adjacencies of one of the lateral walls of the container proper 31 as are the ink outlets 33 . Therefore, the black ink container 3 and color ink container 4 can be reliably mounted into the ink container holder 5 , without causing the ink containers 3 and 4 to become twisted, and can be solidly secured to the ink container holder 5 in spite of the presence of only a small number of ink container locking means.
[0068] In particular, aligning the ink container securing means and ink outlets in a single plane as in this embodiment, minimizes the amount by which the ink containers are twisted when the ink containers are mounted into the ink container holder. In other words, with the provision of the above described structural arrangement, even if an ink container is provided with two or more ink outlets, the ink container can be reliably mounted into the ink container holder, without becoming substantially twisted, as long as the ink outlets are aligned in the same manner as those of the color ink container in this embodiment. Further, positioning the ink container securing means in the adjacencies of one of the lateral walls of the container proper makes it possible to place the ink container positioning mechanism on the area of the container proper, which is relatively high in mechanical strength, making it therefore possible to obtain an ink container reliably mountable in the ink container holder, that is, making it possible to obtain an ink container, the ink outlets 33 of which are reliably connected to the ink delivery tubes 23 . The above described structural arrangement for an ink container is extremely beneficial for reducing the thickness of the walls of an ink container in order to increase the internal volume of the ink container without increasing its external size.
[0069] Incidentally, not only does “aligning the container locking means and ink outlets in a single plane” means that the axial lines of the openings of the ink outlets 33 coincides with the plane which includes the center lines of the locking claw 36 and latching claw 38 , but also that they coincide with the line connecting the centers of the ink locking claw 36 and latching claw 38 .
[0070] Referring to FIG. 2( a ), the black ink container 3 is provided with a guiding projection 43 , which is on only one of the lateral walls of the black ink container 3 , which is parallel to the ink container insertion direction, and the color ink container 4 is also provided with a guiding projection 43 , which is also on only one of the lateral walls of the color ink container 4 , which are parallel to the ink container insertion direction. The guiding projection 43 of the black ink container 3 guides the black ink container 3 along the guiding rail 28 of the ink container holder 5 when the black ink container 3 is mounted into the ink container holder 5 , and the guiding projection 43 of the color ink container 4 guides the color ink container 4 along the guiding rail 29 of the ink container holder 5 when the color ink container 4 is mounted into the ink container holder 5 .
[0071] Next, the ink container holder 5 in this embodiment will be described in detail with reference to the drawings.
[0072] Referring to FIGS. 1, 2, and 3 , the ink container holder 5 is roughly in the form of a topless box having the first ink container compartment 11 in which the black ink container 3 holding black ink is removably mounted, and the second ink container compartment 12 in which the color ink container 4 holding color inks is removably mounted. The first and second ink container compartments 11 and 12 are positioned next to each other, and are effected by the lateral walls 21 of the ink container holder 5 and a partitioning wall 22 . That is, the space surrounded by the lateral walls 21 of the ink container holder 5 is divided by the partition wall 22 , into two sub-spaces, or two compartments, into which the black ink container 3 and color ink container 4 are mounted one for one.
[0073] Referring to FIG. 1( b ), one of the lateral walls 21 of the ink container holder 5 (left lateral wall in FIG. 1( b )), which is parallel to the direction in which the black ink container 3 is mounted into the first ink container compartment 11 , is provided with the guiding rail 28 , which smoothly guides the black ink container 3 , while regulating the movement thereof, when the black ink container 3 is mounted into, or removed from, the ink container holder 5 .
[0074] Also referring to FIG. 1( b ), the partitioning wall 22 of the ink container holder 5 is shaped so that its top edge functions as the guiding rail 29 which smoothly guides the color ink container 4 into the second ink container compartment 12 , while regulating the movement of the color ink container 4 , when the color ink container 4 is mounted into, or removed from, the ink container holder 5 .
[0075] In other words, the ink container holder 5 is provided with only two guiding rails, that is, one guiding rail 28 and one guiding rail 29 . The guiding rail 28 is on one of the lateral walls of the ink container holder 5 , parallel to the ink container insertion direction, and the guiding rail 29 is the specifically contoured top edge of the partitioning wall 22 of the ink container holder 5 . Therefore, the ink container 3 ( 4 ) is guided from only one side, in terms of the ink container insertion direction. The guide rail 28 ( 29 ) has a horizontal portion which is roughly parallel to the bottom wall of the ink container holder 5 , and a tilted portion which is tilted downward, in terms of the direction perpendicular to the bottom wall of the ink container holder 5 , as seen from the trailing side in terms of the ink container insertion direction. The horizontal and tilted portions are continual.
[0076] As the ink container 3 ( 4 ) is mounted into the ink container holder 5 , they are guided, horizontally as well as diagonally downward, by the guide rail 28 ( 29 ), respectively, until the container 3 ( 4 ) reaches the bottom wall of the ink container compartment 11 ( 12 ).
[0077] The role of the guide rail 28 ( 29 ) is to regulate the movement of the ink container 3 ( 4 ) in order to prevent the problem that when the ink container 3 ( 4 ) is mounted into the first (second) ink container compartment 11 ( 12 ), the ink container holder 5 is damaged due to the contacts between the ink-container 3 ( 4 ) and the ink delivery tubes 23 of the ink container holder 5 . More specifically, the ink delivery tube 23 of the first ink container compartment 11 , that is, the space for the black ink container, is located roughly at the center of the bottom wall of the first ink container compartment 11 , in terms of the lengthwise direction of the compartment 11 , which is parallel to the ink container insertion direction. In comparison, the three ink delivery tubes 23 , one for each color ink, of the second ink container compartment 12 , that is, the space for the color ink container 4 , are aligned in the ink container insertion direction. Thus, the possibility that the color ink container 4 will come into contact with the ink delivery tubes 23 of the ink container compartment 12 is greater than the possibility that the ink container 3 will come into contact with the ink delivery tube 23 of the ink container compartment 11 . Therefore, in this embodiment, the guiding rail 28 for the black ink container 3 is made different in shape from the guiding rail 29 for the color ink container 4 , optimizing thereby the movement of the ink container 3 ( 4 ) in order to prevent the ink container 3 ( 4 ) from coming into contact with the ink delivery tubes 23 .
[0078] The first (second) ink container compartment 11 ( 12 ) of the ink container holder 5 is provided with a locking hole 26 , into which the locking claw 36 of the ink container 3 ( 4 ) engages, and which is virtually at the bottom (in immediate adjacencies of bottom wall). The first (second) ink container compartment 11 ( 12 ) of the ink container holder 5 is provided with a locking hole 27 , into which the latching claw 38 of the latching lever 37 of the ink container 3 ( 4 ) engages. The locking hole 27 is located at the opposite end of the ink container holder 5 from the locking hole 26 . The top edge of the this wall of the ink container compartment 11 ( 12 ) of the ink container holder 5 having the locking hole 27 functions as a second guiding portion, which comes into contact with the bottom wall of the ink container 3 ( 4 ), guiding thereby the ink container 3 ( 4 ) while controlling the movement thereof, when the ink container 3 ( 4 ) is mounted into the ink container compartment 11 ( 12 ) of the ink container holder 5 .
[0079] Next, the movement of the ink container 3 ( 4 ), which occurs as it is mounted into the ink container holder 5 , will be described.
[0080] [0080]FIG. 6 is a perspective view of the combination of the color ink container 4 and ink container holder 5 , showing the movement of the color ink container 4 , which occurs during the mounting of the color ink container 4 into the ink container holder 5 .
[0081] The movement of the color ink container 4 , which occurs during the mounting into the ink container holder 5 , is basically the same as that of the black ink container 3 . Thus, only the movement of the color ink container 4 , which occurs during the mounting of the color ink container 4 into the ink container holder 5 , will be described; the movement of the black ink container 3 will not be described.
[0082] [0082]FIG. 6( a ) shows the color ink container 4 in the initial stage of the mounting of the color ink container 4 into the ink container holder 5 , and FIG. 6( b ) shows the color ink container 4 in the middle stage of the mounting of the color ink container into the ink container holder 5 , in which the ink container 4 is being guided by the guiding rail 29 of the ink container holder 5 . FIG. 6( c ) shows the color ink container 4 in the final stage of the mounting of the color ink container 4 into the ink container holder 5 , in which the color ink container 4 has just been completely mounted into the ink container holder 5 .
[0083] First, referring to FIG. 6( a ), as the color ink container 4 is inserted into the ink container holder 5 , from the front wall side, that is, the side opposite to the latching lever 37 , the guiding projection 43 of the color ink container 4 , which projects a predetermined distance from the bottom end of the front wall of the color ink container 4 , comes into contact with the guiding rail 29 of the ink container holder 5 .
[0084] Next, referring to FIG. 6( b ), as the color ink container 4 is further inserted, the guiding projection 43 slide on the guiding rail 29 , with the rear end portion of the color ink container 4 being in contact with the walls of the ink container holder 5 , that is, being supported by the wall of the ink container holder 5 , which is in contact with the color ink container 4 by its top edge. Further, the front portion of the color ink container 4 is supported by the guiding rail 29 , by the guiding projection 43 of the container 4 . Therefore, all that is necessary to smoothly mount the color ink container 4 into the ink container holder 5 is to simply push the color ink container 4 into the ink container holder 5 .
[0085] The color ink container 4 and ink container holder 5 are designed so that there will be a predetermined amount of clearance between each of the aforementioned lateral walls of the color ink container 4 and the corresponding wall of the ink container holder 5 when mounting the former into the latter. Therefore, when mounting the color ink container 4 into the ink container holder 5 , the color ink container 4 tends to slightly wobble in the direction (left and right direction in FIG. 1( b )) perpendicular to the cartridge insertion direction, in the second ink container compartment 12 of the ink container holder 5 .
[0086] However, this slight wobble of the color ink container 4 in the direction perpendicular to the lateral walls of the color ink container 4 , which occurs while the color ink container 4 is mounted into the ink container holder 5 , is regulated by one of the lateral walls 21 of the ink container holder 5 , a part of which constitutes one of the lateral walls of the second ink container compartment 12 , and the portioning wall 22 having the guiding rail 29 . More specifically, it is regulated by the inward surface of the above described wall 21 of the ink container holder 5 , and one of the surfaces of the partitioning wall 22 . Further, as described above, the guiding projection 43 is specifically positioned so that the bottom wall of the color ink container 4 does not interferes with (contacts) the ink delivery tubes 23 , etc., of the bottom wall of the ink container holder 5 . In other words, with the provision of the above described structural arrangement, it is unnecessary for the color ink container 4 to be modified in external shape, in consideration of the interference between the color ink container 4 and the components of the ink container holder 5 , that is, in order to prevent the color ink container 4 from interfering with the ink delivery tubes 23 , etc., of the second ink container compartment 12 of the ink container holder 5 ; it is unnecessary for the color ink container 4 to be given such an external shape that reduces the internal volume of the color ink container 4 . Therefore, the color ink container 4 in this embodiment can be smoothly mounted into, or removed from, the ink container holder 5 , even though its internal volume is just as large as a color ink container in accordance with the prior art.
[0087] As described above, the distance by which the guiding projection 43 of the color ink container 3 ( 4 ) projects from the external surface of the ink container 3 ( 4 ), must be large enough to assure that the projection 43 will engage with the guiding rail 28 ( 29 ) to correctly guide the ink container 3 ( 4 ) when the ink container 3 ( 4 ) is mounted into, or removed from, the ink container holder 5 . On the other hand, increasing the distance by which the guiding projection 4 projects increases the possibility that the projection 43 will come into contact with the vertical wall of the ink container holder 5 and/or the lateral wall of the ink container in the adjacent ink container compartment. Such contacts between the projection 43 and the vertical wall of the ink container holder 5 and the lateral wall of the ink container in the adjacent ink container compartment generate friction, that is, container restraining force, which interferes with the insertion of the ink container 3 ( 4 ) into the ink container holder 5 . Therefore, the distance by which the projection 43 projects must be set to be large enough to assure that it will not fail to rest on the guide rail 28 ( 29 ), but small enough not to cause unnecessary interferences.
[0088] In other words, the ink container 3 ( 4 ), and ink container holder 5 are desired to be structured to satisfy the following inequality (FIG. 6):
D>C> ( B−A ) (Inequality 1)
[0089] A: external dimension (exclusive of guiding projection 43 ) of container proper 31 , in terms of the direction parallel to the direction in which ink container 3 ( 4 ) is inserted into the ink container holder 5 ;
[0090] B: internal dimension of the first (second) ink container compartment 11 ( 12 ) of the ink container holder 5 , in terms of the direction parallel to the direction in which ink container 3 ( 4 ) is inserted into the ink container holder 5 ;
[0091] C: distance by which the projection 43 on one of the lateral walls of the ink container 3 ( 4 ) projects from the lateral wall; and
[0092] D: thickness of the guiding rail 28 ( 29 ) of the ink container holder 5 .
[0093] With the measurements of A−D set to satisfy Inequality 1, it is assured that when ink container 3 ( 4 ) is mounted into, or removed from, the first (second) ink container compartment 11 ( 12 ) of the ink container holder 5 , the guiding projection 43 of the ink container 3 ( 4 ) will properly rest the guiding rail 28 ( 29 ) of the ink container holder 5 , and will be smoothly guided by the guiding rail 28 ( 29 ) without becoming disengaged therefrom. Further, the aforementioned contacts which interfere with the mounting of the ink container 3 ( 4 ) into the first (second) ink container compartment 11 ( 12 ) do not occur.
[0094] Further, as described above, the ink container 3 ( 4 ) slightly wobbles left and right when it is mounted into the ink container holder 5 . Even though this wobbling movement of the left (right) side of the ink container 3 ( 4 ) having the guiding projection 43 which is guided by the guiding rail 28 ( 29 ), perpendicular to the bottom wall of the first (second) ink container compartment 11 ( 12 ), is properly regulated, the wobbling movement of the right (left) side of the ink container 3 ( 4 ), that is, the side opposite to where the guiding rail 28 ( 29 ), perpendicular to the bottom wall of the first (second) ink container compartment 11 ( 12 ), is not regulated. Therefore, when the ink container 3 ( 4 ) is mounted into the ink container holder 5 , it becomes slightly tilted relative to one of the lateral walls 21 of the ink container holder 5 , and the partition wall 22 of the ink container holder 5 . Naturally, therefore, the shape of the guiding rail 28 ( 29 ) and the shape of the guiding projection 43 are desired to be designed in consideration of the angle at which the ink container 3 ( 4 ) tilts as described above.
[0095] In particular, in the case of an structural arrangement in which the ink outlets 33 Y, 33 M, and 33 C are positioned closer to one of the lateral walls of the ink container holder 5 , parallel to the ink container insertion direction, it is desired that the lateral wall of the ink container holder 5 closer to the ink outlets 33 Y, 33 M, and 33 C is provided with a guiding mechanism similar to the aforementioned guiding projection of the ink container 3 ( 4 ), the guiding rail 28 ( 29 ) of the ink container holder 5 , etc.
[0096] Further, it is possible for the guiding projection 43 , with which the ink container 3 ( 4 ) is provided, to be deformed by the external force to which the ink container is subjected when the ink container is mounted into, or removed from, the ink container holder 5 . Therefore, in order to improve the ink container 3 ( 4 ) in terms of operational reliability, it is desired that the guiding projection 43 is attached to the area of the ink container 3 ( 4 ), which is relatively greater in mechanical strength, for example, the joint between the external walls of the ink container 3 ( 4 ), more specifically, the joint between the front wall and one of the two side walls of the ink container 3 ( 4 ), parallel to the ink container insertion direction.
[0097] Referring to FIG. 6( c ), the mounting of the color ink container 4 ends as soon as the color ink container 4 , which is being pushed into the ink container holder 5 , comes into contact with the bottom wall of the ink container holder 5 , by virtually the entirety of its bottom surface. As will be evident from FIG. 6, during the insertion of the color ink container 4 into the ink container holder 5 , the locking claw 36 located at the bottom end of the front wall of the color ink container 4 is inserted into the locking hole 26 of the ink container holder 5 .
[0098] Then, the rear portion of the color ink container 4 is to be pushed in the direction indicated by an arrow mark E shown in FIG. 6( c ). As the rear portion is pushed in the above described direction, the color ink container 4 rotates about the locking claw 36 in the locking hole 26 . As a result, the latching lever 37 is forced into the ink container holder 5 , and the latching claw 38 of the latching lever 37 latches with the edge of the latching hole 27 , assuring that each of the ink outlets 33 of the color ink container 4 will remain properly connected to the corresponding ink delivery tubes 23 of the ink container holder 5 .
[0099] When the color ink container 4 is mounted into the ink container holder 5 as described above, it is assured that the ink delivery tubes 23 of the ink container holder 5 come into contact with the ink holding members (ink delivery member 35 ) in the ink outlets 33 of the color ink container 4 , one for one, and ink is reliably supplied to the recording head. Also, when the color ink container 4 is mounted into the ink container holder 5 as described above, each of the elastic members 25 fitted around the ink delivery tubes 23 , one for one, is compressed in its thickness direction, that is, the direction perpendicular to the bottom wall of the ink container holder 5 , airtightly sealing the adjacencies of the peripheral surface of each ink outlet 33 of the color ink container 4 and the adjacencies of each ink delivery tube 23 of the ink container holder 5 . Therefore, should ink leaks from between one of the ink outlets 33 of the color ink container 4 and the corresponding ink delivery tube 23 of the ink container holder 5 , the ink will be confined in the immediate adjacencies of the joint between the ink outlet 33 and ink delivery tube 23 .
[0100] On the other hand, when removing the color ink container 4 from the ink container holder 5 , the latching lever 37 is to be pushed in the direction indicated by an arrow mark F shown in FIG. 6( c ). As the latching lever 37 is pushed as described above, the latching claw 38 disengages from the edge of the latching hole 27 of the ink container holder 5 , allowing the color ink container 4 to be pulled out of the ink container holder 5 by grasping the rear end portion of the color ink container 4 . Then, as the color ink container 4 is pulled outward, the locking claw 36 of the color ink container 4 comes out of the locking hole 26 , and the color ink container 4 comes out of the ink container holder 5 in its entirety. Obviously, even when the color ink container 4 is pulled out of the ink container holder 5 , the movement of the guiding projection 43 (ink container 4 ) is regulated by the guiding rail 29 , and therefore, the ink delivery tubes 23 do not interfere with the movement of the color ink container 4 .
[0101] As described above, according to this embodiment, when mounting the ink container 3 ( 4 ) of the recording head cartridge 1 into the ink container holder 5 of the recording head cartridge 1 , or removing the ink container 3 ( 4 ) from the ink container holder 5 , one side of the ink container 3 ( 4 ) is guided by the guiding rail 28 ( 29 ), and the other side is directly regulated (guided) by one of the lateral walls of the ink container holder 5 . Therefore, it is assured that the ink container 3 ( 4 ) will not be incorrectly mounted into the ink container holder 5 .
[0102] Also according to this embodiment, the guiding rails 28 and 29 , and the guiding projections 43 , of the recording head cartridge 1 , which are for preventing the ink container 3 ( 4 ) from being incorrectly mounted into the ink container holder 5 , need to be provided only on one side of the ink container holder 5 and ink container 3 ( 4 ), respectively, in terms of the ink container insertion direction, making it unnecessary to provide the guiding rail 28 ( 29 ), and the guiding projection 24 , on both sides of the ink container holder 5 and ink container 3 ( 4 ), respectively, in terms of the ink container insertion direction, as in the case of a recording head cartridge in accordance with the prior art. In other words, the space necessary for one of the two sets of the guiding rails and guiding projections, which the prior art requires, can be eliminated to reduce in size the ink container 3 ( 4 ) and ink container holder 5 of a recording head cartridge.
[0103] Also according to this embodiment, the top edge of the partitioning wall 22 of the ink container holder 5 , is utilized as the guiding rail 29 , making it possible to reduce in size the ink container 3 ( 4 ), and ink container holder, of a recording head cartridge, compared to a recording head cartridge, in accordance with the prior art, in which the guiding rail is independent from the partitioning wall.
[0104] In other words, according to this embodiment, even a recording head cartridge, the black ink container 3 and color ink container 4 of which are different in their movements which occur when they are mounted into the ink container holder 5 , can be reduced in size while assuring that the recording head and the like will not be damaged by incorrect mounting of the black ink container 3 or color ink container 4 .
[0105] Incidentally, in the case of the above described embodiment, the latching lever 37 is employed as a means for securing the ink container 3 ( 4 ) to the ink container holder 5 . However, the application of the present invention does not need to be limited to a recording head cartridge employing a latching lever as the means for securing an ink container to an ink container holder. That is, the present invention is applicable to any recording head cartridge which efficiently regulates the movement of an ink container with the use of guiding rail, whether the lever of the ink container locking mechanism is on the ink container side, or ink container holder side, or whether the ink container securing system employs the locking lever or not.
[0106] Further, this embodiment is described with reference to the ink container which contains an ink absorbing member formed of fibrous material. The application of the present invention, however, does not need to be limited to such an ink container. For example, the material for the ink absorbing member may be formed of one of the known foamed material such as foamed urethane. Moreover, the application does not need to be limited to an ink container containing an absorbent member.
[0107] Further, the liquid to be held in an ink container does not need to be limited to the aforementioned black, cyan, magenta, and yellow inks. For example, it may be the liquid for forming a printed circuit, or the like liquid.
[0108] (Embodiment 2)
[0109] Next, the recording head cartridge in the second embodiment of the present invention will be described with reference to the appended drawings. The recording head cartridge in this embodiment is basically the same in structure as the above described recording head cartridge 1 in the first embodiment. Therefore, the components, portions, etc., of the recording head in this embodiment, which are the same as those in the first embodiment, will be given the same referential symbols as those given for the description of the first embodiment, and will not be described here.
[0110] [0110]FIG. 7 is a perspective view of the recording head cartridge and ink container holder in this embodiment. FIG. 7( a ) shows the ink container which is not in the ink container holder, and FIG. 7( b ) shows the pair of ink containers, and the ink container in which the ink containers are to be mounted. FIG. 8 is a plan view of the recording head cartridge.
[0111] The recording head cartridge 2 in this embodiment comprises: a recording head (unshown) for ejecting ink; a pigment ink container 6 which holds pigment black ink to be supplied to the recording head; a dye ink container 7 which holds dye black ink to be supplied to the recording head; and an ink container holder 8 in which the ink containers 6 and 7 are removably mounted.
[0112] The ink containers 6 and 7 are roughly the same in shape. The ink container 6 ( 7 ) is provided with an ink outlet 33 , which is in the middle of the bottom wall of the ink container container proper 31 . Therefore, the ink containers 6 and 7 are virtually the same in their movements which occur when they are mounted into the ink container holder 8 .
[0113] Referring to FIG. 7, each of the pigment black ink container 6 and dye black ink container 7 is provided with a guiding projection 43 for guiding the ink container 6 ( 7 ) along the guiding rail 30 of the ink container holder 8 when the ink container 6 ( 7 ) is mounted into the ink container holder 8 . The guiding projection 43 is on only one side of the ink container 6 ( 7 ), more specifically, the partitioning wall 44 side of the ink container 6 ( 7 ) in terms of the ink container insertion direction. The guiding rail 30 is the top edge of the partitioning wall 44 of the ink container holder 8 , and is shared by the ink containers 6 and 7 .
[0114] Structuring the ink containers 6 and 7 , and the ink container holder 8 , so that the guiding rail 30 , that is, the top edge of the partitioning wall of the ink container holder 8 , is shared by the two containers 6 and 7 , makes the thickness of the partitioning wall 44 equal to roughly twice the distance by which the guiding projection 43 of the ink container 6 ( 7 ) projects, increasing therefore the mechanical strength of the partitioning wall 44 . Further, with the provision of such a structural arrangement, if the ink container 6 ( 7 ) is inserted into the wrong ink container compartment, the guiding projection 43 of the ink container 6 ( 7 ) comes into contact with the lateral wall 21 of the ink container compartment 11 ( 12 ) of the ink container holder 8 , making it virtually impossible to insert the ink container 6 ( 7 ) further into the ink container holder 8 . In other words, the above described structural arrangement makes it possible to prevent the ink container 6 ( 7 ) from being mounted into the wrong ink container compartment.
[0115] Incidentally, this embodiment was described with the structural arrangement in which the guiding rail 30 , that is, the specifically contoured top edge of the partitioning wall 44 of the ink container holder 8 was shared by the ink containers 6 and 7 , which are mounted next to each other. However, the two guiding rails different in contour, as those in the first embodiment, may be provided as integral parts of the partitioning wall 44 of the ink container holder 8 .
[0116] Further, this embodiment was described with reference to the recording head which comprises two ink containers, and the ink container holder in which the two ink container are mounted. However, this embodiment is also applicable to a recording head comprising three or more ink containers, for example, black, cyan, magenta, and black ink containers, which are independent from each other.
[0117] As described above, according to the present invention, the guiding projection for guiding a liquid container when mounting the liquid container into a liquid container holder has to be on only one of the two lateral walls, parallel to the direction in which the liquid container is inserted into the liquid container holder, of the liquid container. In other words, the space occupied by one of the pair of guiding projections on the two lateral walls, parallel to the liquid container insertion direction, of a liquid container in accordance with the prior art, can be eliminated. Therefore, not only is it possible to reduce the size of a liquid container while assuring that the liquid container is reliably mounted into a liquid container holder, but also to assure that even if the liquid container is incorrectly mounted into a liquid container holder, the liquid container holder, etc., are not damaged.
[0118] While the invention has been described with reference to the structures disclosed herein, it is not confined to the details set forth, and this application is intended to cover such modifications or changes as may come within the purposes of the improvements or the scope of the following claims.
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A liquid container detachably mountable to a container holder, the container holder includes a container body for containing liquid and including a front side engaging portion and a rear side engaging portion for engagement with the container holder, the front side engaging portion and rear side engaging portion being disposed at a leading side and a trailing side, respectively with respect to an inserting direction of the container into the container holder; and a projection, provided on only one of lateral sides of the container body which extend parallel with the inserting direction, for being guided, when the container is mounted to the container holder, along an upper end of a guide wall provided in the container holder while the other lateral side is being limited by an inner surface of the container holder, and the container is being rotated substantially about the front side engaging portion.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to the field of nasal dilators and air filtration and, more particularly, to an interal nasal dilator incorporating filtration having two semi-spherically topped substantially cylindrical reticulated foam depth filters with an integral interconnecting resilient member and arculate band set for insertion into the user's nostrils for nasal dilation and air filtration.
2. Description of the Related Art
Millions of people suffer from nasal obstructions or physiological conditions that make nasal breathing difficult, uncomfortable, or impossible. Examples of such conditions include narrowing of the nasal valve, allergic reactions, enlarged adenoid tissue and swollen nasal mucosa. The nasal valve, named by P.S. Mink in 1903 is the narrowest area in the nasal cavity, the adjacent area being larger both upstream and downstream. The nasal valve is located at the junction of the upper lateral and lower lateral cartilages about one third of the way from the tip of the nose.
The mucus membranes in the nasal valve area are extremely vascular. Any inflammation in this area causes swelling of the vascular tissue, narrowing down the nasal valve space and causing difficulty breathing. Decongestants can often help to reduce the swelling and make it easier to breathe. However, they can have a deleterious effect after several days of use and may cause an increase in swelling.
The airflow resistance provided by the nasal airways during breathing is essential for good pulmonary function. The nose is responsible for most of this resistance and consequently within the nasal air passageways, the nasal valve functions as a sort of flow limiting device. However, if the nasal valve area is reduced due to mucusal swelling or because the outer wall tissue of the nasal passage draws in during inhalation, breathing through the nose becomes difficult creating a tendency to mouth breathe.
Breathing through the mouth bypasses the natural air handling system of the body thereby negating all the built-in physiological benefits. Some reasons nasal breathing is superior include: (1) air is held in the lungs longer thus facilitating the interchange of oxygen and carbon dioxide, (2) air passing through the nasal mucosa carries the stimuli to the reflex nerves that control breathing, (3) the nostrils and cilia filter the air, (4) the sense of smell is enhanced, (5) the air is warmed, moisturized or dehumidified, (6) the tendency to snore, a precursor of sleep apnea, is reduced and (7) common cold germs and bacteria are more easily intercepted and discarded.
The advantage of breathing through the nose clearly offers significant physiological benefits. This is especially so for athletes and others who participate in strenuous physical activities such as sports. They process a far greater volume of air than more sedentary people and consequently are sensitive to restrictions in the air pathways such as the nasal valve. Clearly, any approach that mitigates a reduced nasal passageway and filters the air at the same time offers significant health benefits to the millions of people who suffer from nasal obstructions or physiological conditions that make nasal breathing difficult, uncomfortable, or impossible.
One such approach is a surgical technique using alar batten grafts as described by Becker et al, Journal of Long-Term Effects of Medical implants, 13(3)259-269(2003). Another surgical technique is a revision rhinoplasty, internal valve stenosis as described by Becker et al. However, surgical intervention is expensive, time consuming and may not entirely ameliorate the problem.
For those seeking a non-surgical or non-pharmaceutical option, there is generally known prior art that teaches the use of nasal dilators. As defined by the Food and Drug administration, “a nasal dilator is a device intended to provide temporary relief from transient causes of breathing difficulties resulting from structural abnormalities and/or transient causes of nasal congestion associated with reduced nasal airflow.” A nasal dilator, therefore, decreases airway resistance and increases nasal airflow.
There are two kinds of nasal dilators, external and internal. The external dilator, which is not a feature of the present invention, is constructed from one or more layers of material upon which a truss member is attached, with a skin adhesive applied to adhere to the outside of the nose. The external nasal dilator acts with a pulling action against the truss member to pull on the external nose tissue to open the nasal passageways. The adhesive must have enough strength to hold the dilator to the nose but not too much so that it is difficult or painful to remove. The internal nasal dilator has historically been made of metal or plastic and is placed inside the nostrils. It opens the nasal passages by pushing the nostrils open by pressing on the interior nasal side walls.
As a second alternative to a surgical approach to treat nasal obstruction, many others have proposed the use of internal nasal dilators. Unfortunately, most have overlooked the advantages of coincident filtration.
Examples of US internal nasal dilator patents include:
Year
Number
Issued
Inventor
Title
6,328,754
2001
Marten et al
Nasal dilator
6,270,512
2001
Jean Rittmann
Internal nasal dilator
6,238,411
2001
Robert Thorner
Internal nasal dilator
6,106,541
2000
Charles Hurbis
Surgically implanted dilator
5,922,006
1999
Joe Sugarman
Nasal appliance
5,895,409
1999
Mehdizadeh
Nasal dilator
5,816,241
1998
Cook
Coiled nasal dilator
5,479,944
1996
Bjorn Petruson
Nasal devices
5,350,396
1994
Isaac Eliachar
Nasal splint
4,759,365
1988
Leo Askinazy
Spring coil wire device
4,414,977
1983
Rezakhany
Nasal dilator
4,201,217
1980
Robert Slater
Nostril expander
3,710,799
1973
Carlos Caballero
Nose dilator
3,460,533
1965
C. Riu Pla
Nasal expander-inhaler
2,515,756
1950
C. Bove
Nasal appliance
1,709,740
1929
J. R. Rogers
Nasal distender
1,672,591
1928
W. A. Wells
Nostril dilation
1,597,331
1926
H. Thurston et al
Nostril expander
1,481,581
1924
H. R. Woodward
Nostril expander
1,255,578
1918
C. Boxley
Nasal appliance
1,135,675
1915
G. E. Dixon
Nostril dilating device
1,077,574
1913
H. R. Woodward
Nostril expander
1,014,758
1912
A. C. Knowlson
Nostril expanding device
1,014,076
1912
F. M. McConnell
Nasal expander
851,048
1907
H. R. Woodward
Nostril expander
513,458
1894
W. A. Dayton
Nasal expander
Examples of US internal nasal dilator patent application publications include:
Year
Number
Pub.
Inventor
Title
2004/0059368
2004
Paz Maryanka
Nasal Cavity Dilator
2004/0147954
2004
Charles Wood
Internal nasal dilator
2003/0144684
2003
Ronald Ogle
Adjustable nasal dilator filter
Examples of foreign internal nasal dilator patents include:
Year
Number
Issued
Inventor
Title
Country
DE19736717
1998
M. F. B. Velasquez
Nostril
Germany
expander
CH689199
1998
Berthod Remy
Nasal
Switzerland
passage
expander
A review of the prior art teaches that solutions were being sought for nasal breathing impediments for two centuries. Generally the devices proposed in the patents are suitable for their intended purposes but suffer from the significant disadvantage of no coincident filtration. For example, both U.S. Pat. No. 6,270,512 issued to Rittman and U.S. Pat. No. 6,238,411 issued to Thorner do not incorporate any filtration, as does the present invention. The depth filter of the present invention incorporates reticulated foam that captures and holds contaminates by providing a tortuous path for the air flow to follow as it passes through the filter media. A foam depth filter has the greatest particle retention efficiency and airflow while still maintaining the lowest pressure drop of all the common filter materials. Also, both Rittman and Thorner teach the use of a hard spring like material that fits within the nostril—0.020″ gauge steel wire (Rittman) and phos-bronze spring material (Thorner). Unlike the present invention that utilizes soft gentle foam to hold the dilator in place, the use of metal spring material can be uncomfortable to insert in the nostrils and difficult to adjust for various nose shapes and sizes.
Two internal nasal dilator patent application publications U.S. 2003/0144684, Ogle and U.S. 2004/0147954, Wood, teach air filtration in addition to internal nasal dilation. Ogle teaches of two 0.050 inch diameter nylon loops joined by a retaining tube. Upon careful insertion in the nostrils the nylon loops apply an outward force to the inside of the nasal tissue walls causing dilation. Ogle also teaches that the loops will cause a static electrical charge as air moves over the nylon loops and that this charge will capture particulate. Unlike the present invention, which utilizes a highly efficient depth filter, it is unlikely that the 0.050″ thick nylon loops situated in the mucosa of the inside of the nose will generate a meaningful static charge of sufficient amount to facilitate particulate capture. In addition, the loop diameter is so small that the loops may cause discomfort or erode the inside of the nose.
Wood teaches of two tapered housings that are intended to be inserted in the nostrils. The tapered housings are constructed of a resilient material configured as an open framework of tubular mesh in the manner of nasal filter prior art. Wood teaches that various filtering media can be placed within the tubular framework to filter air prior to introduction into the lungs. Unlike the present invention, which incorporates a resilient member to provide the dilation force, the tapered shape must be inserted further into the nose to achieve greater dilation. Depending upon the angle of the housing taper, the device could be very uncomfortable to insert and wear. The tapered shape is extremely stiff in the axial direction, possibly causing great discomfort during insertion. Also, there are small, difficult-to-handle pieces, the housings are not conformable to the inside of the nose and it is difficult for the housings to seal in different size nostrils thereby facilitating blowby, the passage of air between the tapered housing and the inside of the nose. Wood also teaches that the housings may be reusable possibly leading to contamination, which may be present in the nose including rhinoviruses, adenoviruses, and bacteria. Also, Wood teaches that air filtration media configured in a hollow conical shape may accomplish air filtration but presents no data to indicate that filtering or even breathing through the filter is possible. As determined by laboratory simulation, discussed later, the present invention utilizes a highly efficient depth filter rated at a retention efficiency of 97% for particulate 7 microns and larger at a flow rate of approximately 1 cubic feet per minute and a filter pressure drop of less than one inch of water.
It is therefore desirable to provide for nasal dilation and at the same time utilize a unitary foam depth filter to clean the air drawn into the lungs.
It is further desirable that an internal nasal dilator filter provide a method for dilating the nose and filtering the air inhaled through the nose by providing a reticulated foam filter shaped to be soft and gentle to the interior of the nose while effectively preventing airborne contaminates such as allergens, animal dander, house dust, mites and grass pollens from entering the respiratory system.
As opposed to a filter media with a separate piece inserted in a tapered housing, it is desirable that the filter consists of a single filter material molded into a shape that can be easily and safely inserted into and removed from the interior of the nose and nostrils. A unitary design provides the maximum surface area and volume for maximum airflow and filter efficacy.
Another desirable feature of a new internal nasal dilator filter is that when fully seated within the nostrils its appearance will be aesthetically pleasing.
It is further desirable to provide an internal nasal dilator filter that will remain in place during eating, drinking, talking and heavy exertion but may be expelled in the event of an explosive sneeze.
Additionally it is desirable to provide an internal nasal dilator filter that is easily manufactured, and intended to be disposable thereby minimizing the opportunity to reinsert a unit contaminated with viruses, bacteria and allergens.
It is also desirable to provide a simple, low cost, portable, internal nasal dilator filter that can be economically used by all members of society.
It is also desirable to utilize the natural ability of foam to expand, fill and form to the nostril area thereby sealing the internal nasal dilator filter within the nostrils, eliminating filter blow-by and providing maximum filtering area. Also it is desirable that the foam can easily be compressed both axially and radially, Further, it is desirable to utilize the inherent ability of the resilient member and foam to apply gentle pressure to expand the outer nasal wall tissues from the septum structures thereby providing nasal dilation, increased air flow and subsequent filtering efficacy.
Still further, it is desirable to provide an internal nasal dilator filter of the depth filter type which will capture and hold contaminates by providing a tortuous path for the air flow to follow as it passes through the filter media.
SUMMARY OF THE INVENTION
The present invention provides a combination of internal nasal dilation and nasal filtration operating synchronously. Given this particular combination, the increase in airflow resistance due to the foam filter is offset by the increased airflow caused by the dilation thereby providing an increase in clean air to the lungs.
Air filtration is achieved by retaining particulate in a nasal foam depth filter as air is inhaled through the nose. The filter retention efficiency is 97% for particulate 7 microns and larger at a flow of approximately 1 cubic feet per minute (I CFM) and a filter pressure drop of less than one inch of water (1″ H 2 O).
Internal nasal dilation is provided by the effect of a resilient member adhesively affixed to the nasal foam depth filter and which when bent from a planar surface applies equal outward biasing forces to the inside of the nose so that breathing is facilitated. The soft, gentle foam of the depth filter distributes the biasing force and protects the inside of the nose from irritation. The present invention thus provides an improved internal nasal dilator filter which functions to provide increased air flow through dilation while improving the quality of breathing air by removing particulate during respiration.
The present invention is a combination of internal nasal dilation and internal nasal filtration functioning synergistically to overcome nasal airflow resistance and to provide a greater quantity of filtered air to the lungs by utilizing a highly efficient depth filter to clean the air. The present invention consists of two semi-cylinders of reticulated foam filter media with a spherical shape on the distal (interior nose) end and a flat surface on the proximal end joined to each other at the proximal end with a thin flexible band. The thin flexible band is integrally molded with the semi-cylinders and is made from the same material and at the same time as the semi-cylinders.
Overlaying the thin flexible band and adhesively attached to it and both semi-cylinders is a resilient member in its normal planar orientation. Internal dilation is provided by the effect of the resilient member which when bent from a planar surface applies outward biasing forces to the inside of the nose so that breathing is facilitated. The soft, gentle foam of the filter distributes the biasing forces and protects the inside of the nose from irritation.
The resilient member and adhesively attached foam is intended to be formed into a graceful “U” shape with the resilient member to the inside of the “U.” The distal, spherical shaped end of each semi-cylinder is intended to be inserted in the nostril and located just inside and within the nasal vestibule. The spherical ends guide the internal nasal dilator filter into position and prevent damage to delicate nasal membranes. The proximal end is tucked in within the nasal vestibule just behind where the ala of the nostril narrows. The resilient member and thin flexible band prevent over-insertion of the semi-cylinders and serve as a handle to remove the internal nasal dilator filter from the nose.
The energy expended and applied to the resilient member to form the “U” shape is exactly opposite to the first and second biasing force, or restoring force developed by the resilient member. So that when placed in both nostrils the internal nasal dilator filter constantly exerts an outwardly restoring force (orthogonally against the nasal tissues) of a magnitude sufficient to return the resilient member to an unbent, planar state. Therefore, various embodiments of the present invention provide a desired amount of dilation force as determined by the physical characteristics of the resilient member with differing characteristics leading to differing degrees of dilation.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other features and advantages of the present invention will be better understood by reference to the following detailed description when considered in connection with the accompanying drawings wherein:
FIG. 1 is a bottom, front, left side perspective view of the internal nasal dilator filter of the present invention;
FIG. 2 is a top, plan view of the internal nasal dilator filter of FIG. 1 ;
FIG. 3 is a front elevation view of the internal nasal dilator filter of FIG. 1 , the rear view being a mirror image thereof;
FIG. 4 is a right side elevation view of the internal nasal dilator filter of FIG. 3 , the left side elevation being a mirror image thereof;
FIG. 5 is a front view of the internal nasal dilator filter of the present invention formed into a “U” shape prior to insertion in the nostrils;
FIG. 6 is a front view of the internal nasal dilator filter of the present invention inserted in the nostrils;
FIG. 7 is an elevation, section view of the internal nasal dilator filter of the present invention inserted in the nostrils;
FIG. 8 is a plan and end view of the resilient member of the internal nasal dilator filter of the present invention; and,
FIG. 9 illustrates a laboratory simulator used to measure the retention efficiency of the filter portion of the internal nasal dilator filter of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring to the drawings, FIG. 1 shows the assembly of the internal nasal dilator filter invention. The filter portion incorporates two semi-cylindrical shapes 12 of the same nominal diameter, which have at each distal end a spherical shape 14 to match and blend with the nominal semi-cylindrical diameter and at each other proximal end a base 16 with a flat surface whose plane is perpendicular to the cylinder axis. A thin, strong, flexible band 18 made of the same material as the semi-cylinders joins the semi-cylindrical shapes. The entire filter portion is made from the same material, reticulated foam of the polyurethane or silicone chemical family and of the polyether or polyester category. For the embodiments shown, the semi-cylindrical shapes and connecting flexible band are integrally molded, Referring again to FIG. 1 , extending longitudinally along the thin, strong, flexible band 18 and further extending along a loft line of the circumferential surface of a portion of both of the semi-cylindrical shapes is a plastic, flexible resilient member 20 , which for the embodiment shown is adhesively attached. FIG. 1 shows an embodiment of the present invention in the “relaxed” state. In use, the resilient member is bent into a “U” shape causing the semi-cylindrical shapes to be substantially parallel with the attachment loft lines of the circumferential surfaces to which the resilient member is attached adjacent one another on the legs of the U. The resilient member 20 applies a first and second biasing force, orthogonal to the lateral nostril walls, when bent in the shape of a “U”, as will be shown in greater detail subsequently.
The manufacturing process for the filter portion of the present invention consists of first producing the foam by a chemical reaction process and then removing the cell walls within the foam by a thermal or chemical process thereby producing reticulated foam. The reticulated foam consists of a three dimensional matrix with voids and intricacies within a skeletal structure.
The reticulation process removes the cell walls, leaving only a structure of skeletal strands and voids. This makes the reticulated foam exceptionally porous and permeable but with many particulate catching strands and great contaminate holding capacity within the void spaces.
The reticulated foam manufacturing process is well understood by those skilled in the field and results in a foam with consistent properties including density, tensile strength, tear strength, elongation, compression set and pore size (ppi—pores per inch).
The pores per inch specification relates directly to the efficaciousness of the filter, with a higher number relating directly to greater filtering ability and a greater breathing resistance. Current embodiments of the present invention are molded using reticulated foam of from 40 to 130 ppi so that the user may choose the best filtering characteristic based on individual need.
The reticulated foam is manufactured in large sections approximately six feet by four feet by one foot thick and then supplied to a foam fabricator skilled in the field. For current embodiments, the fabricator slits the foam to the appropriate thickness of about 0.65 inch with a 48 inch by 72 inch sheet, saws the sheet to the handling blocks of about 12 inches and then die-cuts the blocks to produce individual precurser blocks of 1 inch by 2 inches by 0.65 inch which are then further die-cut to shape approximating the semi-cylinders and connecting band suitable as a preform for the molding process. The preform is then placed in a mold and, utilizing heat and pressure, the net shape of the product incorporating the present invention is produced (including a felting step to compress the connecting band). When the product comes from the mold, the molded preform is bent to place a loft line on each of the semi-cylinders in substantially planar relation with the flexible band and the self adhesive resilient member 20 is centered, overlaid and adhered to the thin, flexible band 18 and semi-cylinders producing a product that is ready for use.
Referring to FIGS. 2 and 3 , there is a slight tapering of the semi-cylindrical shape from the proximal end or base 16 to the beginning of the spherical shape 14 providing a frustoconical section. This taper and the rounding at the vertex of the distal end of the spherical shape 14 allows for an easier insertion into the nose by guiding and gently expanding and forming the nostrils during insertion. The foam employed in the embodiments of the invention is easily compressed in an axial and radial direction, whereby insertion discomfort is minimized.
Referring to FIGS. 2 and 3 , the thin flexible band 18 is integrally molded to the proximal end 16 of the semi-cylindrical shapes and coincident with the centerline that joins the centers of the faces at the base 16 of the proximal ends of both semi-cylindrical shapes 12 . The thin flexible band 18 has one surface in the same plane as the flat surface of the base 16 of the semi-cylindrical shapes and the other surface in a parallel plane a small distance away from the proximal end plane.
Referring to FIGS. 1 , 2 , 4 and 6 , the thin flexible band 18 and resilient member 20 are substantially thinner and narrower than the semi-cylindrical shapes thereby allowing great conformability to the exterior of the end of the nasal septum 22 . This conformity allows the base 16 of the proximal end of the semi-cylindrical shapes to be placed within the nasal vestibule just behind the narrowing of the nostril, the ala 24 . The foam of the filter is so soft and gentle that when formed into the “U” shape and inserted in the nostrils, the resilient member sinks into and is cradled by the foam.
The internal nasal dilator filter is gently restrained within the nostrils so that it will not be dislodged by normal activities such as talking and eating and yet still release under the pressures of an explosive sneeze.
Again referring to FIGS. 1 and 2 , the semi-cylindrical shape has a slightly flattened surface 32 on all four sides to better match the ovoid shape of the nostrils. The slightly flattened sides of the cylinders are spaced circumferentially around the frustoconical semi-cylinder and smoothly blended with the spherical shape 14 to assure a gentle yet retained fit within the nostrils.
FIG. 5 shows the internal nasal dilator filter 10 with the resilient member 20 formed from its normal, at rest planar shape, into a smooth “U” shape, as it would be inserted into the nostrils. The “U” shape applies first and second biasing forces at ninety degrees to the long axis of the “U”. This force is applied to both the right and left of the interior nose tissue expanding and dilating the nasal air passageways. The force is cushioned by the projected width of the foam filter so there will be no irritation to the sensitive tissues of the inside of the nose.
Referring to FIG. 6 , the internal nasal dilator filter 10 is shown inserted into the nostrils. When the device is inserted the filter foam is compressed as it passes into the vestibule area and expands to seal the nostril area. Due to the narrow shape of the resilient member with respect to the semi-cylinders, the first and second biasing forces are distributed over the rounded shape of the semi-cylinders. This then distributes the stress over a larger area and reduces the possibility of nose irritation.
Referring to FIG. 7 , when installed in the nose, the internal nasal dilator filter dilates the air passages in the nostrils 24 of the nose 26 to achieve a result similar to adhesive dilators that are affixed to the exterior of the nose. The foam expansion to seal the nostrils presents a larger filter surface area and, as a consequence, lower face velocity across the filter resulting in greater filter efficiency.
Again referring to FIG. 7 , the proximal ends 16 of both semi-cylindrical shapes 12 expand the nostril to conform to the shape of the filter, secure the internal nasal dilator filter to the nostril and assure that all the inhaled air passes through the reticulated air filter. The adaptability, softness and gentle expansion ability of the foam easily conforms to the resilient member and nostril to make a leak proof seal around the nostrils. The gentle expansion ability of the foam makes a nominal size suitable for many people. It is understood that the size of the may be varied in alternative embodiments to accommodate noses of other shapes and sizes.
Referring to FIG. 8 , the resilient member 20 is indicated as a single piece for ease of visualization. In various alternative embodiments, more than one resilient member is employed and the size of the resilient member is varied in area, thickness, length, and shape. For this exemplary embodiment typical dimensions are length 1.75″ by 0.010″ thickness by 0.13″ wide. The material of construction of the resilient member is varied in alternative embodiments but provides that the first and second biasing forces are developed orthogonally when the resilient member is bent into the “U” shape. Some materials found to be acceptable include polycarbonate (PC), polypropylene (PP), polyvinyl chloride (PVC) and acrylonyitrile butyl styrene (ABS).
The adhesive for the present embodiment is of the transfer adhesive type of high tack and strong adhesion to both the resilient member and the polyurethane filter foam.
Although several manufacturers are capable of producing an acceptable adhesive, the following 3M Medical Specialties, St Paul Minn. adhesives have been found to perform well— 1509 , 1512 , 1522 and 1524 . These adhesives are hypoallergenic, conformable and have faceside adhesive strength in the 25 to 53 oz./in. range.
Referring to FIG. 9 the laboratory simulator is used to measure the particle retention ability or efficiency of the filter portion of the internal nasal dilator filter.
The test apparatus consists of an ambient, unfiltered air input and a filtered air input connected to a laser particle counter. The filtered air input is a tee fitting designed to accept both the right and left nostril filters of an internal nasal dilator filter whereas the ambient air input is unfiltered. Both filtered and unfiltered air inputs are connected by tubing to the laser particle counter.
The laser particle counter, model C 1-500 as manufactured by Climet Corporation, Redlands Calif., is of the manifold design so either the filtered or unfiltered input can be automatically selected during the test period. In addition, the laser particle counter measures 12 different particle size ranges at the same time while maintaining a flow rate of one cubic foot per minute (1 CFM).
A test sequence consists of automatically counting the particles in all 12 ranges in the ambient, unfiltered flow and then counting the particles in the same ranges in the filtered flow. The entire counting cycle is automatically repeated 8 times and the average particle count determined for each of the 12 ranges for both the filtered and unfiltered airflows. The retention efficiency is determined from the following formula:
Removal Efficiency (%)=(1−filtered count/unfiltered count)*100
The filter was tested in the laboratory simulator described with respect to FIG. 9 at a one cubic foot per minute (I CFM) air flow. Table 1 presents the removal efficiency percentages at each of 12 ranges for the filter portion of an internal nasal dilator filter.
It is important to specify the flow rate as a test parameter so the particle counts are taken at a normal breathing condition. If the flow rate is too low it could indicate that the pressure drop across the filter is excessive and breathing through the filter would be difficult or impossible.
Normal, at rest, breathing is approximately 12-15 times a minute at a volume of 25-30 cubic inches or 0.25 cubic feet a minute. A flow rate of 1 cubic feet per minute therefore represents a safety factor of 4 to allow for an increase in breathing rate and amount inhaled during moderate work or exercise.
TABLE 1
Particle Size Range (microns)
Removal Efficiency (%)
0.3–0.4
6
0.4–0.55
6
0.55–0.7
6
0.7–1.0
7
1.0–1.3
10
1.3–1.6
19
1.6–2.2
33
2.2–3.0
54
3.0–4.0
71
4.0–5.5
89
5.5–7.0
93
7.0–10.0
97
Having now described the invention in detail as required by the patent statutes, those skilled in the art will recognize modifications and substitutions to the specific embodiments disclosed herein. Such modifications are within the scope and intent of the present invention as defined in the following claims.
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A device combining internal nasal filtration and internal nasal dilation operating synchronously provides air filtration by retaining particulate in a single piece foam nasal filter during inhalation through the nose. Internal nasal dilation is provided by the effect of a resilient member adhesively affixed to the nasal foam filter and which when bent from a planar surface applies outward biasing forces to each nostril so that breathing is facilitated. The soft, gentle foam of the nasal filter distributes the biasing forces over a large area and protects the inside of the nose from irritation. An improved internal nasal dilator filter functions to provide increased air flow through dilation while removing various sizes of particulate through filtration.
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TECHNICAL FIELD
This invention relates to the production of mineral fibers and, more specifically, to producing textile glass fibers, by a rotary process.
BACKGROUND OF THE INVENTION
A common prior art method for forming glass fibers for use in wool products, such as insulation materials, is the use of a rotary process. Glass in its molten state is forced through the orifices in the peripheral wall of a centrifuge or spinner to create streams of molten glass. Thereafter, the streams are further attenuated into glass fibers of smaller diameter by the action of gases discharged downwardly in an annular or cylindrically shaped gaseous flow circumferentially positioned relative to the spinner. Some prior art rotary processes use an annular combustion chamber positioned around the spinner to produce high temperature, high velocity, gases of combustion which are discharged downwardly in a circumferential flow. In other prior art methods, air or steam blowers are utilized either alone or in combination with burners to provide a downward or pulling force.
Krakauer et al. U.S. Pat. No. 3,347,648 discloses the use of a water spray after attenuation and commingling of the filaments to accelerate cooling the filaments whereby resin or binder may be applied sooner. Contrary to the present invention, the rotary process disclosed in Krakauer et al. uses a high velocity, high temperature external burner positioned to discharge a hot high temperature gaseous blast downwardly closely adjacent the spinner to attenuate the glass fibers. The Krakauer et al. water supply pipe applies water to the fibers after they have turned down and fiber commingling has occurred.
Textile fibers are generally longer and stronger than wool fibers produced by prior art rotary processes. For the purposes of this invention, textile fibers are fibers of sufficient length and strength to be used in textile materials, for reinforcing purposes in fiber reinforced plastics and as reinforcing fibers in such products as roofing shingles.
After the longer length textile fibers are manufactured they often are cut into shorter lengths for certain reinforcing applications.
In a prior art rotary process, where rotary glass fibers are manufactured for non-textile applications, the tensile strength of the glass fibers is normally considerably lower than 50,000 p.s.i. (35.1 kg/sq. mm.). Textile fibers should have tensile strengths of 150,000 p.s.i. (105.3 kg/sq. mm.) and preferably 300,000 p.s.i. (210.7 kg/sq. mm.).
Attempts have also been made in the prior art to produce textile fibers by the rotary process. The high fiber production rate of a rotary process is much greater than the fiber production rates of non-rotary processes. One prior art attempt at a rotary process is shown in U.S. Pat. No. 3,900,302. These prior art attempts to form textile glass fibers by the rotary process have not, to the knowledge of the present inventors, been successful. Accordingly, the primary purpose of the present invention is to form satisfactory textile mineral fibers, such as textile glass fibers, by a rotary process.
SUMMARY OF THE INVENTION
The present invention is directed to a method of making glass fibers in a rotary process. The glass fibers are textile fibers for use in textile applications including FRP products and roofing shingle products. The textile glass fibers, according to the present invention, are produced by using a rotary centrifuge having peripheral walls defining a plurality of orifices. The centrifuge spins on its axis of rotation. The steps include discharging and attenuating streams of molten glass fibers from the rotary centrifuge along paths generally perpendicular to the axis of rotation of the centrifuge. The glass fibers are turned downwardly normally by the use of a cylindrically shaped gaseous stream. Prior to such turning and/or the general commingling of the glass fibers, the fibers are quenched by the application of a liquid.
In a preferred method, sizing is applied to the glass fibers either during or subsequent to the quenching step.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic elevational view partially in cross-section, showing the rotary centrifuge discharging streams of glass fibers and the quenching of the fibers by the application of a liquid, according to the present invention;
FIG. 2 is a schematic view in elevation of one embodiment of apparatus for making rotary textile glass fibers, according to the present invention; and
FIG. 3 is a view similar to FIG. 2 showing another embodiment of apparatus for making rotary textile glass fibers, using an external annular burner, according to the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
As shown in FIG. 2, a spinner or centrifuge 10 is mounted for rotation on a quill 11. The spinner 10 includes a bottom wall 12 and a peripheral wall 13 integrally connected to a ring-shaped top wall 14.
The peripheral wall 13 defines a plurality of orifices 16. A molten stream of glass 17 enters the spinner 10 and is forced outwardly against the peripheral wall 13 by centrifugal force. The molten glass passes through the orifices 16 to form fibers 18. The glass passing through the orifices 16 is maintained in a plastic, attenuable condition by heat supplied by a plurality of internal burners 38. Positioned exteriorly of the spinner 10 and located circumferentially around the peripheral wall of the spinner 10 is a high pressure annular blower 23 for providing additional attenuation forces on the fibers by forcing high velocity, high pressure, air downwardly. A quenching ring 26 surrounds the spinner and is preferably concentrically located with respect to the blower 23. The quenching ring 26 through its nozzles 27 discharges a stream of quenching liquid downwardly to engage the fibers 18 prior to a time that they have commingled and are turned by the forces generated by the annular blower 23. Referring to FIG. 1, an immaginery cylinder 34 defined by the center of the spray path emitted from the circumferentially mounted nozzles 27 is positioned an incremental distance "d" from an immaginery cylinder of rotation 32 which is the point or plurality of points where the attenuating fibers begin their downward movement.
Referring to FIG. 1, the immaginery cylinder of rotation 32 has a radius R T . The spinner 10 has a radius R S , while the quench ring 26 has a radius R N . The annular blower 23 has an exit which defines a radius R B with the axis of rotation 30 of the spinner 10.
In a preferred spacing, if R S =7.5 inches (19 c.m.) R N is between 7.75 inches (19.7 c.m.) and 8.5 inches (21.6 c.m.), while R B is 8.75 inches (22.2 c.m.); and the difference between R B and R N is 0.25 inches (0.64 c.m.) to 1.0 inch (2.54 c.m.).
The quenching liquid applied by the quenching ring 26 is localized between the wall 13 of the spinner 10 and the blower 23 such that the liquid does not strike the spinner wall 13 but is applied prior to the commingling and/or the turndown of the fibers 18 at R T . The quenching liquid is applied exterior of the centrifuge and at a position to temper the fibers into high strength textile fibers. Preferably the radius R T is close in dimension to the radius R B and in practice it has been found to be preferable to have R T approximately 0.0625 of an inch (0.16 c.m.) smaller than R B .
The immaginery cylinder of rotation 32 indicates generally where the attenuating fibers 18 begin their downward movement.
A sizing can be applied to the fibers 18 with quenching liquid or at a position below the spinner 10.
A typical size which may be utilized comprises a film former, a dispersing agent, a lubricant and a silane. More specifically the following compositions may be used:
______________________________________Film Former Viny1 205 manufactured by Air ProductsDispersing Agent Fatty Acid Amine Reaction ProductLubricant Emery 7440 (a mineral Oil Dispersion) manufactured by EmerySilane A-1100 (Ammino Silane) manufactured by Union Carbide.______________________________________
While the above size compositions may be utilized, it is understood that the textile rotary process described herein is not limited to the specific size disclosed above.
A quenching liquid must be used as opposed to a quenching fluid gas. The quenching liquid which essentially is water or water with an additive, such as the sizing, has sufficient BTU's of cooling to sufficiently quench the fibers prior to the drag forces of the blower 23 pulling and commingling the fibers as they attenuate.
While it is not completely understood why the quenching liquid application allows the production of textile quality fibers by a rotary process, it is felt that the quench provides a rapid cooling of the fibers at a desired location before turndown and/or commingling. By using such a process, the inventors have been able to produce textile glass fibers by a rotary process of sufficient lengths and strengths for commercial or industrial uses.
As the term "commingling" is used in the present specification and claims, it means the location in the fiber path where a large number of fibers engage or commingle with one another. This location is normally immediately before or at the turn down of the fibers where they turn from a path perpendicular to the axis of rotation of the spinner to a path generally parallel to the axis of rotation. The term "commingling" as used in the present specification and claims does not include the touching of small numbers of random fibers which occurs throughout the process beginning immediately after the fibers are formed at the peripheral wall of the spinner.
In the present embodiments, quenching liquid is applied to the glass fibers in the range of 0.2 to 1.2 lbs. of water (0.09 kg. to 0.54 kg. of water) to 1 lb. of glass (0.45 kg. of glass). A preferable range of quenching liquid is 0.6 to 0.7 lbs. of water (0.27 kg. to 0.32 kg. of water) to 1 lb. of glass (0.45 kg. of glass).
Referring to FIG. 1, which is a diagrammatic view, the spinner 10 includes an axis 30 which is the center of rotation of the spinner. While the peripheral wall 13 is shown as generally parallel to the axis 30 it is understood that the peripheral wall 13 may be angled and still fall within the scope of the present invention. The cylinder of rotation 32 has the axis 30 as its axis and indicates the point where the attenuating fibers 18 generally begin their downward motion. The nozzles 27 are positioned in a ring and define the immaginery cylindrical surface 34 which is the center of the cylinder of quenching liquid supplied through the quenching ring 26. The quenching liquid cylinder 34 is concentric with and spaced inwardly from the cylinder of rotation 32 by a predetermined or incremental distance "d" as shown in FIG. 1. It has been found that it is most important that the quenching liquid be applied to the primary fibers 18 prior to the time that they reach the cylinder of rotation 32 and prior to turndown.
Referring to FIG. 3, another embodiment of apparatus for fiberizing molten mineral material is shown. A spinner 10' is mounted for rotation on a quill 11'. The spinner 10' includes a bottom wall 12', a peripheral wall 13' and a top wall 14'. A plurality of orifices 16' are defined by the peripheral wall 13'.
A molten glass stream 17' enters the spinner 10' and is forced outwardly against the peripheral wall 13' by centrifugal force. The molten glass passes through the orifices 16' to form glass fibers 18'.
An annular burner 20 maintains the glass fibers 18' in a plastic attenuable condition. The annular burner 20 is an exterior burner and in the present embodiment is mounted above and slightly outside of the peripheral wall 13' of the spinner 10'. As shown, the burner 20 has a rather open throat and the gases passing from the burner have a low velocity. The velocity of the gases from the burner 20 is insufficient to actually attenuate the glass fibers 18' issuing from the spinner 10'. This is in contrast to other prior art burners which use high velocity gases for the purpose of attenuating the fibers. The glass fibers 18' are further attenuated by the action of high velocity gases discharged from an annular blower 23'.
While temperature conditions vary, the temperature of the molten glass within the spinners 10 and 10' would approximate 1900° F. (1038° C.). Generally the temperature of the molten glass within the spinner 10' will fall within a range of 1500° F. and 2400° F. (816° C. and 1316° C.).
In the embodiment shown in FIG. 3, the annular burner 20 is a low velocity burner which maintains the heat in the attenuating glass fibers while the drag or attenuating forces are created by the annular blower 23. Under this process, a quenching ring 26' having a plurality of downwardly positioned nozzles 27' applies a quenching liquid, indicated by dashed lines in FIG. 3, to the fibers after they leave the spinner 10' and prior to the time that they commingle or are turned downwardly by the attenuating blower 23'. At the point that the quenching liquid is applied, as shown in FIG. 3, the attenuation has occurred because of the centrifugal forces generated by the spinner 10' and because of the downward pull created by the blower 23; and the attenuation is not, for example, the result of a high velocity external burner (not shown) which would commingly the fibers and prevent the desired affect of the quenching liquid.
Many changes may be made to the above described apparatus and methods without departing from the following claims.
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A method of making textile glass fibers in a rotary process is disclosed. A spinner bearing molten glass rotates on its axis of rotation. Glass is forced through orifices and the resulting fibers are moved along paths generally perpendicular to the axis of rotation. Prior to commingling or turn down of the fibers a quenching liquid is applied to the fibers.
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BACKGROUND OF THE INVENTION
1. Field of the invention
This invention relates to a thermal copying apparatus which makes an original and a plain sheet to be in intimate contact with each other and carries out thermosensitive copying operation by irradiating a light from an exposure source.
2. Description of the prior art
The thermal copying apparatus irradiates an original pressed onto a recording sheet by a light from an exposure source to generate a temperature pattern corresponding to an original image. Due to the temperature pattern, the original image is copied on the recording sheet.
One known example is structured such that a light source is disposed within a transparent tubular member and an original and a recording sheet are fed between the transparent tubular member and a pressure roller which is pressed onto the tubular member.
Another known example is structured such that an original and a recording sheet are pressurized between a flat glass plate and a platen each time they are conveyed by a predetermined distance, and the original is light-radiated through the glass plate.
Those structured as above, however, are disadvantageous in that if foreign matters such as dust in air are entered between the transparent member and the pressure roller or between the glass plate and the platen, then the quality of copying will be outstandingly degraded. Also, the apparatus with the mechanism for intermittently pressurizing the original and the recording sheet will become unavoidably complicated in structure. Further, in multicolor copying operation, the problem of color position deviation would arise from the reciprocal movement of the recording sheet required.
In addition, a temperature bias is caused at the original and the recording sheet due to the temperature of the transparent member, resulting in a change of copying density.
Further in addition, the transparent member will be cooled by the original or recording sheet which are fed, so that the temperature distribution on the surface thereof will be made not-uniform, which will cause an unevenness in copying density.
Still further, the temperature of the transparent member will be increased during copying operation and particularly when it is increased in excess the image copied will become fogged. Thus, the transparent member is required to be cooled. But if it is not uniformly cooled, an evenness in copying density will be caused.
SUMMARY OF THE INVENTION
An object of this invention is to provide a thermal copying apparatus capable of producing a uniform density of copy image.
Another object of this invention is to provide a thermal copying apparatus having the copying energy reduced.
A further object of this invention is to have the above mentioned apparatus realized by a simple structure.
A thermal copying apparatus in accordance with this invention comprises a holding member and a transparent member for holding therebetween an original and a recording sheet so that the original and the recording sheet are in intimate contact with each other, a heating means for heating the transparent member, a light source for producing a light for irradiating the original through the transparent member to perform an copying operation thermosensitively, and a conveying means for conveying the original and the recording sheet.
The light source produces the light to perform the copying operation each time when the original and the recording sheet are conveyed by a predetermined distance. The transparent member is heated by the heating means so that a reduction of copying density due to a fall of temperature of the transparent member at the side at which the original and the recording sheet are fed can be compensated.
Furthermore, the thermal copying apparatus in accordance with this invention is preferably equipped with a cooling means for cooling the transparent member. The cooling means generates cooling gas flowing in a direction perpendicular to the conveyed direction of the original and recording sheet, and periodically reverses the following direction of the gas so that the transparent member is cooled uniformly. In addition, the temperature of the transparent member would become a bias for the original and the recording sheet and if the copying operation is carried out using an energy at a same level, then the copying density would change depending on the temperature of the transparent member. To avoid this, the apparatus in accordance with this invention preferably has means which detects temperature of the transparent member and controls the flash energy of the light source.
By using the above mentioned structural elements independently or in combination, the cooling action of the transparent member due to the original or the recording sheet can be compensated. Also, the copying density can be made uniform by cooling the transparent member and/or controlling the flash energy of the light source in accordance with a change in temperature of the transparent member.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view showing a preferred embodiment of thermal copying apparatus in accordance with this invention.
FIG. 2 is a sectional view showing a structure of a mask sheet.
FIG. 3 is a sectional view showing a structure of a exposure section of the preferred embodiment shown in FIG. 1.
FIG. 4 is a front view and a plan view of a transparent heating element of the preferred embodiment shown in FIG. 1.
FIG. 5 shows a temperature characteristic of a surface of a glass plate cooled by the mask sheet.
FIG. 6 is a block diagram showing a control circuit of the preferred embodiment shown in FIG. 1.
FIG. 7 is a front view showing another example of transparent heating element.
FIG. 8 shows a charging circuit and a flash trigger circuit in the control circuit shown in FIG. 6.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Hereinafter, the embodiment of this invention will be described by referring to the drawings. In FIG. 1, a mask sheet 4 is supplied from a supplying reel 40 to be wound up on a winding reel 41 which is driven by a sheet motor 17. A recording sheet 5 is supplied, in the same manner as the mask sheet, via a supplying roller (not shown) from a supplying cassette (not shown) to be held by a pawl 1a of a drum 1. After completion of copying, the recording sheet is released from the drum via a releasing roller (not shown) because a peeling roller 9e peels off the mask sheet 4 and the pawl 1a is disengaged. The mask sheet 4 and the recording sheet 5 are supported by the drum 1 and intimately contacted each other by being pressed onto the drum 1 at a predetermined strength of force by a glass plate 2 having a predetermined curvature.
A rotary encoder 15 is disposed coaxially with the drum 1 for detecting a rotational angle of the drum. A xenon flash lamp 3 which serves to act as an exposure light source is disposed confrontedly adjacent to the glass plate 2 and a reflector 11 is disposed around the lamp 3.
The mask sheet 4, as shown in FIG. 2, comprises an aluminum layer 4b deposited on one surface of a transparent sheet 4a and a thermomelting ink 4c coated on the other surface of the transparent sheet 4a. A discharge recording head 8 has a plurality of recording needles (not shown) at the top end thereof. Signal voltages are applied to the needles through a recording head driver (shown later) in accordance with a pattern to be copied thereby removing the aluminum layer 4b of the mask sheet 4 to correspond to the pattern. The recording sheet 5 is placed on the mask sheet 4 on the surface on which the thermomelting ink 4c is coated.
A capstan 6 is driven by a capstan motor 16 to convey the mask sheet 4 cooperatively with a pinch roller 7. Roller 9a through 9e form a conveying route of the mask sheet 4, and particularly the roller 9b serves also as a return electrode for the discharge recording.
A cooling fan 10, which is driven by a fan motor 10a, is to cool the xenon flash lamp 3 and the glass plate 2.
The glass plate 2 and the reflector 11 define a wind path 12 for flowing the cooling air in the direction perpendicular to the direction that the recording sheet 5 and the mask sheet 4 are conveyed.
Referring to FIG. 3, transparent heating elements 31a and 31b of indium oxide (In 2 O 3 ) for heating the glass plate 2 and temperature sensors 32a and 32b for detecting the temperature of the glass plate 2 are disposed on the lower surface of the glass plate 2. The transparent heating elements 31a and 31b are, as shown in FIG. 4, separately deposited on the lower surface of the glass plate 2 and connected to a heating control circuit (shown later) thereby to be controllable independently.
In FIG. 6, a block 61 is a microprocessor unit (MPU), a block 62 is a random-access memory (RAM), and a block 63 is a ready-only memory (ROM) The MPU 61 sends commands in accordance with a program stored in the ROM 63 based on data from the rotary encoder 15 and the temperature sensors 32a and 32b to the head driver 64, capstan motor driver 66, sheet motor driver 67, fan motor driver 68, charging circuit 70, flash trigger circuit 72 and heat control circuit 73.
The operation of the thermal copying apparatus structured as above will be shown below.
The mask sheet 4 is recorded with an image pattern by the discharge recording head 8, and the recording sheet 5 is conveyed to the pawl 1a of the drum 1 via the supplying roller to be held on the drum. When the Capstan motor 16 and the sheet motor 17 are driven, the mask sheet 4 is conveyed from the supplying reel 40 to the winding-up reel 41 while successively passing through the rollers 9a through 9e. The rotatable drum 1 rotates in synchronism with the conveyance of the mask sheet 4 while holding the recording sheet 5, so that the mask sheet 4 and the recording sheet 5 are successively intimately contacted each other at the predetermined strength of force between the drum 1 and the glass plate 2. If the xenon flash lamp 3 emits a light under such condition as above, the light transmits where the aluminum layer 4b has been removed but is reflected at where the layer 4b remains so that the thermomelting ink 4c accumulates heat and melts by receiving the light corresponding to the image pattern thereby to copy the image pattern on the recording sheet 5.
The recording sheet 5 is conveyed with the mask sheet 4 because the latter is conveyed continuously. The glass plate 2 is held in a fixed position and the mask sheet 4 is conveyed while sliding on the surface of the glass plate 2. The xenon flash lamp 3 flashes each time when the mask sheet 4 and the recording sheet 5 are conveyed by a predetermined distance. The flash is caused by a high voltage pulse which is generated by closing a trigger switch 721 of the flash trigger circuit 72 in response to a command from the MPU 61 under a condition that a capacitor 701 is charged. Timings to operate the discharge recording head 8 and the xenon flash lamp 3 are determined by the MPU 61 by counting pulses from the rotary encoder 15.
If the copying operation is carried out as above, temperature of the glass plate 2 will become higher than ambient temperature due to the flash of the xenon flash lamp 3. However, as shown in FIG. 5, since the glass plate 2 is cooled by the mask sheet 4 which is lower in temperature, the portion where the mask sheet 4 is fed into (indicated at A) becomes lower in temperature by T a than that of the portion where it is fed out (indicated at B). The mask sheet thus fed is warmed up to the temperature of the glass plate 2 during conveying, so that temperature differences will be produced where the copying is to be made. The temperature differences at the mask sheet will cause differences in heat quantities for heating the thermomelting ink 4c to its melting point, so that the copying operation using an energy at a same level causes the copying density to be varied.
In this embodiment, in order to reduce the copying energy at the beginning of the copying operation, the glass plate 2 is heated during a waiting state of the apparatus by applying an electric current to the transparent heat elements 31a and 31b. In this case, the transparent heat element 31a generates a larger amount of heat than the element 31b so that the portion indicated at A is held at a temperature higher by T b (Tb≈Ta)than that of the portion indicated at B of the glass plate 2. When the copying operation is started, a larger electric current is applied to the transparent heat element 31a than during waiting. If the temperature of the glass plate 2 is being uniformalized during waiting, the A-portion of the plate 2 will be cooled by the mask sheet 4 immediately after the beginning of the copying operation and a time until the temperature of that portion of the glass plate 2 elevates after the application of larger electric current to the element 31a will be delayed. However, this can be solved by making the A-portion of the glass plates 2 higher in temperature by T b than the B-portion during waiting as described above.
Temperatures of the glass plate 2 are detected by the temperature sensors 32a and 32b. According to the detected temperatures, the electric currents applied to the transparent heat elements 31a and 31b are controlled by the heat control circuit 73. Currents to be applied to the transparent heat elements 31a and 31b in accordance with the temperatures detected by the temperature sensors 32a and 31b are determined by data stored in the ROM 63.
As described above, the preheating of the glass plate 2 makes it possible to apply a temperature bias to the mask sheet 4 thereby to reduce the copying energy just after the beginning of copying operation as well as to compensate the cooling action of the glass plate 2 due to the mask sheet 4 or the recording sheet 5. Further, it is possible to make the power unit and apparatus small-sized as well as to render the copying density remarkably uniform.
In the embodiment shown above, the transparent heat element is divided into two parts, 31a and 31b, and a current applied to each of them is controlled to produce a temperature gradient between two portions, A and B, of the glass plate 2.
But is also possible to provide a transparent heat element having slits which are different in interval between the two portions, A and B, as shown in FIG. 7 to vary a current density for applying thereto thereby to produce a temperature gradient therebetween. Also, if an energy necessary to do copying immediately after the beginning of the operation is well supplied, there is no need to apply an electric current to the transparent heat element 31b during waiting.
If the temperature of the glass plate 2 is elevated up to near the melting point of the thermomelting ink 4c due to the flash of the xenon flash lamp 3, the ink coated in areas other than the image pattern recorded on the aluminum layer 4b would be copied on the recording sheet 5. This leads to an outstanding deterioration in copying quality. Thus, the necessity of cooling the glass plate 2 is arised. In this embodiment, the glass plate 2 and the reflector 11 are disposed so as to provide a kind of duct so that a cooling air can be supplied to effectively cool the glass plate 2 during passing through the duct. In this case, however, the supply of the cooling air only in one direction may cause the cooling action not to be uniform, because the area near the inlet of the air is more effectively cooled than the area near the outlet thereof. As the result, the copying density will become lower at the inlet area than at the outlet area. With different temperatures of the mask sheet 4, the amount of heat necessary to heat the thermomelting ink 4c to its melting point varies, so that the copying operation at the same level of energy results in not-uniform copying density.
Thus, this embodiment is structured such that the cooling fan 10 is reversed in rotating direction by the fan motor driver 68 at predetermined cycles to periodically reverse the flowing direction of the cooling air . The reversing interval depends on the heat capacity of the glass plate 2 and is preferably set within a range from 6 to 12 seconds. With this structure, the glass plate 2 can be cooled uniformly from its both sides to obtain uniform temperature distribution and copying density.
Instead of the use of one cooling fan to be periodically reversed, two cooling fans may be disposed at both sides of the wind path(duct) and operated alternately at predetermined intervals to supply the cooling air alternately in opposite directions.
The charging circuit 70, as shown in FIG. 8, boosts and rectifies an alternate current from an AC power source 80 to charge the capacitor 701. The charging operation completes when data from a D/A converter 701 indicates that the capacitor 701 has been charged up to a charging voltage which is determined from temperature data detected by at least one of the temperature sensors 32a and 32b. The control of the charging voltage is carried out by switching a solid state relay (SSR)703 in response to a signal from the MPU 61. The xenon flash lamp 3 flashes in response to a trigger signal from the flash trigger circuit 72 after the capacitor 701 has been charged up to a predetermined voltage. By controlling the flash energy as described above, the copying operation is always carried out under the optimum energy condition to obtain a uniform copying density.
In this embodiment, the mask sheet 4 is structured as shown in FIG. 2, but it may also be possible to use an ordinary paper as the mask sheet and a thermosensitive paper as the recording sheet. In addition, the mask sheet 4 and the recording sheet 5 are intimately contacted each other between the drum 1 and the glass plate 2, but if they are structured such as to be conveyable in intimately contacting each other, a flat holding member and a flat transparent member may be used. Further in addition, any transparent material other than glass can be used in lieu of the glass plate 2. Still further in addition, temperature sensors are disposed one on each of A- and B-portions of the glass plate 2, but only one element may be disposed at a position where the typical temperature of the glass plate can be detected.
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A thermal copying apparatus disclosed holds an original and a recording sheet in intimate contact with each other between a holding member and a transparent member and operates a light source to irradiate the original through the transparent member thereby to effect a copying operation thermosensitively. The apparatus further has at least one of a heater for heating the transparent member at a portion where the original and the recording sheet are fed into prior to the copying operation, a cooling fan for generating a cooling gas flowing perpendicularly to the conveying direction of the original and the recording sheet and reversing its flowing direction at predetermined cycles, a sensor for detecting temperature of the transparent member, and a circuit for controlling energy of the light source in accordance with the detected temperature, thus being capable of always obtaining uniform copying density.
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CROSS-REFERENCE TO RELATED APPLICATIONS
Not applicable.
STATEMENT REGARDING THE FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not applicable.
REFERENCE TO A MICROFICHE APPENDIX
Not applicable.
BACKGROUND OF THE INVENTION
Combustion engines which compress the combustion air have an ambient temperature sensitivity—both the capacity and the efficiency decrease as the ambient temperature increases. The power demand of the compressor section of the engine is approximately proportional to the absolute temperature of the inlet air, which makes the efficiency of the engine proportional to the inverse of the absolute temperature. The compressor capacity, and hence overall engine capacity, is proportional to the density of the inlet air.
The net result is that for a compressed air combustion engine, both the power output and engine efficiency are de-rated at warm ambients. The degradation is not so severe with reciprocating engines, which require little more than stoichiometric air. The degradation is very severe with combustion turbines, which require on the order of 3 or 4 times stoichiometric air.
One known method of counteracting the warm ambient degradation of compressed air combustion engines is by cooling the inlet air, either evaporatively or with a refrigerant. The refrigerated cooling can be done either in refrigerated air coils or by direct contact with sprayed chilled water. The refrigeration is supplied by either mechanical or absorption refrigeration systems, and in some instances through a cold storage medium (ice or chilled water).
Another approach to cooling combustion engine inlet air is by over-spraying, typically via fogging. Sufficient water is injected into the air in fine droplet form such that it not only reduces the temperature adiabatically to the dew point, but additional droplets remain un-evaporated, and carry into the engine compressor. Those droplets rapidly evaporate as compression proceeds, slowing the temperature increase caused by compression, and hence effectively adding to the amount of inlet cooling. For the droplets to remain suspended in the air into the compressor rather than separate out excessively, they should be in the fog-size range, i.e., less than 40 microns in diameter and preferably 5 to 20 microns. Another advantage of this size range is that the droplets are small enough that they do not erode the compressor blades.
The problems with the current approaches to cooling engine compressor inlet air include the following. Most compressors would benefit thermodynamically from sub-freezing inlet temperatures, or at least could be designed to benefit from those temperatures. However, there are many practical difficulties. Especially with high rotational speed combustion turbines, there is a possibility of ice buildup on inlet guide vanes, which then could spall off and damage the compressor blades. This imposes a practical limiting temperature of about 4° C. for many inlet cooling systems. Cooling below that temperature will require some additional technique of reducing the humidity level of the cold air below saturation—reheat, etc. On the refrigeration side, special measures are also required to deal with the H 2 O removal from the air in sub-freezing conditions: periodic defrosting of the air coils, or continuous addition of a melting agent. Furthermore, the refrigeration system requires proportionately more input power to reach the lower temperatures—more shaft power for mechanical refrigeration, or higher quality heat for absorption refrigeration. With mechanical refrigeration, the power necessary to reach sub-freezing temperatures is so large, and the marginal improvement in the engine due to colder compression is so small, that there is little or no net gain from cooling to sub-freezing temperatures.
Even when the inlet cooling is restricted to above-freezing temperatures, other major problems remain. The compressor benefit is substantially due to the sensible cooling of the inlet air, with almost no added benefit from the latent cooling, i.e., the amount of moisture condensed out of the air. However, the latent cooling typically represents 25 to 50% of the total refrigeration load. For example, consider 35° C. air at 50% relative humidity, which is cooled to 5° C. at 100% relative humidity. The moisture content decreases from 1.8 weight percent to 0.55 weight percent. For these conditions, only 51% of the total refrigeration provides sensible cooling, and 49% causes the water condensation. Thus, much of the refrigeration is effectively wasted.
Another problem is that the water removal results in reduced mass flow through the turbine, proportionately reducing its power output. Air flow can be correspondingly increased, but that adds compression power.
The overspray or fogging approach to inlet cooling also presents problems. The two foremost are that the cooling is adiabatic, as opposed to the diabatic cooling of the refrigeration approach; and that a source of pure water is required for every bit of cooling accomplished. The adiabatic limitation causes the inlet sensible temperature to be no lower than the dew point. The cost and availability of pure water mitigate against this approach at many sites.
It is known that injection of some water, as either vapor or liquid, into the compressed air of a combustion turbine increases the capacity and decreases the emissions and heat rate. However, a costly supply of pure water is required.
What is needed, and included among the objects of this invention, are apparatus and process which overcome the prior art problems cited above, i.e., an inlet cooling system wherein the latent load contributes to power augmentation and heat rate improvement in addition to the sensible load contribution; where the benefits of the water injection are available without the limitations of needing a large source of pure water and that the inlet temperature is limited to the dew point; where the thermodynamic benefits of sub-freezing inlet temperatures are achievable without the practical problems; and wherein the refrigeration system is activated by low temperature waste heat so as not to detract from the compressor shaft power reduction (system power gain) provided by the inlet cooling system.
The Nagib '71 article shows that recuperated combustion turbines derive the maximum benefit from inlet cooling. Recuperation causes lower exhaust temperatures, and inlet cooling causes a further reduction in exhaust temperature. Similarly, cogeneration and combined cycle configurations have very low exhaust temperatures. Prior art waste heat-activated absorption inlet cooling cycles require exhaust temperatures of about 200° C. or higher. For the more aggressive spray cooling disclosed here, such temperatures will not usually be available. Thus, one important aspect of this disclosure is the identification of an absorption cycle which can be powered by waste heat well below 200° C.
In order to condense moisture out of the exhaust, it must be cooled to well below 80° C. It would be advantageous if the absorption cycle heat input caused that low a temperature, to minimize any need for additional ambient cooling of the exhaust.
BRIEF SUMMARY OF THE INVENTION
This disclosure recites a compressed air combustion engine with inlet cooling supplied by an absorption unit powered by the combustion exhaust. Moisture is condensed from the inlet air and/or from the exhaust, and is sprayed into the compressed air and/or fogged into the chilled inlet air. The special flow sequence desirable in a two-pressure absorption cycle in this service is disclosed, as well as the three-pressure absorption cycle which provides maximum thermodynamic benefit.
In particular, an apparatus for energy conversion is disclosed comprised of:
a) a combustion engine comprised of a compressor, a combustor, and a work expander;
b) an engine inlet air chiller;
c) an absorption refrigeration unit which supplies chilling medium to said chiller;
d) an exhaust heat exchanger which transfers heat to said ARU from said engine exhaust;
e) a means for collecting condensate from at least one of said chiller and said exhaust heat exchanger; and
f) a means of injecting at least part of said collected condensate into said compressor discharge vapor.
In another embodiment, the energy conversion apparatus is comprised of:
a) a combustion engine with a combustion air compressor;
b) an absorption refrigeration unit (ARU) which is powered by engine exhaust;
c) a sequential path for absorbing solution in said ARU comprised of the following components in sequence:
i) a solution pump;
ii) a solution cooled vapor rectifier (SCVR);
iii) a solution heat exchanger (SHX);
iv) an exhaust heated once-through co-current vapor generator; and
v) a vapor liquid separator which sends vapor to said SCVR and liquid to said SHX.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
FIG. 1 illustrates one combination of essential features of this invention, wherein spray injecting moisture is collected by chilling the inlet air with the exhaust heat-powered absorption refrigeration unit (ARU) refrigeration.
FIG. 2 is a second embodiment, wherein the inlet air is humidified before chilling, so as to increase the yield of de-mineralized moisture collected; and spray injection moisture is also collected from the exhaust.
FIG. 3 discloses that the moisture collected from the inlet air can be routed to either or both of two locations as the need arises: into the chilled inlet air as fog; or into the compressed air. It also discloses details of the two-pressure ARU configuration which allows use of low temperature exhaust heat.
FIG. 4 illustrates a recuperated combustion engine adapted for spray injection moisture collection at two locations, and also a three-pressure ARU which permits exceptionally low exhaust temperatures to be used.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1, a combustion engine which converts fuel energy to mechanical energy is comprised of compressor 10 , combustor 11 , fuel supply 12 , and work expander 13 (e.g., a turbine). Inlet air to the compressor is chilled in chiller 14 , which is supplied chilling medium (e.g., refrigerant) from absorption refrigeration unit (ARU) 15 , which is heated by exhaust gas from expander 13 . Moisture condensed from the air is collected and pressurized by pump 16 , then spray injected into the compressed air from compressor 10 , prior to undergoing combustion in combustor 11 .
FIG. 2 illustrates several desirable added features beyond those disclosed in FIG. 1 . Components 20 - 26 have similar descriptions as corresponding 10 - 16 of FIG. 1 . Humidifier 27 (e.g., an evaporative cooler) adiabatically humidifies the inlet air before it is chilled—this increases the moisture loading, and hence the amount of de-mineralized water which can be collected for re-injection. Recuperator 28 increases the energy efficiency of the overall cycle. Pump 29 pressurizes the moisture condensed from the exhaust for injection into the compressed air.
FIG. 3 provides preferred elaboration of FIG. 1, with additional features. Inlet air to combustion engine compressor 30 is chilled in inlet chiller 34 . Condensed moisture is collected in receiver 310 and pressurized by pump 36 . It can then be routed through valve 311 to fogging apparatus 312 , and/or through valve 313 to spray apparatus 314 located in the discharge line from compressor 30 . After being combusted with fuel 32 in combustor 31 , the hot combustion gas is work expanded in expander 33 , and the hot exhaust is routed through heat recovery vapor generator 315 , which contains at a minimum a once-through co-current mass exchange high-pressure solution vapor generator 316 . “Once through” signifies that the fluid makes a single pass through this component 316 each time it enters, as illustrated. Conventional heat recovery steam generators are of the recirculating type, with a steam drum, wherein the liquid passes multiple times through the boiling coils each time it enters the generator.
The waste heat-powered two-pressure ARU depicted in FIG. 3 is comprised of high-pressure generator 316 which supplies two-phase solution to high-pressure separator/rectifier 317 . The separated vapor is rectified adiabatically, and also diabatically at solution-cooled rectifier 318 , and then condensed in condenser 319 . The liquid condensate is sub-cooled in refrigerant heat exchanger 320 , and then reduced in pressure at expansion valve 321 , and supplied to chiller coils 34 , where it evaporates. The cold vapor is warmed in refrigeration heat exchanger 320 , then absorbed in the low-pressure absorber 322 . The liquid separated in separator 317 is cooled in solution heat exchanger 323 , reduced in pressure by means for pressure reduction 324 , and then absorbs the vapor in low-pressure absorber 322 . Solution pump 325 pressurizes the low-pressure absorbent solution back to high pressure, which is then routed through solution-cooled rectifier 318 , solution heat exchanger 323 , and once-through high-pressure generator 316 , thence to separator 317 to complete the cycle. The rectification in rectifier 317 proceeds more efficiently, and hence the entire ARU, when a minor fraction of the solution is refluxed directly into the rectifier through bypass 326 .
Injecting a given amount of moisture as fog in the chilled inlet air provides a greater increase in power, whereas spraying the same amount into the compressed air provides a greater increase in efficiency (decrease in heat rate—for recuperated cycle). Hence, this flowsheet allows either or both to be done, as needs dictate. In any event, the fogging and/or spraying should be varied slowly so as to not thermally shock or otherwise damage the apparatus from differential thermal expansion.
The maximum safe moisture loading possible with fogging is much lower than that possible by spraying into the compressed air. Typically about 1% by weight of the inlet air or less is obtainable by condensation from the inlet air, and that is approximately the amount which can safely be fogged into saturated air. On the other hand, much larger amounts can be sprayed into the compressed air, e.g., up to 7 or 8%. The collected moisture can be supplemented by a separate source of de-mineralized water. A preferred approach when water is scarce or costly is to extract significant moisture from the exhaust gas. That is what is illustrated in FIG. 4 .
In FIG. 4, the components 40 - 426 have descriptions similar to the correspondingly numbered components in FIGS. 2 and 3. In order to cool the exhaust sufficiently to condense out moisture to be collected at receiver 428 , a lower temperature coil 427 is provided which is a once-through intermediate pressure solution vapor generator (IP generator). Some additional ambient cooling may also be necessary at coil 429 . Also, a damper-controlled bypass 430 will assist in maximizing the cooling of the non-bypassed exhaust into the condensation range.
Solution from low-pressure solution pump is split by splitter 431 , with part routed through IP generator 427 into IP vapor-liquid separator 432 , and the remainder to IP absorber 433 , where it absorbs the vapor from IP separator 432 . The resulting absorbent solution is pressurized to high pressure by high-pressure (HP) solution pump 434 , and routed to solution-cooled rectifier 418 . The liquid from separator 432 is let down in pressure at expansion valve 435 , and routed to LP absorber 422 .
The third (intermediate) pressure level allows generator 427 to operate at a lower temperature level. This has two beneficial effects. The amount of heat necessary at HP generator 416 is decreased, and hence it can use a lower temperature inlet exhaust heat, on the order of 150° C. Secondly, IP generator 427 cools the exhaust to lower temperatures, e.g., on the order of 75° C., already below the dewpoint. This facilitates moisture condensation.
Any known type of ARU may be used, e.g., LiBr—H 2 O or NH 3 —H 2 O. The latter is preferred because it more readily adapts to the directly integrated configurations of FIGS. 3 and 4, i.e., refrigerant supplied directly to the chiller and solution supplied directly to the heat recovery vapor generator (HRVG). This reduces cost and allows use of lower exhaust temperatures.
The minimum required exhaust temperature can be further reduced in those flowsheets having an IP absorber by adding a second coil at the entrance of the inlet chiller, cooled by an IP evaporator. The IP vapor is then absorbed in the IP absorber.
For NH 3 —H 2 O ARUs, the low pressure is in the approximate range of 3 to 6 bar, high pressure (caused by ambient cooling temperature) of 8 to 20 bar, and IP 1 to 4 bar above low pressure.
This moisture spray can be after only partial compression (inter-stage spray) as well as after final compression.
The combustion engine can be a reciprocating type in lieu of the illustrated turbine type.
Other exhaust heat recovery apparatus may be present, e.g., cogeneration of steam, in the hotter section of the HRVG.
Some of the cooled inlet air and/or spray cooling may be applied to electrical circuit cooling as needed.
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An improvement to an energy conversion engine in which fuel is combusted with compressed air is disclosed. Referring to FIG. 3 , the inlet air to compressor ( 30 ) is chilled in chiller ( 34 ) sufficiently to condense moisture. The moisture is pressurized and routed to at least one of chilled inlet fogger ( 312 ) and compressed air sprayer ( 314 ). Engine exhaust heats an absorption refrigeration unit once-through generator ( 316 ), which supplies the refrigeration to chiller ( 34 ).
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BACKGROUND
[0001] 1. Field of the Invention
[0002] This invention relates to the field of material removing tools, and in particular, to saw blades having gullets spaced along the periphery thereof, the gullets being sized and shaped to form indicia corresponding to an aspect of the tool.
[0003] 2. Background Information
[0004] Common material removal tools include cutting and abrasive tools such as saw blades, abrasive saw blades, and core drill bits, which are widely used on conventional power saws and grinding machines. These tools are often circular, and configured for being centrally mounted on a machine spindle for operational rotation thereabout. Other such tools, such as band saw blades and the like, are configured for being driven around a pair of pulleys. All of these tools tend to be configured for uni-directional material-removing movement relative to a workpiece.
[0005] Such tools have often been provided with peripheral gullets or gullet-like indentations (i.e., voids) to provide functions such as debris (e.g., swarf) removal, cooling, and stress relief, during operation. Gullets/voids have also been used in grinding and sanding wheels to provide visual access to the workpiece during operation, such as disclosed in U.S. patent application Ser. No. 09/769,941 to Conley, et al., filed on Mar. 2, 2001, entitled Abrasive Wheels With Workpiece Vision Feature.
[0006] The uni-directional nature of many of these tools generally necessitates proper installation on the machine. The requisite directional orientation is often not easily apparent to casual or even experienced users by a simple visual inspection of the tool itself. For this reason, the proper directional orientation of the tool is often printed, painted, or otherwise marked directly on the tool, to facilitate proper installation. Additional markings, including trademark, trade dress, or other source of origin elements, are also often affixed directly to the tool in a similar manner. Disadvantageously however, such indicia is often worn away or otherwise removed during tool operation, to complicate the proper identification of orientation and/or source of origin of the tool. This may lead to improper re-installation in the event the tool is removed from the machine, and may lead to fewer re-orders due to a failure to properly identify the source of origin of the tool.
[0007] Thus, a need exists for an improved cutting/abrasive tool that addresses the aforementioned drawbacks.
SUMMARY
[0008] One aspect of the present invention includes a circular diamond abrasive saw blade including a circular metallic body having a substantially central aperture through which the saw blade is mountable to a rotatable drive shaft. A series of cutters are located in spaced relation along a periphery of the body, and a series of gullets are located in spaced relation between the cutters. The gullets extend radially inward from the periphery of the body, and are sized and shaped in the form of indicia. The indicia may include letters, numbers, graphic shapes, and/or combinations thereof.
[0009] Another aspect of the present invention includes a tool configured for being driven in a longitudinal direction to remove material from a workpiece. The tool includes a body, mountable to a drive mechanism, and a series of cutters located in spaced relation along a periphery of the body. At least one gullet is located between the cutters, the gullet extending inwardly from the periphery. The gullet is sized and shaped to form indicia, such as in the form of letters, numbers, graphic shapes, and/or combinations thereof.
[0010] A further aspect of the invention includes a method for labeling a metallic core diamond abrasive cutting tool. The method includes cutting a series of symbols, such as letters, numbers, graphic shapes, and combinations thereof, from the metallic core to visually label the tool and provide stress relief along a perimeter of the metallic core during operation of the tool.
[0011] In yet another aspect of the invention, a method is provided for fabricating a circular abrasive cutting tool having permanent indicia thereon. The method includes providing a substantially circular body having a central aperture through which the body is mountable to a rotatable drive shaft, and providing cutters along a periphery of the body. The method also includes locating at least one gullet on the body, extending from the periphery towards the aperture, and configuring the gullet(s) in the form of indicia selected from the group consisting of alphanumeric and design symbols.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] The above and other features and advantages of this invention will be more readily apparent from a reading of the following detailed description of various aspects of the invention taken in conjunction with the accompanying drawings, in which:
[0013] [0013]FIG. 1A is a plan view of one embodiment of a material removal tool of the present invention, with optional aspects thereof shown in phantom;
[0014] [0014]FIG. 1B is a plan view, on an enlarged scale, of a portion of the material removal tool of FIG. 1A;
[0015] [0015]FIG. 2 is an elevational view of the material removal tool of FIG. 1A;
[0016] [0016]FIG. 3 is a plan view of an alternate embodiment of a material removal tool of the present invention; and
[0017] FIGS. 4 - 6 are views similar to that of FIG. 3, of still other embodiments of the material removal tool of the present invention.
DETAILED DESCRIPTION
[0018] Referring to the figures set forth in the accompanying drawings, the illustrative embodiments of the present invention will be described in detail hereinbelow. For clarity of exposition, like features shown in the accompanying drawings shall be indicated with like reference numerals and similar features as shown in alternate embodiments in the drawings shall be indicated with similar reference numerals.
[0019] Embodiments of the present invention include metallic core diamond abrasive cutting tools, e.g., saw blades of the type commonly used to cut masonry, having gullets configured as alphanumeric, and/or graphical, indicia. These gullets are typically cut into the metallic core, but may be provided using any suitable metal fabrication process or technique. The gullets may be configured to provide source of origin information (e.g., trademark or service mark indicia), safety information, or a combination thereof. For example, the gullets may be configured with letters and/or symbols that represent a tool seller's name or trademark, and/or which are assymetrical, so as to be legible when the tool is installed in the proper (e.g., rotational) orientation on a particular piece of equipment (e.g., power saw).
[0020] Embodiments of the invention thus offer the combined functions of providing indicia that will not wear off or become similarly compromised during use, while simultaneously providing stress relief along the perimeter of the metallic core.
[0021] Where used in this disclosure, the term “axial” when used in connection with a tool (e.g., saw blade) described herein, shall refer to a direction relative to the tool, which is substantially parallel to its center of rotation a (FIGS. 1A and 2) during operation. The “longitudinal” and/or “cutting” direction of a tool refers to the direction of material-removing movement of the tool relative to a workpiece. For example, in the event the tool is circular, the longitudinal/cutting direction is orthogonal to the axial direction. The “face” of a tool is a surface thereof, which extends in the cutting direction.
[0022] Referring now to the figures, various embodiments of the present invention are described. Turning to FIGS. 1 A- 2 , an embodiment of the present invention includes a cutting tool, such as a masonry circular saw blade 10 . Blade 10 includes a metallic core 12 , having a central hole or aperture 11 through which the blade 10 may be mounted and fastened to the spindle of a circular saw (not shown) in a conventional manner, e.g., with a threaded fastener. As shown, the core 12 is substantially circular in shape, and may comprise substantially any material having a sufficient specific strength, and desirably, a density of, about 2.0 to about 8.0 g/cm 3 . Examples of suitable materials are steel, aluminum, titanium, bronze, their composites and alloys, and combinations thereof. Reinforced plastics having sufficient specific strength may also be used to construct the core. Generally desirable metallic core materials include ANSI 4140 steel and aluminum alloys, 2024 , 6065 and 7178 .
[0023] A plurality of cutters 14 is disposed in spaced relation along the periphery of the core, between a series of gullets 16 , 18 . As shown, cutters 14 may include abrasive segments of the type used on conventional abrasive saw blades. These segments include abrasive grain brazed or otherwise secured to the surface of core 12 . Substantially any conventional abrasives may be used, such as, but not limited to, alumina in fused, sintered, and/or sol gel form, silica, silicon carbide, zirconia-alumina, fused or sintered alloys of alumina with at least one ceramic oxide selected from the group consisting of MgO, COO, TiO 2 , V 2 O 3 Cr 2 O 3 , ceria, boron suboxide, garnet, and emory. Superabrasive grains may also be used, including but not limited to diamond and cubic boron nitride (CBN), with or without a metal coating.
[0024] Moreover, as an optional variation, blade 10 may be provided with cutters 14 ′ which include a series of teeth 15 , as shown in phantom in FIG. 1A. Teeth 15 may be of nominally any size and shape commonly used on saw blades, e.g., to cut relatively soft materials such as wood, plastic, and the like. As a further variation, teeth 15 may be provided with conventional hardened tips (not shown), such as fabricated from tungsten carbide.
[0025] As shown, the gullets 16 , 18 extend radially inward from the periphery of core 12 , preferably terminating at a radiused (e.g., substantially circular) surface 20 (FIG. 1B). The skilled artisan will recognize that radiused surface 20 advantageously helps to attenuate stresses that may otherwise tend to generate stress fractures in the core at the base of the gullet.
[0026] The gullets may be configured in the form of substantially any desired indicia, including alphanumeric characters and/or various design elements. For example, in the embodiment shown in FIGS. 1A and 1B, gullets 18 are configured to form the letter “W”.
[0027] As also shown, every gullet 16 , 18 , need not be configured as indicia. Rather, the indicia-configured gullets 18 may be interspersed among conventional gullets 16 as shown. This interspersed arrangement may be particularly useful in embodiments that employ cutters 14 ′, each of which have a relatively large number of teeth 15 and gullets 16 , as described hereinabove.
[0028] Gullets 18 are typically cut into the core using conventional cutting or milling processes. However, the gullets may be provided using any suitable fabrication process, including molding, stamping, or laser cutting.
[0029] Turning to FIGS. 3, 5, and 6 , alternate embodiments of wheel 10 are shown as wheels 110 , 310 , 410 , having gullets 118 , 318 , 418 , which are shaped as the letters, “N”, “C”, and “V”, respectively. Although these figures depict wheels that each have gullets of the same letter, individual wheels may be provided with substantially any combination of alphanumeric, or other, symbols. A single wheel may thus be provided with gullets configured as various letters, to enable acronyms, abbreviations, or words to be formed. In this manner, tools 10 , 110 , etc., may be customized for particular purchasers.
[0030] For example, turning now to FIG. 4, a tool 210 manufactured by “Saint-Gobain Abrasives, Inc.” may be customized with a repeating pattern of “s”, “t” and “g” shaped gullets 218 , 218 ′, 218 ″. In addition to alphanumeric indicia, the gullets may be configured in the form of a corporate logo. (An example of a corporate logo that may be suitable for such use is the NIKE® SWOOSH® logo, Nike Corporation, Beaverton Oreg.). This embodiment thus provides a non-removable trademark/indication of source of origin, which may serve as a convenient means for maintaining brand identity among their customers.
[0031] This embodiment also provides a convenient means for ‘brand-labeling’ the tools for re-sale, such as by configuring the gullets with indicia associated with the customer/reseller. In this manner, the reseller may be provided with a customized tool line for sale to its end-user customers. This approach, including the nominally permanent marking, may encourage greater brand loyalty by their customers.
[0032] Also, as discussed hereinabove, while the gullets 18 , 118 , etc., combine identification with the functional aspects of stress relief and debris/swarf removal, another potential functional aspect of these embodiments is increased safety. Since the alphanumeric indicia is cut into the core, extending completely through the axial dimension thereof, these indicia will be properly viewable and/or legible, (i.e., upright and legible from left to right at the top of the blade as shown in FIG. 4) from one face of the blade, while the mirror image (i.e., upright, but backwards at the top of the blade) would be seen from the other face (e.g., in the event the blade were installed incorrectly). As mentioned hereinabove, many saw blades are uni-directional, i.e., they are designed to cut in a single direction through a workpiece. The skilled artisan will recognize that such uni-directionality is typically a function of asymmetries in the configuration of the segments 14 , such as generated by the orientation of individual abrasive grains and/or cutting teeth thereon. As such, operation of such blades in the reverse direction may result in inefficient cutting performance and/or reduced safety. To address these concerns, embodiments of the present invention may be fabricated so that the alphanumeric indicia are properly viewable from the threaded-fastener-side of a particular power saw, such as shown in FIG. 4, when properly installed. These embodiments thus provide an easily discernable visual indication of whether or not the blade 18 , 118 , etc., is properly installed. Moreover, since this directional information is provided independently of conventional painted or otherwise applied markings on the face of the core 12 , the quality of such visual indication will not rub off, smudge, or otherwise degrade during use.
[0033] Although the present invention has been described with respect to circular saw blades, the skilled artisan will recognize that substantially any type of cutting or grinding tool of the type having gullets, may be used, without departing from the spirit and scope of the invention. For example, otherwise conventional band saw blades may be provided with the gullet configurations disclosed herein. In addition, non-abrasive circular saw blades of the type commonly used to cut wood, plastic, and other relatively soft materials may incorporate the gullets described herein. Moreover, although the tools described herein are cutting tools or abrasive cutting tools, the skilled artisan should recognize that gullets configured as described hereinabove, may be applied to other types of material removal tools, such as conventional steel core, segmented diamond abrasive wheels, without departing from the spirit and scope of the present invention.
[0034] In addition, although the embodiments described herein disclose gullets shaped as indicia, such indicia may be placed elsewhere on the tool, such as inward of the tool's periphery, without departing from the spirit and scope of the invention.
[0035] In the preceding specification, the invention has been described with reference to specific exemplary embodiments thereof. It will be evident that various modifications and changes may be made thereunto without departing from the broader spirit and scope of the invention as set forth in the claims that follow. The specification and drawings are accordingly to be regarded in an illustrative rather than restrictive sense.
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A tool such as a circular diamond abrasive saw blade includes a circular metallic body having a substantially central aperture through which the saw blade is mountable to a rotatable drive shaft, and a plurality of cutters disposed in spaced relation along a periphery of said body. A plurality of gullets are located in spaced relation between the cutters, extending radially inward from the periphery. The gullets are sized and shaped in the form of alphanumeric or graphical indicia.
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FIELD OF THE INVENTION
This invention relates to a novel and improved strengthening or reinforcing member of high strength steel that is adapted particularly for strengthening or reinforcing a metal panel or plate. More specifically, the invention relates to a novel and improved beam for reinforcing an automotive vehicle door.
BACKGROUND OF THE INVENTION
In the automotive vehicle industry today, it is necessary to comply with government regulations that establish certain minimum strength requirements for the side doors of the vehicles. The purpose of such regulations is to minimize the safety hazard caused by an intrusion into the passenger compartment in a side impact accident.
Various types of reinforcing door beams have been proposed to meet these requirements, e.g., tubular steel beams, sheet steel stampings, and roll formed high strength steel sections of various configurations. Engineers responsible for designing reinforcing door beams must contend with a number of requirements that often conflict with one another. For example, it is desirable to maximize the performance of reinforcing door beams by designing beams that absorb high loads (principally bending loads), deflect significantly before failure, and absorb as much energy as possible during the absorption of impact loads. At the same time, it is also desirable to minimize the weight and size of reinforcing door beams. With regard to size, placement of a door reinforcing beam within an automobile door assembly makes it important for the door reinforcing beam to have a relatively small cross-sectional geometry, in order to avoid interference with other structures and/or mechanisms within the door, such as those used to operate a window associated with the door. Such size and weight considerations can make it difficult to achieve the desired performance of reinforcing door beams for load capacity, deflection before failure, and impact energy absorption.
Previously proposed door beams provided the desired degree of high strength, but often presented other disadvantages. For example, martensitic steel has limited ductility, thus placing some restrictions on the permissible cross sectional configurations obtainable by roll forming. Accordingly, past designs for door reinforcement members constructed of high strength martensitic steel typically had cross-sectional geometries, such as, for example, a hat-shaped cross-sectional geometry, that buckled or spread on bending, thereby reducing mass effectiveness in providing side impact protection.
SUMMARY OF THE INVENTION
The present invention is directed to an improved roll formed, ultra high strength steel beam having a closed cross-sectional geometry. More particularly, the present invention is directed to roll formed, ultra high strength steel beams having a closed cross-sectional, and generally trapezoidal shaped, geometry.
This is accomplished by forming the closed cross-sectional geometry by induction welding opposite edges of the roll formed beam to one another. As used herein, the term "ultra high strength steel" means steel having a yield strength of 80 KSI (5.52 MPa) or higher.
Other features and advantages are inherent in the methods and apparatus claimed and disclosed or will become apparent to those skilled in the art from the following detailed description in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is described in detail below with reference to the accompanying drawings, in which:
FIG. 1 is a side elevational view of an automotive vehicle showing a reinforcing member in the side door of the vehicle, in accordance with one embodiment of the invention;
FIG. 2 is a schematic cross-sectional view taken generally along the line 2--2 of FIG. 1;
FIG. 3 is a schematic representation of the reinforcing member when subjected to a commonly used bending force test;
FIG. 4 is a cross-sectional view of the reinforcing member, taken generally along the line 4--4 of FIG. 2;
FIG. 4A is a cross-sectional view, similar to that of FIG. 4, showing a prior art reinforcing member;
FIG. 5 is a cross-sectional view, similar to that of FIG. 4, showing a first alternative embodiment of the reinforcing member; and
FIG. 6 is a cross-sectional view, similar to that of FIG. 4, showing a second alternative embodiment of the reinforcing member.
DETAILED DESCRIPTION
Referring to FIGS. 1 and 2, an automotive vehicle 10 is shown which has a side door 11 formed from spaced inner and outer panel portions 12 and 13, respectively. An elongated reinforcing beam 14 is positioned transversely within the door and is secured adjacent the inside surface of the outer panel 13 by means of suitable end brackets, shown schematically as 16 and 17, which transmit the load to the hinge and latch portions of the door structure, respectively. Typically, a gap of about 0.20 inches (about 5.0 mm) is provided between the inside surface of the outer panel 13 and the reinforcing bar 14 with soft rubber "gum drops" (not shown) disposed within the gap, so that the outer panel 13 is not deformed (i.e., creased) by relatively light loads applied to the outer panel 13, such as, for example, when a person simply leans against outer panel 13. As seen in FIG. 1, reinforcing beam 14 extends substantially horizontally across the width of side door 11 at approximately the waist height of an occupant seated in the vehicle. However, other orientations of reinforcing beam 14 within side door 11 can also be used.
Although the invention is not limited to a specific cross sectional configuration, the preferred configuration can be described as generally trapezoidal-shaped. As illustrated in FIG. 4, reinforcing beam 14 has a thickness t, typically about 0.05 inches (about 1.27 mm) to about 0.10 inches (about 2.54 mm), and includes a pair of angled web portions 22 and 24, an outboard flange portion 26, and an inboard flange portion 28. Reinforcing beam 14 has an overall height H, typically about 1 inch (about 2.5 cm) to about 1.6 inches (about 4.1 cm). Outboard flange portion 26, has a width W 1 , typically about 0.6 inches (about 1.5 cm) to about 1.2 inches (about 3.1 cm), and is substantially shorter than inboard flange portion 28, which has a width W 2 , typically about 1 inch (about 2.5 cm) to about 1.6 inches (about 4.1 cm). Inboard flange portion 28 is formed by welding opposite edges 30 and 32 of reinforcing beam 14 to one another at a weld 34 after roll forming. Preferably, weld 34 is an induction weld that extends substantially uninterrupted along substantially the entire length of reinforcing beam 14.
The prevailing government strength requirements for the side doors of motor vehicles are defined in the Federal Motor Vehicle Safety Standard No. 214 which specifies a certain minimum crush resistance for the vehicle when subjected to a specified test procedure. FIG. 3 is a schematic illustration of a beam test procedure used to assess side impact performance in connection with the vehicle door illustrated in FIGS. 1 and 2. As noted above, reinforcing beam 14 is mounted within door 11 so that the outboard flange portion 26 of reinforcing beam 14 is adjacent the inside surface of outer panel 23 and thus receives the initial deflecting force of a simulated impact. In the test procedure, a loading device or ram consisting of a rigid cylinder 36 of specified dimensions is used to apply a load to the outer surface of door panel 13 in an inward direction, as indicated by the large arrow, at a specified rate of travel. During the test, the applied load and the displacement are recorded either continuously or in increments, and from these data, the initial, intermediate, and peak crush resistances are determined. As seen in FIG. 3, the bending of reinforcing beam 14 during the test places outboard flange portion 26 in compression, inboard flange portion 28 in tension, and angled web portions 22 and 24 primarily in shear.
As an example, reinforcing beam 14 made from AISI Grade 190 SK high strength steel has been tested in bending and has been found to have the following capabilities for a 40 inch span having a thickness t of about 0.068 inches (about 1.73 mm), W 1 of about 0.85 inches (about 2.16 cm), W 2 of about 1.29 inches (about 3.28 cm), and H of about 1.36 inches (about 3.45 cm):
Weight per unit length=0.98 pounds/foot (1.46 Kg/m)
Peak load=2,714 pounds (12,072 N)
Deflection before drop in load=4.5 inches (11.43 cm)
Energy at 6" deflection=11,687 inch-pounds (1,320 N-m)
Energy at 7" deflection=13,301 inch-pounds (1,503 N-m)
For comparison, a prior art reinforcing beam made from the same type and thickness of steel, but having a hat-shaped cross-sectional geometry, as illustrated in FIG. 4A, with a top width, W 1 of about 1.40 inches (about 3.56 cm), an overall width W 0 of about 2.65 inches (about 6.73 cm), and a height H' of about 1.34 inches (about 3.40 cm), was found to have the following capabilities for a 40 inch (101.6 cm) span:
Weight per unit length=1.06 pounds/foot (1.58 Kg/m)
Peak load=2,727 pounds (12,130 N)
Deflection before drop in load=2.75 inches (7.00 cm)
Energy at 6" deflection=10,305 inch-pounds (1,164 N-m)
Energy at 7" deflection=11,411 inch-pounds (1,289 N-m)
FIG. 5 illustrates a first alternative embodiment of the invention in which a reinforcing beam 114 is substantially identical to reinforcing beam 14 of FIGS. 1 through 4. However, reinforcing beam 114 includes an additional ultra high strength steel reinforcement 140 having a length of about 6 inches (about 15.24 cm) to about 12 inches (30.48 cm) and extending over at least the central part of its span. Reinforcement 140 preferably has a thickness of no more than about half of the thickness t of reinforcing beam 114 (e.g., no more than about 0.034 inches (about 0.86 mm) for a reinforcing beam 114 having a thickness t of about 0.068 inches (about 1.73 mm)) and is secured to the interior surface of an outboard flange portion 126 of reinforcing beam 114 by any suitable means, such as, for example, by spring action against the interior surface of reinforcing beam 114. Reinforcement 140 adds further impact absorbing capability for reinforcing beam 114, as compared to reinforcing beam 14, by delaying the onset of buckling of outboard flange portion 126 when subjected to an impact load.
FIG. 6 illustrates a second alternative embodiment of the invention in which a reinforcing beam 214 is configured and sized similarly to reinforcing beam 14 of FIGS. 1 through 4. However, reinforcing beam 214 includes a rounded outboard flange portion 226 instead of the substantially flat outboard flange portion 26 of reinforcing beam 14. Rounded outboard flange portion 226 preferably has an inner radius of curvature R1 of about 0.30 inches (about 0.76 cm) to about 0.6 inches (about 1.52 cm).
It is believed that, for optimal performance, a reinforcing beam in accordance with the invention having a flat outboard flange portion should have the outboard flange portion width W 1 on the order of about 14 times the thickness t of the reinforcing beam, or less. The outboard flange portion width W 2 should also be equal to or less than 0.75 times the inboard flange portion width W 2 , in order to avoid excessive strain in tension on the inboard flange portion during bending that occurs if the cross-sectional geometry approaches a substantially square shape.
Similarly, it is believed that, for optimal performance, a reinforcing beam having a rounded outboard flange portion in accordance with the invention should have the inner radius of curvature R1 on the order of about 9 times the thickness t of the reinforcing beam, or less.
The foregoing detailed description has been given for clearness of understanding only, and no unnecessary limitations should be understood therefrom, as modifications will be obvious to those skilled in the art.
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An improved strengthening or reinforcing member, and in particular an automotive vehicle door reinforcing beam, constructed from ultra high strength steel is disclosed. The door reinforcing beam has a substantially trapezoidal shaped cross-sectional geometry and optionally can include an additional reinforcement extending over a central portion of the beam. In an alternative embodiment, a rounded outboard flange portion can be substituted for a generally flat outboard flange portion. The door reinforcing beam exhibits a substantial improvement in load carrying capability for a given mass, as compared to door reinforcing beams having other cross-sectional geometries, such as hat-shaped cross-sectional geometries.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. patent application Ser. No. 13/707,317, filed Dec. 6, 2012, now U.S. Pat. No. 8,893,542, which is a continuation of U.S. patent application Ser. No. 12/702,059, filed Feb. 8, 2010, now U.S. Pat. No. 8,327,689, which is a division of U.S. patent application Ser. No. 11/865,525, filed Oct. 1, 2007, now U.S. Pat. No. 7,849,728, which is a continuation of U.S. patent application Ser. No. 11/210,715, filed Aug. 24, 2005, now U.S. Pat. No. 7,275,417, which is a continuation of U.S. patent application Ser. No. 10/935,024, filed Sep. 7, 2004, now U.S. Pat. No. 6,964,283, which is a continuation of U.S. patent application Ser. No. 10/180,047, filed Jun. 27, 2002, now U.S. Pat. No. 6,802,344, which is a divisional of U.S. patent application Ser. No. 09/725,727, filed Nov. 30, 2000, now U.S. Pat. No. 6,622,757, which relates to and claims priority to U.S. Provisional Patent Application Ser. No. 60/202,659, filed on May 8, 2000, entitled “Method of Determining Failure of Fuel Vapor Recovery System,” U.S. Provisional Patent Application Ser. No. 60/202,054, filed on May 5, 2000, entitled “Fueling System Vapor Recovery Performance Monitor,” and U.S. Provisional Patent Application Ser. No. 60/168,029, filed on Nov. 30, 1999, entitled “Fueling System Vapor Recovery Performance Monitor.” Each of the foregoing applications is incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to a vapor recovery performance monitor for use in connection with gasoline dispensing facilities.
BACKGROUND OF THE INVENTION
[0003] Gasoline dispensing facilities (i.e. gasoline stations) often suffer from a loss of fuel to the atmosphere due to inadequate vapor collection during fuel dispensing activities, excess liquid fuel evaporation in the containment tank system, and inadequate reclamation of the vapors during tanker truck deliveries. Lost vapor is an air pollution problem which is monitored and regulated by both the federal government and state governments. Attempts to minimize losses to the atmosphere have been effected by various vapor recovery methods. Such methods include: “Stage-I vapor recovery” where vapors are returned from the underground fuel storage tank to the delivery truck; “Stage-II vapor recovery” where vapors are returned from the refueled vehicle tank to the underground storage tank; vapor processing where the fuel/air vapor mix from the underground storage tank is received and the vapor is liquefied and returned as liquid fuel to the underground storage tank; burning excess vapor off and venting the less polluting combustion products to the atmosphere; and other fuel/air mix separation methods.
[0004] A “balance” Stage-II Vapor Recovery System (VRS) may make use of a dispensing nozzle bellows seal to the vehicle tank filler pipe opening. This seal provides an enclosed space between the vehicle tank and the VRS. During fuel dispensing, the liquid fuel entering the vehicle tank creates a positive pressure which pushes out the ullage space vapors through the bellows sealed area into the nozzle vapor return port, through the dispensing nozzle and hoe paths, and on into the VRS.
[0005] It has been found that even with these measures, substantial amounts of hydrocarbon vapors are lost to the atmosphere, often due to poor equipment reliability and inadequate maintenance. This is especially true with Stage-II systems. One way to reduce this problem is to provide a vapor recovery system monitoring data acquisition and analysis system to provide notification when the system is not working as required. Such monitoring systems may be especially applicable to Stage-II systems.
[0006] When working properly, Stage-II vapor recovery results in equal exchanges of air or vapor (A) and liquid (L) between the main fuel storage tank and the consumer's gas tank. Ideally, Stage-II vapor recovery produces an A/L ratio very close to 1. In other words, returned vapor replaces an equal amount of liquid in the main fuel storage tank during refueling transactions. When the A/L ratio is close to 1, refueling vapors are collected, the ingress of fresh air into the storage tank is minimized and the accumulation of an excess of positive or negative pressure in the main fuel storage tank is prevented. This minimizes losses at the dispensing nozzle and evaporation and leakage of excess vapors from the containment storage tank. Measurement of the A/L ratio thus provides an indication of proper Stage-II vapor collection operation. A low ratio means that vapor is not moving properly through the dispensing nozzle, hose, or other part of the system back to the storage tank, possibly due to an obstruction or defective component.
[0007] Recently, the California Air Resources Board (CARB) has been producing new requirements for Enhanced Vapor Recovery (EVR) equipment. These include stringent vapor recovery system monitoring and In-Station Diagnostics (ISD) requirements to continuously determine whether or not the systems are working properly. CARB has proposed that, when the A/L ratio drops below a prescribed limit for a single or some sequence of fueling transactions, an alarm be issued and the underground storage tank pump be disabled to allow repair to prevent further significant vapor losses. The proposed regulations also specify an elaborate and expensive monitoring system with many sensors which will be difficult to wire to a common data acquisition system.
[0008] The CARB proposal requires that Air-to-Liquid (A/L) volume ratio sensors be installed at each dispensing hose or fuel dispensing point and pressure sensors be installed to measure the main fuel storage tank vapor space pressure. Note that the term ‘Air’ is used loosely here to refer to the air-vapor mix being returned from the refueled vehicle tank to the Underground storage tank. The sensors would be wired to a common data acquisition system used for data logging, storage, and limited pass/fail analysis. It is likely that such sensors would comprise Air Flow Sensors (AFS's).
[0009] A first embodiment of the present invention provides a more practical and less expensive solution than that proposed by CARB, which can substantially provide the monitoring capabilities needed. In this first embodiment of the present invention, the multiple AFS's called for by the CARB proposal may be replaced by fewer, or only one, AFS in conjunction with a more sophisticated AFS data analysis method.
[0010] With respect to use of vapor pressure sensors, CARB also proposes that these sensors be used to passively monitor the level of pressure in the main fuel storage tank vapor space, which is common to the fueling facility, to not only provide indication of proper operation of Stage-II vapor recovery methods, but also system containment integrity. This is done by monitoring the pressure patterns that occur within the storage tank during the various phases of storage tank and dispenser operation. The complexity of these patterns is a function of the type of Stage-II system in use.
[0011] CARB has proposed putting constraints on the pressure versus time relationships to identify when the vapor recovery system is causing undesirably high pressures for long enough time periods. when the vapor recovery system produces these elevated pressures, it may force significant amounts of vapor past the pressure relief valve at the end of the storage tank vent pipe or out of other leaky system valves and fittings and into the atmosphere as air pollution.
[0012] CARB proposes a passive test for identifying elevated storage tank pressures. The purpose of the passive test is to determine whether vapors are being properly retained in the storage tank vapor space. This is done by continuously monitoring and watching for evidence of a non-tight or improperly operated vapor recovery components by tracking small pressure levels over time and comparing them to prescribed operating requirements.
[0013] For instance, for a vapor recovery system that is intended to continuously maintain negative storage tank vapor space pressures, the CARB proposed requirements were (at one time) that an error condition would exist when pressure exceeds (i.e. is higher than) −0.1 inch water column (w.c.) for either more than one (1) consecutive hour, or more than 3 hours in any 24 hour period. An error condition would also exist when pressure exceeds (i.e. is higher than) +0.25 inches w.c. for either more than one (1) consecutive hour, or more than 3 hours in any 24 hour period. An error condition would also exist if pressure exceeded +1.0 inches w.c. for more than 1 hour in any 24 hour period. Determination of the foregoing error conditions requires frequent pressure measurements, data storage, and analysis. CARB has struggled with these requirements for a passive-type test and has changed them more than once.
[0014] In a second embodiment of the invention the CARB proposed passive pressure monitoring test may be augmented or replaced with an active pressure “tightness” or “leakage” test which provides a more definitive indication of system containment integrity. The active tightness test may only need to be run occasionally to find a break in the system. A once a day or once a month test is consistent with the intent of the variously proposed CARB test pass/fail criteria.
[0015] In yet another embodiment of the invention, the CARB proposed passive test for leakage may be replaced with an improved passive test for vapor leakage. Instead of measuring absolute pressure in the vapor containing elements of a facility, in the improved test changes in pressure over time are used to determine whether vapors are leaking from the system.
[0016] Both the aforementioned CARB methods for determining vapor recovery system performance and those of the invention may be detrimentally effected by the introduction of vehicles with Onboard Refueling Vapor Recovery (ORVR) devices that recover refueling vapors onboard the vehicle. Vapors produced as a result of dispensing fuel into an ORVR equipped vehicle are collected onboard, and accordingly, are not available to flow through a vapor return passage to an AFS for measurement. Thus, refueling an ORVR equipped vehicle results in a positive liquid fuel flow reading, but no return vapor flow reading (i.e. an A/L ratio equal to 0 or close thereto)—a condition that normally indicates vapor recovery malfunction. Because the vapor recovery system cannot distinguish between ORVR equipped vehicles and conventional vehicles, the vapor recovery system may be falsely determined to be malfunctioning when an ORVR equipped vehicle is refueled.
[0017] In the coming years, 2000 to 2020 and beyond, the proportion of ORVR vehicles in use will increase. Therefore this problem will be become more severe in the coming decades. If A/L sensing is to be used successfully for vapor recovery system monitoring, then a method is needed to distinguish between failed vapor recovery test events caused by an ORVR vapor-blocking vehicle and true failed vapor recovery test events (which can only occur for non-ORVR equipped vehicles).
OBJECTS OF THE INVENTION
[0018] It is therefore an object of the present invention to provide a method and system for determining acceptable performance of a vapor recovery system in a fueling facility.
[0019] It is another object of the present invention to provide a method and system for measuring the return flow of vapors from a dispensing point to a main fuel storage tank.
[0020] It is yet another object of the present invention to reduce the number of devices required to determine A/L ratios for individual dispensing points in a fueling facility.
[0021] It is still yet another object of the present invention to provide a method and system for determining the integrity of vapor containment in a main fuel storage tank.
[0022] It is still a further object of the present invention to provide a method and system for analyzing and indicating vapor recovery performance in a fueling facility.
[0023] It is still another object of the present invention to provide a system and method for determining true vapor recovery system failures.
[0024] It is yet another object of the present invention to provide a system and method for distinguishing between low A/L readings caused by a vapor recovery system failure and low A/L readings caused by the fueling of an ORVR-equipped vehicle.
[0025] Additional objects and advantages of the invention are set forth, in part, in the description which follows, and, in part, will be apparent to one of ordinary skill in the art from the description and/or from the practice of the invention.
SUMMARY OF THE INVENTION
[0026] In response to the foregoing challenges, applicants have developed an innovative system for monitoring vapor recovery in a liquid fuel dispensing facility having at least one fuel dispensing point connected to a main fuel storage system by a means for supplying liquid fuel to the dispensing point and a means for returning vapor from the dispensing point, said monitoring system comprising: a vapor flow sensor operatively connected to the means for returning vapor and adapted to indicate the amount of vapor flow through the means for returning vapor; a liquid fuel dispensing meter operatively connected to the means for supplying liquid fuel and adapted to indicate the amount of liquid fuel dispensed at the at least one fuel dispensing point; and a central electronic control and diagnostic arrangement having, a means for determining a ratio of vapor flow to dispensed liquid fuel for the at least one fuel dispensing point, said determining means receiving dispensed liquid fuel amount information from the liquid fuel dispensing meter and receiving vapor flow amount information from the vapor flow sensor, wherein the acceptability of vapor recovery for the fuel dispensing point is determined by said ratio of vapor flow to dispensed liquid fuel.
[0027] Applicants have also developed an innovative system for monitoring vapor recovery in a liquid fuel dispensing facility having at least two fuel dispensing points connected to a main fuel storage system by a vapor return pipeline, said monitoring system comprising: a vapor flow sensor operatively connected to the vapor return pipeline; means for determining dispensed liquid fuel amount information for each fuel dispensing point; and a means for determining a ratio of vapor flow to dispensed liquid fuel for the fuel dispensing points based on vapor flow sensor readings and dispensed liquid fuel amount information, wherein the acceptability of vapor recovery for the fuel dispensing points is determined by said ratio of vapor flow to dispensed liquid fuel.
[0028] Applicants have also developed an innovative method of monitoring vapor recovery in a liquid fuel dispensing facility having at least one fuel dispensing point connected to a main fuel storage system by a means for supplying liquid fuel to the dispensing point and a means for returning vapors from the dispensing point, said monitoring method comprising the steps of: determining at multiple times an amount of vapor flow through the means for returning vapors; determining at multiple times an amount of liquid fuel dispensed through the means for supplying liquid fuel; and determining a ratio of vapor flow to dispensed liquid fuel for the fuel dispensing point based on the amount of vapor flow through the means for returning vapors and the amount of liquid fuel dispensed through the means for supplying liquid fuel, wherein the acceptability of vapor recovery for the fuel dispensing point is determined by said ratio of vapor flow to dispensed liquid fuel.
[0029] Applicants have still further developed an innovative system for monitoring vapor containment in a liquid fuel dispensing facility having a main fuel storage system connected by a vent pipe-pressure relief valve arrangement to atmosphere, said monitoring system comprising: a pressure sensor operatively connected to the vent pipe; a vapor processor operatively connected to the vent pipe; and means for determining the acceptability of vapor containment in the main fuel storage system, said determining means being operatively connected to the pressure sensor to receive pressure level information therefrom and being operatively connected to the vapor processor to selectively cause the vapor processor to draw a negative pressure in the main fuel storage system.
[0030] Applicants have developed an innovative method of monitoring vapor containment in a liquid fuel dispensing facility having at least one main fuel storage tank connected by a vent pipe-pressure relief valve arrangement to atmosphere, said monitoring method comprising the steps of: identifying the start of an idle period for the liquid fuel dispensing facility; monitoring the liquid fuel dispensing facility to confirm maintenance of the idle period; determining whether pressure in the main fuel storage tank is equal or below a minimum level; selectively adjusting pressure in the main fuel storage tank to a preset lower level when the previously determined pressure is above the minimum level; monitoring variation of the pressure in the main fuel storage tank during the remainder of the idle period; determining the end of the idle period; and determining the acceptability of vapor containment in the main fuel storage tank based on the variation of the pressure during the idle period.
[0031] Applicants also developed an innovative method of determining vapor recovery system failures associated with a single fuel dispensing point, said method comprising the steps of: determining the vapor flow to dispensed fuel ratios for a plurality of fuel dispensing points; determining the number of vapor flow to dispensed fuel ratios that are below a preset minimum for each of the plurality of fuel dispensing points; determining the average number of vapor flow to dispensed fuel ratios below the preset minimum for the plurality of fuel dispensing points; and comparing the number vapor flow to dispensed fuel ratios below the preset minimum for each of the plurality of fuel dispensing points to the average number of vapor flow to dispensed fuel ratios below the present minimum to determine whether the vapor recovery system associated with each of the plurality of fuel dispensing points has failed.
[0032] It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only, and are not restrictive of the invention as claimed. The accompanying drawings, which are incorporated herein by reference and which constitute a part of this specification, illustrate certain embodiments of the invention, and together with the detailed description serve to explain the principles of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0033] The invention will be described in conjunction with the following drawings in which like reference numerals designate like elements and wherein:
[0034] FIG. 1 is a schematic view of a fueling system vapor recovery performance monitor in accordance with an embodiment of the present invention.
[0035] FIG. 2 is a schematic view of a fueling system vapor recovery performance monitor in accordance with another embodiment of the present invention.
[0036] FIG. 3 is a graph used to convert vapor leakage rates based on ullage pressures.
DETAILED DESCRIPTION OF THE INVENTION
[0037] A first embodiment of the invention is described in connection with FIG. 1 , which shows a vapor recovery and containment monitoring system for use in a liquid fuel dispensing facility 10 . The dispensing facility 10 may include a station house 100 , one or more fuel dispenser units 200 , a main fuel storage system 300 , means for connecting the dispenser units to the main fuel storage system 400 , and one or more vapor (or air) flow sensors (AFS's) 500 .
[0038] The station house 100 may include a central electronic control and diagnostic arrangement 110 that includes a dispenser controller 120 , dispenser current loop interface wiring 130 connecting the dispenser controller 120 with the dispenser unit(s) 200 , and a combined data acquisition system/in-station diagnostic monitor 140 . The dispenser controller 120 may be electrically connected to the monitor 140 by a first wiring bus 122 . The interface wiring 130 may be electrically connected to the monitor 140 by a second wiring bus 132 . The monitor 140 may include standard computer storage and central processing capabilities, keyboard input device(s), and audio and visual output interfaces among other conventional features.
[0039] The fuel dispenser units 200 may be provided in the form of conventional “gas pumps.” Each fuel dispenser unit 200 may include one or more fuel dispensing points typically defined by the nozzles 210 . The fuel dispenser units 200 may include one coaxial vapor/liquid splitter 260 , one vapor return passage 220 , and one fuel supply passage 230 per nozzle 210 . The vapor return passages 220 may be joined together before connecting with a common vapor return pipe 410 . The units 200 may also include one liquid fuel dispensing meter 240 per nozzle 210 . The liquid fuel dispensing meters 240 may provide dispensed liquid fuel amount information to the dispenser controller 120 via the liquid fuel dispensing meter interface 270 and interface wiring 130 .
[0040] The main fuel storage system 300 may include one or more main fuel storage tanks 310 . It is appreciated that the storage tanks 310 may typically be provided underground, however, underground placement of the tank is not required for application of the invention. It is also appreciated that the storage tank 310 shown in FIGS. 1 and 2 may represent a grouping of multiple storage tanks tied together into a storage tank network. Each storage tank 310 , or a grouping of storage tanks, may be connected to the atmosphere by a vent pipe 320 . The vent pipe 320 may terminate in a pressure relief valve 330 . A vapor processor 340 may be connected to the vent pipe 320 intermediate of the storage tank 310 and the pressure relief valve 330 . A pressure sensor 350 may also be operatively connected to the vent pipe 320 . Alternately, it may be connected directly to the storage tank 310 or the vapor return pipe 410 below or near to the dispenser 200 since the pressure is normally substantially the same at all these points in the vapor containment system. The storage tank 310 may also include an Automatic Tank Gauging System (ATGS) 360 used to provide information regarding the fuel level in the storage tank. The vapor processor 340 , the pressure sensor 350 , and the automatic tank gauging system 360 may be electrically connected to the monitor 140 by third, fourth, and fifth wiring busses 342 , 352 , and 362 , respectively. The storage tank 310 may also include a fill pipe and fill tube 370 to provide a means to fill the tank with fuel and a submersible pump 380 to supply the dispensers 200 with fuel from the storage tank 310 .
[0041] The means for connecting the dispenser units and the main fuel storage system 400 may include one or more vapor return pipelines 410 and one or more fuel supply pipelines 420 . The vapor return pipelines 410 and the fuel supply pipelines 420 are connected to the vapor return passages 220 and fuel supply passages 230 , respectively, associated with multiple fuel dispensing points 210 . As such, a “vapor return pipeline” designates any return pipeline that carries the return vapor of two or more vapor return passages 220 .
[0042] The AFS 500 is operatively connected to a vapor return pipeline 410 . A basic premise of the system 10 is that it includes at most one AFS 500 (also referred to more broadly as vapor flow sensors) for each fuel dispenser unit 200 . Thus, the AFS 500 must be operatively connected to the vapor return system downstream of the vapor return passages 220 . If such were not the case, the system would include one AFS 500 per nozzle 210 which violates the basic premise of the invention. Each AFS 500 may be electrically connected to the monitor 140 by a sixth wiring bus 502 .
[0043] In order to determine the acceptability of the performance of vapor recovery in the facility 10 , the ratio of vapor flow to dispensed liquid fuel is determined for each fuel dispensing point 210 included in the facility. This ratio may be used to determine if the fuel dispensing point 210 in question is in fact recovering an equal volume of vapor for each unit volume of liquid fuel dispensed by the dispensing point 210 .
[0044] In the embodiment of the invention shown in FIG. 1 , each dispensing point 210 is served by an AFS 500 that is shared with at least one other dispensing point 210 . Mathematical data processing (described below) is used to determine an approximation of the vapor flow associated with each dispensing point 210 . The amount of fuel dispensed by each dispensing point 210 is known from the liquid fuel dispensing meter 240 associated with each dispensing unit. Amount of fuel (i.e. fuel volume) information may be transmitted from each dispensing meter 240 to the dispenser controller 120 for use by the monitor 140 . In an alternative embodiment of the invention, the dispensing meters 240 may be directly connected to the monitor 140 to provide the amount of fuel information used to determine the A/L ratio for each dispensing point 210 .
[0045] Each AFS 500 measures multiple (at least two or more) dispensing point return vapor flows. In the embodiment of the invention shown in FIG. 1 , a single AFS 500 measures all the dispensing point vapor flows for the facility 10 . In the case of a single AFS per facility 10 , the AFS is installed in the single common vapor return pipeline which runs between all the dispensers as a group, which are all tied together into a common dispenser manifold pipe, and all the main fuel storage tanks as a group, which are all tied together in a common tank manifold pipe. Various groupings of combinations of feed dispensing point air flow's per AFS are possible which fall between these two extremes described.
[0046] With reference to a second embodiment of the invention shown in FIG. 2 , it is appreciated that multiple AFS's 500 could be deployed to measure various groupings of dispensing point 210 vapor flows, down to a minimum of only two dispensing point vapor flows. The latter example may be realized by installing one AFS 500 in each dispenser housing 200 , which typically contains two dispensing point's 210 (one dispensing point per dispenser side) or up to 6 dispensing points (hoses) in Multi-Product Dispensers (MPD's) (3 per side). The vapor flows piped through the vapor return passage 220 may be tied together to feed the single AFS 500 in the dispenser housing.
[0047] As stated above, the monitor 140 may connect to the dispenser controller 120 , directly to the current loop interface wiring 130 or directly to the liquid fuel dispensing meter 240 to access the liquid fuel flow volume readings. The monitor 140 may also be connected to each AFS 500 at the facility 10 so as to be supplied with vapor flow amount (i.e. vapor volume) information. The liquid fuel flow volume readings are individualized fuel volume amounts associated with each dispensing point 210 . The vapor flow volume readings are aggregate amounts resulting from various groupings of dispensing point 210 vapor flows, which therefore require mathematical analysis to separate or identify the amounts attributable to the individual dispensing points 210 . This analysis may be accomplished by the monitor 140 which may include processing means. Once the vapor flow information is determined for each dispensing point 210 , the A/L ratios for each dispensing point may be determined and a pass/fail determination may be made for each dispensing point based on the magnitude of the ratio. It is known that the ratio may vary from 0 (bad) to around 1 (good), to a little greater than 1 (which, depending upon the facility 10 design, can be either good or bad), to much greater than 1 (typically bad). This ratio information may be provided to the facility operator via an audio signal and/or a visual signal through the monitor 140 . The ratio information may also result in the automatic shut down of a dispensing point 210 , or a recommendation for dispensing point shut down.
[0048] The embodiments of the invention shown in FIGS. 1 and 2 may provide a significant improvement over known systems due to the replacement of the multiple AFS's 500 (one per dispensing point, typically anywhere from 10 or 12 up to 30 or more per site) and their associated wiring with a single, or fewer AFS's 500 (about ½ as many or less, depending upon dispensing point groupings).
[0049] With reference to the embodiments of the invention shown in both FIGS. 1 and 2 , the mathematical analysis performed in the monitor 140 is designed to find correlations between aggregate vapor volume measured during AFS 500 ‘busy periods’ and individual dispensing point 210 dispensed liquid fuel volume readings. The analysis is done separately for each AFS 500 and it's associated dispensing point group (two or more dispensing point's). The end result is a set of estimated dispensing point A/L ratios, one ratio per dispensing point. After a group of AFS 500 busy period data records are accumulated, a series of mathematical steps accomplish this beginning with a simple, 1-variable function solution and ending with more complex function solutions until all ratios are determined. If a ratio can be determined in an earlier step, it is not necessary to estimate it in a subsequent step (it can be set as a constant in later steps to simplify computation of any remaining unknown ratios). The sequence of solvable function types are:
[0050] Type 1: A single linear function with one unknown for any AFS busy records with only 1 active dispensing point.
[0051] Type 2: Two linear functions with two unknowns for any pair of similar AFS busy records with 2 (identical) active dispensing point's (two simultaneous equations with two unknowns).
[0052] Type 3: Three or more linear functions each with two or more unknowns for any remaining (unsolved) set of AFS busy records (at least as many functions as unknowns).
[0053] Each AFS 500 busy period data record is formed after the AFS becomes idle by recording the aggregate vapor volume, A, and the individual metered liquid volumes, L m , where the subscript, m, denotes the dispensing point or meter number. This number ranges from 1 to M total meters. Idle detection can be done by various means, including:
[0054] 1) the monitor 140 can track reported dispenser meter 240 start/stop events from the dispenser controller 120 , the dispenser current loop wiring 130 , or directly from the liquid fuel dispensing meter 240 ; or
[0055] 2) the Automatic Tank Gauging System 360 can provide main fuel storage tank 310 liquid fuel levels to the monitor 140 for detection of static level conditions (no ongoing dispensing) in all the storage tanks 310 .
[0056] The latter method (No. 2) can be used if it is desired that all AFS's 500 be idle prior to forming AFS busy data records. In the case of a single AFS 500 per facility 10 (shown in FIG. 1 ), this method can always be used.
[0057] The simple form of the relationship between A, L, and the A/L ratio, R, for an AFS busy record with one (1) active dispensing point is:
[0000]
A=L
m
R
m
[0058] so the simple solution for function type 1 is:
[0000]
R
m
=A/L
m
[0000] where R m is the estimated A/L ratio for active dispensing point (meter), m.
[0059] In the more general case, each AFS busy period data record, n, has a measured aggregate vapor volume, A n , and the individual metered liquid fuel volumes, L nm , where the first subscript, n, denotes the data record number and the second subscript, m, denotes the dispensing point or meter number as before. The record number, n, ranges from 1 to N total records.
[0060] The generalized form of the relationship between A n , L nm , and R m for multiple-dispensing point records is:
[0000]
A
n
=L
n1
R
1
+L
n2
R
2
+L
n3
R
3
+ . . . L
nm
R
m
[0061] In the case of a pair of similar busy records with 2 active dispensing point's (same 2 dispensing point's in both records) the relationships are:
[0000]
A
1
=L
11
R
1
+L
12
R
2
[0000]
A
2
=L
21
R
1
+L
22
R
2
[0062] so the solutions for functions of type 2 are:
[0000] R 1 =( A 1 L 22 −A 2 L 12 )/( L 11 L 22 −L 12 L 21 )
[0000] R 2 =( A 2 L 11 −A 1 L 21 )/( L 11 L 22 −L 12 L 21 )
[0063] Functions of type 3 can be solved as a least squares problem using standard matrix arithmetic.
[0064] Example record data set with subscript notation:
[0000]
n
A n
L n1
L n2
L n3
etc . . .
L nM
1
18
0
12
6
etc . . .
0
2
33
10
15
0
etc . . .
8
3
21
7
0
0
etc . . .
14
etc . . .
N
18
0
0
18
etc . . .
0
[0065] For the entire data set, the matrix relationship is:
[0000]
[
A
1
A
2
A
3
⋮
A
n
]
=
[
L
11
L
12
⋯
L
1
m
L
21
L
22
⋯
L
2
m
L
31
L
32
⋯
L
3
m
⋮
⋮
⋮
⋮
L
n
1
L
n
2
⋯
L
n
m
]
[
R
1
R
2
⋮
R
m
]
or
A
=
LR
[0066] The solution for the ratio vector, R, is:
[0000] R =( L T L ) −1 L T A
[0000] where the first term is the inverse of the transposed n×m matrix, L, times itself which results in an m×m matrix, the middle term is the transposed matrix, L, which is an m×n matrix, and the last term is the vector A of length n, all of which results in the vector R, of length m (one A/L ratio per meter).
[0067] This approach can provide good estimates of the true A/L ratios, even with excessive variability (noise) in the sensor readings. More records result in better estimates for a given level of variability but there must be at least as many records as unknowns for minimal performance.
[0068] Dispensing point ratio solutions are based on the simplest function type possible. As a data set is processed and ratio solutions are determined, they are in turn used to simplify solutions for remaining records in any record set. As an example, if two records exist in a set, one of type 1 (a single active dispensing point busy period), and a second with two active dispensing points, one of which is the same dispensing point as in the first record, the first record is solved directly as a type 1 function and it's ratio result is used to simplify the function for the second record. This produces a second type 1 function.
[0069] Example Records (2):
[0000]
n
A n
L n1
L n2
1
5
—
10
2
19.5
12
15
[0070] Initial Functions:
[0000] A 1 =L 12 R 2 5=10 R 2
[0000] A 2 =L 21 R 1 +L 22 R 2 19.5=12 R 1 +15 R 2
[0071] Solve first, substitute solution in second to simplify:
[0000] 5=10 R 2 R 2 =5/10=0.5
[0000] 19.5=12 R 1 +15 R 2 19.5+12 R 1 +15*0.5=12 R 1 +7.5
[0072] Solve second as a type 1 function:
[0000] 19.5=12 R 1 +7.5 12=12 R 1 R 1 =12/12=1.0
[0073] This simplification method is used at each step of the data set solution process:
[0074] Step 1: Form simple (1-dispensing point) or generalized function forms for each record.
[0075] Step 2: Solve all Type 1 functions.
[0076] Step 3: Substitute solutions from prior step into remaining set of functions.
[0077] Step 4: Reduce all functions to simpler forms and repeat from step 2.
[0078] Step 5: Find and solve any Type 2 function pairs.
[0079] Step 6: Substitute solutions from prior step into remaining set of functions.
[0080] Step 7: Reduce all functions to simpler forms and repeat from step 2.
[0081] Step 8: If possible, solve remaining functions as a Type 3 least squares problem.
[0082] Step 9: If step 8 is not possible, wait for more data records to solve the remaining functions.
[0083] Alternatively, replace the 9-step sequence with steps 8 and 9 alone. This approach has the benefit of always averaging or reducing the effects of variability in the sensor readings.
[0084] The various embodiments of the invention discussed herein may also be used to detect vapor recovery equipment failures. Stage-II vapor recovery equipment failures can have two distinct effects on patterns of A/L ratios. The failures are determined by identifying these patterns in the solved ratio set. The first type of failure involves a dispensing point nozzle 210 , a hose 212 , or vapor return passage 220 path restriction, or a vacuum assist pump failure which blocks or reduces air-vapor flow. The above solution methods may be used to identify this type of failure by identification of one dispensing point with a consistently lowered ratio.
[0085] The second type of failure that can occur involves a dispensing point 210 with a defective air valve which does not close properly to block reverse vapor flow (i.e. out of the nozzle) when the dispensing point is idle. In such a case the ratio for the defective dispensing point will not be affected because when the dispensing point is active, the vapor flow is normal. However, when idle, vapors from other active dispensing points can be pushed past the defective air valve, out of the leaky dispensing point nozzle, and into the atmosphere. The active dispensing point(s) AFS 500 may or may not register the amount of lost vapor, depending upon whether the leaking dispensing point is part of the AFS group (won't register) or not (will register). If not, the idle AFS 500 will register reverse vapor flow. In that case, the leaking dispensing point can be detected by the reverse flow signal when it should be idle.
[0086] Using the above solution methods described in connection with the first and second embodiments of the invention, when the leaking dispensing point is a member of the active AFS 500 group it results in lowered ratios for all dispensing points in the group except for the leaking dispensing point. Also, the lowered ratios vary depending upon the number of active dispensing point's during each busy period. When more (good) dispensing point's are active in an AFS 500 group, the lost vapor effect is shared in the solution, resulting in less depression of the individual ratios. Furthermore, if only part of the vapors escape to the atmosphere, the effect is reduced, resulting in less depression of the individual ratios. Accordingly, a post-solution analysis may be conducted on the ratio patterns to determine the likely failure type, active dispensing point restriction or idle dispensing point leak.
[0087] A third embodiment of the invention concerns the use of a single vapor pressure sensor 350 (same as CARB requirement) to actively determine the tightness of the overall vapor containing elements of the facility including the fuel storage system 300 , (which includes the vent pipe 320 , pressure relief valve 330 , etc.), the vapor return pipelines 410 , the vapor/liquid splitter 260 , the vapor return passages 220 , the dispenser hose 212 , the nozzle 210 , etc. The vapor pressure sensor 350 may be connected anywhere in the fuel storage system 300 or the pipeline system 400 , which includes but is not limited to the storage tank 310 vapor-space, the common vapor return pipeline 410 , or the storage tank vent pipe 320 . The vapor pressure sensor 350 may be used periodically to actively measure the leakage of vapors from the overall system instead of constantly measuring for leakage amount.
[0088] The method in accordance with the third embodiment of the invention may be carried out as follows. The monitor 140 may be connected to and access pressure readings from the vapor pressure sensor 350 . The monitor 140 controls the active test which is initiated by determining an idle period during which none of the dispensing units 200 are in operation (similar to the A/L detection method using either dispensing meter events or ATGS tank levels). The idle condition may be continuously monitored and the test aborted if any dispensing units go into operation during the test. During the idle period the vapor pressure sensor 350 is used to determine the pressure in the system (i.e. the pressure in the storage tank 310 ). If the pressure is not adequately negative (vacuum) for the test, the vapor processor 340 may be turned on to draw a negative pressure in the storage tank 310 as it processes vapors. If the vapor processor 340 is used, the monitor 140 may be used to monitor the vapor pressure readings until they become adequately negative, typically −2 or −3 inches w.c. Once the vapor pressure is adequately negative, the vapor processor 340 may be turned off. Thereafter the vapor pressure sensor 350 readings may be monitored during the remaining idle time. If the system is adequately tight, the negative pressure readings should hold or degrade only slowly. If the negative pressure degrades too rapidly toward zero, the monitor 140 may indicate that the system has failed the leakage test. A pass/fail threshold is used to make this determination. It can be set as a percentage of the initial negative pressure amount based on the desired detection sensitivity and should be related to the amount of air inflow detected relative to total storage tank 310 vapor space (ullage volume).
[0089] In an alternative of the third embodiment of the invention, a single or multiple AFS's 500 located in the common or multiple vapor return pipeline(s) (same as A/L detection equipment) may be included to conduct an improved active test for system tightness. While a pressure sensor 350 alone suffices for conducting a tightness test, AFS 500 readings can add to the amount of information available to augment test sensitivity and confirm the tightness condition or help locate the source of a leak. Any air inflow from a leak point will register as flow on the AFS(s) 500 . Flow and flow direction are a general indicator of the location of the source of incoming air (which dispensers and/or tanks/vents). Note that the AFS 500 readings are generally the more sensitive indicator of vapor recovery system tightness failure since negative pressure degradation is small due to the small amount of air inflow over seconds or minutes of time relative to the generally large storage tank vapor-space volumes. For significant negative pressure degradation, the amount of air inflow needs to be a significant portion of the storage tank vapor-space volume which can be in the thousands or tens of thousands of gallons.
[0090] The optional AFS(s) 500 , and dispenser controller 120 , dispenser current loop 130 , or optional ATGS 360 are connected to the monitor 140 which acquires and processes the data from the devices to conduct the tightness test and also controls (on/off) the vapor processor 340 . Note that only one vapor pressure sensor 350 is needed for multiple storage tanks 310 as long as they share a common vapor recovery system so that their vapor spaces are connected (piped) together.
[0091] In another alternative embodiment of the invention, the ATGS 360 may not be required to conduct an active test for system tightness. In this case, the idle state of the vapor recovery system during which the tightness test is conducted must be determined by (lack of) fueling meter 240 activity and a precise estimation of leak rate is not possible since tank 310 vapor ullage space volume is not known. Instead, a general pass/fail indication can be provided when the pressure decays at a preset rate during a test period.
[0092] In yet another embodiment of the present invention, the systems shown in FIGS. 1 and 2 may be used to conduct an improved passive vapor containment test. This test uses pressure in the vapor containing elements of the facility, barometric pressure, and ullage space measurements to calculate the change in pressure over time for the vapor containing elements of the facility. This calculation, which is not usually based on data collected when the facility is operating at −2 to −3 inches w.c., may then be normalized to indicate leakage rates for a facility held at −2 to −3 inches w.c.
[0093] This passive method may be initiated by monitoring the pressure of the main fuel storage system 300 or any vapor containing element of the facility 10 between fuel dispensing periods with the pressure sensor 350 . Pressure data derived from sequential groupings of monitored pressures and ullage determinations derived from the ATGS 360 readings are recorded at periodic intervals by monitor 140 . The derived recorded data permits the determination of rate of change of pressure, p rate , versus time, t, obtained from a linear regression model:
[0000]
p=p
rate
·t
[0000] within each interval, the main storage system 300 total ullage volume, V ullage represented by the sum of the individual storage tank 310 ullage volumes, V ullage :
[0000] V ullage =v ullage1 +v ullage2 + . . . +v ullageN for tanks 1 to N
[0000] where
[0000] v ullage =(tank capacity)−(volume of fuel in tank)
[0000] obtained from the ATGS 360 , and the average pressure, p avg over each interval:
[0000] p avg =( p 1 +p 2 + . . . +p N )/ N for pressure samples 1 to N in the interval
[0000] are recorded if the correlation to the linear model is acceptable, generally based on high correlation between pressure with respect to time and the model.
[0094] Upon collection of a daily sample of such records, the product of pressure rate and the total ullage volume, p rate ·V ullage , is sorted by the associated average pressure, p avg , and grouped into equally spaced average pressure ranges. A collection of averages of the products, (p rate V ullage ) avg , within each group:
[0000] ( p rate V ullage )avg=(( p rate ·V ullage ) 1 +( p rate ·V ullage ) 2 + . . . +( p rate ·V ullage ) N )/ N
[0000] for products 1 to N in each group. The midpoints of the average pressure ranges, p mid , within each group are used with a linear regression model to estimate the rate of change of pressure times ullage volume, P rate V at a selected test pressure, p test , of, say, 2 inches of water column, if the correlation to the linear model:
[0000] P rate V =( P rate V ) slope ·p test
[0000] is acceptable generally based on high correlation between the average products, (p rate V ullage ) avg , with respect to midpoint pressures, p mid , and the model. A typical graph of this model for a tank system is shown in FIG. 3 . It is noted that the curve must cross the origin which indicates no rate of change of pressure, thus no leakage, when there is zero pressure drop across any leakage path, since for leakage to occur a pressure driving force is needed regardless of ullage volume.
[0095] The regression yields the slope coefficient, (P rate V) slope , which is used to calculate the estimated pressure times ullage volume, P rate V at a selected test pressure, p test , of, say, 2 inches of water column at which a leakage test failure rate can be defined, similar to the standard CARB TP-201.3 test procedure. In other words, if there is a leakage path and if the pressure in the ullage space of the tank system is set to 2″ wcg (water column gauge) (above ambient pressure), the tank will leak at the estimated rate, v rate , of:
[0000] v rate =P rate V ( p test )/ p
[0000] where p is the absolute pressure in the tank ullage space, typically 410″ wca (water column absolute) (assuming ambient is 408″ wca). This can be interpreted to mean that the rate of volume vapor loss from a leaking tank is equal to the proportional rate of change of absolute pressure times the total ullage volume. Note that p test is a gauge pressure (referenced to ambient) and p is an absolute pressure (referenced to a vacuum). This relationship is derived from the ideal gas law, which governs the relationship between pressure, p, and volume, v, in an enclosed space at low pressures and temperatures:
[0000]
p·v=n·R·T
[0096] where n is moles of gas, R is the universal gas constant, and T is absolute temperature. Replacing n with mass per molecular weight (MW):
[0000] p·v=m·R·T /MW
[0000] Rearranging terms and replacing constant terms with k:
[0000] m=k·p where k=v ·MW/( R·T )
[0000] Rate of mass loss due to a leak from an enclosed space is found by forming the relationship of the difference between the ending and starting mass divided by starting mass and the time period of the loss:
[0000] ( m 2− m 1)/ m 1· t =( k·p 2− k·p 1)/ k·p 1· t
[0000] Δ m /( m 1· t )=( p 2− p 1)/ p 1· t
[0000] Δ m /( m 1· t )=Δ p/p 1· t
[0000] Δ m/t=Δp·m 1/ p 1· t
[0000] The last form describes the rate of mass loss as a function of starting mass times proportional pressure change rate over the test period. To find volume loss rate, relate mass and volume by mass density, p:
[0000] ρ= m/v or m=ρ·v so m 1= p 1· v and mass loss: Δm=ρ·Δv
[0000] Substituting in above equation:
[0000] ρ·Δ v/t=Δp·ρp 1· v/p 1· t
[0000] Assuming mass density does not change appreciably:
[0000] Δ v/t=Δp·v/p 1· t where ρ1≈ρ
[0000] Dropping the subscript and using notation for volume loss rate, v rate :
[0000]
v
rate
=Δp·v/p·t
[0000] which can be interpreted to mean that the volume loss rate is the proportional change of pressure times volume per unit time. But part of this expression is the calculated value derived from measurements in the above section:
[0000] v rate =P rate V/p where v rate =Δp·v/t at the selected test pressure, 2″ wcg
[0097] Using the above example, the volume leak rate, v rate , is:
[0000] v rate =P rate V/p= 6000/410=14.6 CFH or cubic feet per hour at 2″ wcg
[0098] As described above, in yet another embodiment of the invention, the system may also perform a method of distinguishing between true vapor recovery failure events and ORVR equipped vehicle refueling events. Identifying a false vapor recovery system failure due to refueling an ORVR-equipped vehicle may be accomplished by applying standard statistical concepts to a group of dispensing or refueling events from all the dispensing points 210 at a dispensing facility 10 to identify true failed vapor collection dispensing points as opposed to failed tests due to ORVR vapor-blocking activity.
[0099] There are two assumptions that may be made as a predicate to determining true failed vapor collection: (1) that ORVR and non-ORVR activity occurs somewhat randomly amongst all the dispensing points; and (2) that average ORVR activity does not reach 100% of all refueling events (a maximum of 80% can be assumed). Given these assumptions, a group of vapor collection event A/L measurements taken from all the dispensing points 210 at a dispensing facility 10 may be used to make the following determinations:
[0100] 1) Determine if the proportions of failed (close to zero A/L) and non-failed events are statistically different at individual dispensing points relative to their expected proportions, due to the activity of ORVR vehicles, derived from all the dispensing points; and
[0101] 2) Determine if the proportion of the failed (close to zero) events at each dispensing point are statistically different from the proportion of the failed events derived from all the dispensing points, which are largely due to the effect of ORVR vehicles.
[0102] As a result of these determinations, the A/L ratio measurements may be used to test for blockage or leakage caused vapor recovery failure, with a mix of ORVR and non-ORVR vehicle activity.
[0103] On a regular (e.g. daily) basis, each dispensing point 210 may have a number of A/L determinations associated with it. It is presumed that there are k dispensing points 210 and the i th dispensing point has n i A/L ratio determinations. Let X i be the number of A/L determinations for dispensing point I that indicate a “zero” or “blocked” A/L ratio. The assumption is that fueling an ORVR vehicle will result in a zero or blocked A/L ratio. The total number of A/L determinations for the site is:
[0000]
n=Σn
i
[0000] and the total number of zero A/L ratios is:
[0000]
X=ΣX
i
[0104] An overall test can be conducted to determine whether there are any significant differences in the proportion of A/L ratios indicating blocked vapor flow among the dispensing points 210 . This can be accomplished using a chi-squared test on the table of data from the k dispensers:
[0000] Dispenser 1 Dispenser 2 Dispenser k Total Number X1 X2 . . . Xk X blocked Not blocked n1 − X1 n2 − X2 . . . nk − Xk N − X Number n1 n2 . . . nk N
The chi-squared statistic is given
[0000] by: X 2 =Σ( O i E i ) 2 /E i
[0000] where O i is the number observed in each cell of the table and E i is the expected number in that cell. The data in the cells indicate the number of A/L ratios that indicate a “blocked” condition for each dispensing point and the number of A/L ratios indicating a “not blocked” condition for that dispenser. The expected number “blocked” ratios for dispenser I is:
[0000] E i1 =n i ( X/N )
[0000] and the expected number of “not blocked” ratios for dispenser I is:
[0000]
n
i
−E
i
[0105] The summation is carried out over 2 k cells. This statistic is compared to the critical value from a chi-squared table with k−1 degrees of freedom. If it is significant, there is evidence that the dispensers have different proportions of blocked A/L ratios, so that one or more would appear to be blocked on at least an intermittent basis.
[0106] In turn, an individual test can be performed for each dispenser. This tests whether each dispenser has a proportion of zero A/L ratios that exceeds the overall proportion for the station. The following equation may be used to compute the overall proportion of zero A/L ratios for the period:
[0000]
P=X/N
[0000] The following equation may be used to compute the proportion of zero A/L ratios for each dispenser:
[0000]
p
i
=x
i
/n
i
[0000] From the foregoing calculations, it may be concluded that there is evidence that dispenser I is blocked if:
[0000] p i >P+z α (0.16/ n i ) 1/2
[0000] where z α is the upper α percentage point from a standard normal distribution. If a 1% significance level is desired, z α is 2.326, for example, (or 1.645 for a 5% significance level). The number 0.16 in the formula results from assumption of the most conservative case; that 80% of the vehicles are ORVR vehicles. Once a truly blocked dispensing point is detected, an audio or visual signal may be provided by the monitor 140 to indicate this condition. Truly blocked dispensing points may also be automatically shut down as a result of such detection.
[0107] It will be apparent to those skilled in the art that various modifications and variations may be made in the preparation and configuration of the present invention without departing from the scope and spirit of the present invention. For example, various combinations of the methods described above may be implemented without implementing the full system shown FIGS. 1 and/or 2 . Thus, it is intended that the present invention cover the modifications and variations of the invention.
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A method and apparatus for monitoring and determining fuel vapor recovery performance is disclosed. The dispensing of liquid fuel into a tank by a conventional gas pump nozzle naturally displaces a mixture of air and fuel ullage vapor in the tank. These displaced vapors may be recovered at the dispensing point nozzle by a vapor recovery system. A properly functioning vapor recovery system recovers approximately one unit volume of vapor for every unit volume of dispensed liquid fuel. The ratio of recovered vapor to dispensed fuel is termed the A/L ratio, which should ideally be approximately equal to one (1). The A/L ratio, and thus the proper functioning of the vapor recovery system, may be determined by measuring liquid fuel flow and return vapor flow (using a vapor flow sensor) on a nozzle-by-nozzle basis. The disclosed methods and apparatus provide for the determination of A/L ratios for individual nozzles using a reduced number of vapor flow sensors. The disclosed methods and apparatus also provide for the determination of fuel dispensing system vapor containment integrity, and the differentiation of true vapor recovery failures as opposed to false failures resulting from the refueling of vehicles provided with onboard vapor recovery systems.
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BACKGROUND OF THE INVENTION
The invention relates to improvements in sonde housings used in horizontal direction drilling to carry a radio transmitter that indicates the location and orientation of a drill head.
Horizontal direction drilling in geological formations is widely used to place product such as pipe, conduit or cable underground. Typically, the location and orientation of the drill head is monitored as it progresses through the earth so that corrections can be made to keep the actual path as close as possible to the desired path. The location and orientation of the drill head is signaled to the surface by a radio transmitter carried in a so-called sonde housing that is interposed in the drill string just behind the drill head. The sonde housing includes passages for fluid that is used in the drilling process and that advantageously cools the sonde housing so that heat from the drilling operation does not overheat the electronics of the transmitter.
Conventional prior art sonde housings have been fabricated by machining steel bars or tubes to provide a chamber for the transmitter and axial passages for the fluid. That fluid creates a jet at the drill face or provides hydraulic power for a directional drill motor and, as mentioned, cools the transmitter. Typically, the prior art sonde housings are relatively expensive because of the special machining operations that are performed to create the chamber and various passages through the full length of the housing. This cost is significant to a drilling company because the typical sonde housing has a limited life. The fluid that passes through the sonde housing is continuously recycled. Although it is filtered, fine sand particles remain in the fluid causing it to be highly abrasive. The fluid, because of its abrasiveness, wears away at the passages in the housing eventually destroying it. Another problem frequently encountered with known types of sonde housings is related to slots or other apertures formed in the housing wall that allow transmission of radio waves out of the metal housing. The slots are frequently filled with epoxy or other non-metallic material to exclude fluid from the chamber in which the transmitter is received. This material is prone to leak internally after a period of use with the result that the transmitter and its associated battery can become cemented in the chamber by fluid borne solids making it very difficult to remove the transmitter without harm.
SUMMARY OF THE INVENTION
The invention provides an improved sonde housing that can be economically manufactured and that has improved performance both in resistance to wear and resistance to internal leakage. Various internal parts, while being made of relatively inexpensive materials, are capable of an extended service life meeting or exceeding that of more expensive traditional materials. Still further, internal parts that are susceptible to wear by abrasion from the fluid being conducted through the housing are replaceable at relatively low cost. As disclosed, the sonde housing comprises an outer metal cylindrical shell or main body having tool joints at each end. The shell wall is slotted at circumferentially spaced locations for transmission of radio signals from the transmitter carried within the shell body. A cartridge assembly is positioned in the shell body to provide a sealed chamber for the transmitter, an annulus for conducting fluid through the housing and a sleeve to seal the radio transmission slots in the shell wall and to protect the shell wall from abrasion from the circulating fluid. The main parts of the cartridge are formed of a suitable plastic so that they are extremely cost effective and, advantageously, are inherently transparent to the radio wave signals generated by the transmitter.
In the disclosed arrangement of the housing, the sleeve of the cartridge not only protects the shell body from abrasion, but also by sealing the radio signal emitting apertures in the shell wall, avoids the seal failure problems normally encountered in the prior art where the apertures are sealed with epoxy.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A and 1B are left and right-hand portions of a sonde housing, constructed in accordance with the invention taken in a longitudinal cross-sectional view;
FIG. 2 is a cross-sectional view of the sonde housing taken in a plane transverse to the longitudinal axis of the housing as indicated by the arrows 2 — 2 in FIG. 1A; and
FIG. 3 is a transverse cross-sectional view of a main shell body of the housing taken in the plane indicated at 3 — 3 in FIG. 1 A.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings, there is shown a sonde housing assembly 10 . FIGS. 1A and 1B are complimentary to one another; the housing assembly 10 is illustrated in two parts so that a larger drawing scale is obtained but it will be understood that the actual housing assembly is a single integrated assembly. The housing assembly 10 comprises a main shell body 11 having end pieces or tool joints 12 , 13 at each end. The shell body 11 is preferably formed as a length of suitable round steel tubing which may be a high alloy hardened steel material for improved strength. The end pieces 12 , 13 are also fabricated of a suitable steel and are in the form of hollow heavy wall sleeves having through bores 16 , 17 . In the illustrated case, the end piece or tool joint 12 on the right has an internal thread form designated by the American Petroleum Institute as an API IF thread which is commonly used in drill pipe. The end piece or tool joint 13 at the left is an internal thread designated by the American Petroleum Institute as an API REG thread which is used to couple with the drill head of horizontal directional drilling apparatus known in the art.
An extension 21 on an inward end of each of the end pieces 12 , 13 is telescoped into a bore 22 of the shell body 11 to facilitate alignment and assembly of these parts. Axially and radially outward of the extension 21 , each end piece 12 , 13 is chamfered to permit a circumferentially continuous fluid-tight weld bead 23 to be formed between the end piece and the shell body 11 to thereby join these parts together. The shell body 11 has a plurality of apertures in the form of axially extending slots 26 cut through its wall 27 to permit external transmission of radio waves from a transmitter carried in the housing assembly 10 as discussed below.
Positioned in the shell body 11 before one or both of the end pieces 12 , 13 are welded on is a cartridge assembly 31 . The cartridge assembly 31 includes an outer sleeve 32 and an inner tube 33 within the sleeve. The sleeve 32 and tube 33 are held in concentric relation by a pair of annular adapters 34 and a ring 36 . Preferably, the adapters 34 are identical units having the general form of a short tube or ring with an internal cylindrical surface or bore 37 and a cylindrical outer surface 38 . As shown in FIG. 2, a wall 39 of the adapter 34 is drilled or otherwise formed with a plurality of axial bores or passages 41 angularly spaced about its circumference. At an inner end, the adapter 34 has a counter bore 42 for receiving a short portion of the length of the inner tube 33 . Similarly, the inner end of each adapter 34 has a reduced diameter outer surface 43 that fits into the inside diameter of the sleeve 32 . When the ends of the sleeve 32 and the tube 33 are respectively assembled in and on the adapter 34 , these parts are held concentric with one another. The ring 36 is similar in cross-section to the adapters 34 , but shorter in length, and is disposed around the tube 33 and in the sleeve 32 . The ring 36 is adhesively attached or otherwise fixed at the mid-lengths of the tube 33 and sleeve 32 . The ring 36 includes circumferentially spaced axial passages 46 to permit fluid passage through an annulus 35 between the tube 33 and sleeve 32 . In the illustrated example, the tube 33 and sleeve 32 are made of rigid polyvinylchloride such as the type conventionally used for plastic pipe. The surfaces of contact between the adapters 34 and ring 36 with the tube 33 and with the sleeve 32 are joined together with a suitable adhesive. Outer ends of the tubular adapters 34 have internal threads 47 . A retainer 51 at one end of the cartridge assembly 31 (FIG. 1A) has external threads complimentary to the adapter threads 47 . The retainer 51 has an outer portion 53 with a hexagonal or other acircular cross-section in end view enabling it to be tightened or untightened in the adapter threads 47 . A radial shoulder 54 of the retainer 51 is proportioned to abut an end face 56 of the adapter 34 when the retainer is fully threaded into the adapter. The contact between the shoulder 54 and end face 56 prevents the retainer 51 from being over-tightened. The retainer 51 has a central axial bore 57 in which is received an indexer 58 . The indexer 58 has a cylindrical central portion 59 sized to rotate in the retainer bore 57 . The indexer 58 is captured on the retainer 51 with a metal snap ring 61 at one end and a radially extending flange 62 at the other end. An elastomeric O-ring 63 disposed in a peripheral groove on the central cylindrical portion 59 of the retainer seals with the bore 57 . An elastomeric O-ring 64 located in a groove in the flange 62 seals against a radial inner face of the retainer 51 . At an outer end 66 , the indexer 58 has a hexagonal profile, in end view, to permit the indexer to be selectively rotated with a wrench. On an inner radial face, the indexer 58 has an integral key 69 that enables it to be rotationally interlocked with a radio transmitter 67 disposed in a chamber 68 circumferentially bounded by the inner surface of the tube 33 . The transmitter 67 is manually rotated or “clocked” in the chamber 68 , as is known in the art, by rotating the indexer 58 .
On an opposite end of the cartridge 31 (FIG. 1 B), a plug 71 with male threads complimentary to the adapter threads 47 is removably threaded into the adapter 34 . The plug 71 has a peripheral groove that receives an elastomeric O-ring 73 which seals with the adapter counterbore 42 . An outward portion 74 of the plug 71 has a hexagonal shape when viewed axially to permit the plug to be tightened or untightened into the threads 47 of the adapter. A radial shoulder 76 on the plug 71 abuts the end face 56 of the adapter 34 to prevent the plug from being inadvertently over-tightened.
The transmitter 67 and a battery 78 , both known in the art, can be disposed in the chamber 68 . A compression spring 79 holds the transmitter 67 and battery 78 in place with the transmitter coupled with the key 69 on the indexer 58 . The transmitter 67 and battery 98 can be assembled and removed from the chamber 68 through the end piece 12 by installing or removing the plug 71 with a wrench.
The cartridge assembly 31 comprising the outer sleeve 32 , inner tube 33 , adapters 34 , retainer 51 and plug 71 is inserted in the shell body 11 before at least a last one of the two end pieces 12 or 13 is welded or otherwise joined to the shell body. The cartridge assembly 31 is fixed relative to the shell body 11 by tightly fitting spring pins 81 extending through holes drilled through the shell wall 27 and into the walls of the adapters 34 . The outer periphery of the adapters 34 is machined or otherwise formed with a pair of spaced circumferential grooves in which are received elastomeric O-rings 82 . The O-rings 82 provide a fluidtight seal between the cartridge assembly 31 and interior surface of the bore 22 of the shell body 11 .
In use, fluid typically primarily recycled water is received by the end piece 12 (FIG. 1B) from a drill pipe string to which the end piece or tool joint is coupled by threading it onto the same. The fluid diverges over the plug 71 and passes through the several peripheral openings or passages 41 in the associated adapter 34 . This fluid then passes through the annulus 35 between the inner tube 33 and outer sleeve 32 , the passages 46 in the ring 36 and through the openings or bores 41 in the other adapter 34 and ultimately passing out of the end piece 13 . It will be understood that substantially the full circumference of the tube 33 and, therefore, the transmitter 67 is surrounded by this fluid so that full cooling of the transmitter is obtained.
The fluid pumped through the sonde housing assembly 10 , despite filtering, can become abrasive by picking up fine sand or other particulate material from the geological formation through which it is recycled. In this circumstance, the surfaces of the cartridge assembly 31 can become worn away with extended use even though it has been found that plastic material such as polyvinylchloride is remarkably durable when compared with the typical steels used in similar applications. The cartridge assembly 31 can be replaced by cutting off one of the end pieces 12 or 13 from the shell body 11 at the weld bead 23 , removing the worn cartridge assembly and replacing it with a new one. Thereafter, the end piece can be rewelded onto the shell. It will be understood that the inner tube 33 and outer sleeve 32 , being formed of a non-metallic material such as polyvinylchloride or other material of suitable structural strength and transparent to radio waves, eliminate the need for separately sealing the apertures or slots 26 in the wall 27 of the shell body 11 .
It should be evident that this disclosure is by way of example and that various changes may be made by adding, modifying or eliminating details without departing from the fair scope of the teaching contained in this disclosure. The invention is therefore not limited to particular details of this disclosure except to the extent that the following claims are necessarily so limited.
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A sonde housing construction that is cost effective to manufacture, has a prolonged service life and has an internal cartridge that has replaceable parts and that can be entirely replaced. The cartridge which in service contains and protects a radio transmitter also serves to protect a main shell body from abrasion by drilling/cooling fluid while sealing radio wave apertures formed in the shell body. The cartridge creates an annular flow path for drilling/cooling fluid that ensures complete cooling protection of the transmitter.
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THE PRIOR ART
In the case of face-to-face plain velvet and carpet weaving machines the pile height between top and bottom fabric is determined by the balance arising between the ground warp tension and the pile warp tension. The pile warp is fed into the weaving system by a pile feeder mechanism, and the pile warp is kept at tension with tension springs by means of a swing roller. The pile feeder consists of a set of rollers, the centre roller of which is driven by a pile regulator. The pile warp supply can be set by changing two change wheels in the pile regulator. Such a pile regulator produces a constant pile warp feed.
When a particular design pattern in plain velvet requires little or no pile warp feed, the drive of the pile feeder is interrupted by an electromagnetically controlled gear coupling.
The data for whether or not to control is stored for each shot in the data carrier for the weaving frame motion of the heald loom.
In the weaving machines belonging to the known prior art the use of a computer is limited purely to monitoring the thread supply, and never concerns the control thereof.
Document EP-A-0224464 discloses a method for monitoring thread supply shot by shot during the weaving of pile fabrics, by means of a jacquard weaving loom. The length of a pile thread to be woven is entered in a processor as the reference value. The recorded conveyed thread length is compared with the reference value. During the comparison made, data is supplied as a function of a signal indicating whether the thread must form pile or otherwise.
An alarm signal is emitted if pile thread is not being woven in, or if the thread length being conveyed is outside the set tolerances.
During weaving frame pattern definition for face-to-face plain velvet and carpet, many articles are developed with two or three pile warp systems.
Each of these pile warp systems has its own pile warp beam with pile warp let-off motion, pile feeder roller and gear coupling, but no pile regulator of its own. There is only one common pile regulator for one or more pile warp beams.
Said pile regulator has a set of change wheels for each individual pile warp supply, with a gear coupling for temporary interruption and/or switching on/off of said pile warp supply. In the case of double-gripper weaving machines which rotate more slowly (240 r.p.m.) these devices have worked faultlessly and met the strict quality standards in the field of pile height regularity and stripe formation. In the case of the current highspeed double-gripper weaving machines for plain velvet (320-340 r.p.m.) these devices are no longer adequate for weaving certain velvet articles with several pile warp systems and short-pile single systems. At a stopping/starting point a line mark becomes apparent in the weft direction in the pile surface. This is also the case where two-pile warp systems change in order to form working pile. This line mark is caused by a difference in pile height. It should not be confused with the starting stripe, which is due more to a local change in weft density as the result of a "weaker" starting beat-up of the weaving reed.
This phenomenon indicates that the pile warp beam has not reached speed fast enough; during full weaving speed said pile warp beam has to start from a stationary position and ensure the full pile supply for a few shots, before coming to rest again in the case of pile warp systems with intermittent and/or changing pile warp use. The electromagnetic gear couplings have an electrical and mechanical inertia, with the result that at high speed it is impossible here to switch on and off with sufficient accuracy and for each shot. The pile regulator--pile feeder drive unit is a gear train which ultimately shows considerable play at the periphery of the pile feeder roller: the counter-pile warp tension, caused by the pile beam warp let-off motion reacting too slowly, also has an effect here.
For these reasons, it is purely a matter of trial and error in article development to try and establish precisely at which shot the old pile warp system must be switched off and at which shot the new system must already be switched on. The development time or perfecting of an article with several pile warp systems is therefore very complicated and time-consuming. Besides, for some articles a good result is not obtained in the case of double-gripper weaving machines or at high weaving speeds (320-340 r.p.m.).
In the case of other plain velvet fabrics with a pile warp system, e.g. chiffon and cotton fabric for curtains and ladies' clothing, the pile height is fairly low, and the slightest irregularity in pile warp supply is apparent as a shadow band in the weft direction on the pile surface. In a first examination the following reason was found for this: eccentrically rotating pile warp beams, slightly eccentrically rotating pile feeder rollers, periodic jamming of guide rollers, eccentricities in the pile warp regulator gear train which are the cause of "hard" and "soft" running working points; in short, faults in the mechanical drive steps.
In general, it can therefore be said that, as regards dynamics, a mechanical pile feeder with standard electrically controlled pile warp beam let-off motion does not meet the weaving conditions of a high-speed face-to-face weaving machine. The pile warp is woven faster than the mechanical system--which is limited by its own inertia--can feed in starting and stopping conditions at full weaving speed.
SUMMARY OF THE INVENTION
The object of the invention is to provide an attractive and reliable solution to the problem of too slow a supply from a mechanical pile feeder, and also further greatly to shorten and simplify, and make more flexible, the article change-over time and article development time.
The present invention relates to a pile feeder control system and pile warp let-off motion for a face-to-face weaving machine intended for weaving plain velvet and carpets, comprising a pile feeder and a pile warp beamlet-off motion equipped with a computer suitable for calculating the necessary pile warp feed for each operating cycle of the weaving machine and using said calculation as a reference value.
For this purpose, there is provided a pile feeder control system and combined ground warp let-off motion in which the entire system of mechanical groups, such as pile feeder, pile regulator, gear coupling and pile beam warp let-off motion, is replaced by a computer-controlled or direct pile warp beam let-off motion which is capable of achieving a constant pile feed for plain face-to-face velvet or carpet where this is required for cut velvet and uniform pile height, interrupting the pile warp feed where necessary, in other words, providing only the pile warp feed which is required by the pile weave on each shot. In this way it becomes possible to have each of the three beams in operation with a different pile feed at the same moment. It is also possible to make the pile feed vary in stages or make a gradual increase (positive or negative) during the weaving process. The setting parameters for the pile warp feed are stored in the memory of the microprocessor control system of the weaving machine: pile height per shot, shot density and weave. The pile length produced is scanned and processed in the regulator.
The invention thus relates to a pile feeder and combined ground warp let-off motion, comprising a computer-controlled or a direct pile beam drive which performs both functions, pile feeder and pile warp beam let-off motion, combined directly by means of an intelligent control system of the pile warp let-off motion.
This is achieved by equipping a double-gripper weaving machine with a pile warp beam let-off motion which operates sufficiently accurately and is sufficiently dynamic to ensure that the pile warp is fed to the weaving system without the intervention of any mechanical pile feeder setting.
This pile warp beam let-off motion can be used on 1, 2 and up to 3 pile warp beams, and it can achieve a pile height from 2 mm to 70 mm between top and bottom fabric. The system is capable of calculating the necessary pile warp feed for each operating cycle of the weaving machine. Said pile warp feed is supplied statically and dynamically as a function of the operating cycle of the weaving machine: stop--slow running--fast running--inching operation. The final result is a better quality of fabric which is free from pile warp change stripes. The system can rapidly start and stop pile warp beams up to 1500 mm in diameter, on the one hand, in order to avoid pile height variations during starting/stopping and, on the other hand, in order to avoid pile warp change stripes.
According to the invention, the double-gripper weaving machine also makes it possible to alter the desired pile feed without mechanical changes on the machine. The change-over times of the machine when a new beam is being placed also become shorter, since the pile threads need no longer be passed through the pile feeder system. Moreover, part of the additional cost of the computer-controlled system is recovered through dispensing with the mechanical groups.
These characteristics and other characteristics and special features of the invention will emerge further from the detailed description which follows, with reference to the special drawings, which show an embodiment of the invention by way of example and not in any limited sense.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic illustration of a mechanical pile feeder with standard electrically controlled pile warp beam let-off motion according to the prior art;
FIG. 2 is a diagrammatic illustration of a pile feeder according to the invention with direct pile beam drive;
FIG. 3 is a diagrammatic illustration of a mechanical pile feeder with electrically controlled pile beam warp let-off motion according to the prior art;
FIG. 4 is a diagrammatic illustration of the combined pile feeder and pile warp beam let-off motion according to the invention;
FIG. 5 is a diagrammatic illustration of the functional groups of the combined pile feeder and pile warp beam let-off motion according to FIG. 4, coupled to a drive of a ground warp beam according to the invention; and
FIG. 6 is a side view of pile and ground warp beam arrangement of a face-to-face weaving machine.
DESCRIPTION OF EMBODIMENTS
In these figures the same reference symbols refer to the same or similar elements.
As illustrated in FIG. 1, a pile feeder 1, belonging to the prior art, consists of a set of rollers 2, which are driven by a pile regulator 9.
Until now the quantity of pile yarn 4 used per shot of the weaving machine 13 was set and regulated by means of a mechanical system (the pile regulator 9). The drive of the pile warp beam 5 is by means of a motor 6 and a reduction 6A, the speed of the motor being controlled from a speed regulator 7. Said speed regulator 7 ensures that exactly the same quantity of pile yarn is supplied from the beam 5 as is required by the pile feeder 1. The weaving machine is controlled by a control means 20 receiving setting parameters (input in the drawing), said means 20 sending signals to a speed regulator 3 and receiving signals from said speed regulator 3.
The control system used in FIG. 1 consists of an analog angle recorder 8 with an encoder 8A which passes on data to the speed regulator 3. Said speed regulator 3 sends to and receives signals from the speed regulator 7 of the motor 6.
When a particular design pattern in plain velvet requires little or no pile warp feed, the drive of the pile feeder 2 is interrupted by an electromagnetically controlled gear coupling 9' (see FIG. 3).
FIG. 2 gives a diagrammatic illustration of an embodiment of a computer-controlled pile feeder according to the invention. The whole system of mechanical elements, such as pile feeder 1, pile regulator 9, gear coupling 9' and a pile beam warp let-off motion, is replaced by a computer-controlled pile warp thread let-off motion.
A measuring wheel pulse generator 10 with encoder 10A passes on data to a synchronized control system 11.
The setting parameters (input in the figure) are stored in the memory of a microprocessor control system 12 of the weaving machine 13.
The system 11 receives signals from the pulse generator 13A of the machine, from the encoder 10A, from the microprocessor control system 12, from the motor 6 and from the regulator 7, and sends signals to the microprocessor control system 12 and to the regulator 7. Said regulator 7 receives also a feedback signal from the motor 6.
The drive of the pile warp beam 5 is controlled by the same regulator 7 as that of the already known pile warp let-off motion, but additional accessories are provided:
servo drive 6B;
servomotor 6 with resolver 6C and holding brake 6D (FIG. 4).
The drive of the ground warp beam 50 is also controlled by servo drive 60B and servomotor 60 with resolver 60C and handbrake 60D, but the tension in the ground warp is held constant by means of a measuring system consisting of a cam and a linear probe on compensation device 61 (FIG. 5).
Gears 60A (Reduction) are placed between the motor 60 and the beam 50. Advantageously, a protective system on the ground warp tension is also provided.
The control system of FIG. 5 comprises the following modules:
User interface 12 on the weaving machine, in which the desired pile feed can be entered shotwise as a function of the weave to be woven on each shot;
A regulating system 70 on the pile warp beam let-off motion. This regulating system is preferably a multi-axis control system, provided for one or more pile warp beams and preferably for one or more ground warp beams. The regulation of the ground warp beams (max. 2) can be combined in this regulator, with the result that the total cost can be reduced. Since the system must run in synchronism with the main axis of the machine, an axis 131 must be provided in order to constitute a 1/1 (synchronism) reference RS from the weaving machine 13. Since the diameter of the pile beam changes with time, an axis must also be provided per beam for measuring pile warp feed rate;
A four-quadrant servo system consisting of a servodrive with corresponding motor 6 and holding brake 6D, in order to be able to work with intermittent pile feeder operation for each operating cycle of the weaving machine 13;
A reduction gearbox 6A which has a high output. The reduction gearbox is not self-braking and must have low play;
A measuring system 10 to compensate for the varying current beam diameter;
An interface card between the weaving machine control system and the regulator of the beam position. On the one hand, said interface card contains preferbaly a parallel interface with optical division for the control and protection signals of the beam position. On the other hand, a serial interface is preferably provided, in order to be able to override the necessary parameters;
A 1/1 reference signal RS from the machine 13;
Protective system for undertension or overtension;
The regulating circuit of FIG. 5 which comprises:
a speed regulating circuit between servo drive 6B, 60B and servomotor 6, 60;
a high-speed regulating circuit between regulator 70 and motor (via the servo drive 6B) which controls the desired motor speed (measured by means of the resolver 6C on the motor 6, taking into account the reduction ratio 6A and the current beam diameter) as a function of the desired pile feed and the current speed of the machine (measured by means of the resolver on the machine); and
a low-speed regulating circuit between the regulator 70 and the motor: the desired motor speed is adapted as a function of the (slowly) changing beam diameter. For this purpose, a measuring wheel 10 with encoder 10A is fitted on the pile beam, so that the current pile feed can be measured. The regulating parameters of the system can also be adapted as a function of the changing beam diameter.
FIG. 6 shows a side view of a pile and ground warp beam arrangement of a face-to-face weaving machine. Situated at the top are three pile warp beams 5 and at the bottom two ground warp beams 50. The position of the mechanical pile feeders is indicated by reference symbol 1.
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In a double-gripper weaving machine, intended for weaving plain velvet and carpets, a pile feeder and a combined pile warp beam let-off motion are equipped with a computer in order to calculate the necessary pile warp feed of each operating cycle of the weaving machine and use said calculation as a reference value, both functions pile feeder and pile warp beam let-off motion, being performed directly. The pile warp beam let-off motion has a regulating system consisting of a multi-axis control system provided for one or more pile warp beams.
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BACKGROUND OF THE INVENTION
[0001] The present invention relates to display mounts and in particular to an improved display mount including an improved load bearing slatwall equipment hanger.
[0002] In some control center environments, visual access to displays is critical in performing vital functions. Display mounts must provide adjustment for the best viewing positions to minimize fatigue. Known monitor mounts include stacked pivoting arms which provide movement in literally any direction. In some applications there is a desire to restrict movement to in-out for the arm while maintaining a tilt/pivot motion of the monitor. Such in-out motion could be achieved using a parallel horizontal arm structure. Unfortunately, parallel horizontal arms cannot efficiently support the weight of some monitors.
[0003] Other known display mounts include slides for forward and rearward motion. At full extension such slides have reduced rigidity and may bind or fail. Additionally, sliding mounts require two slides for stability, much like a drawer would have. The two slides on a carriage may feel reasonably stable in the closed position, but as the slides approach the extended position there is excessive lateral instability and there is nothing forcing the slides to extend synchronously, and a slide mount which requires a short compressed length has poor stability when extended.
[0004] Further, display mounts are often mounted to a slatwall and are attached to the slatwall using equipment hangers and clamps. Such slatwalls comprises a multiplicity of vertically spaced apart parallel horizontal slats (e.g., “T” shaped features). The slatwall hangers may include either an offset which hooks in and up, or a “J” that hooks in and down. The slatwall provides an easily reconfigurable mounting system which simple addition, removal, and adjustment of hangers.
[0005] Some equipment requires clamping the hangers to the slatwall to fix the hanger position preventing the easy movement of the hangers. Known slatwall clamps reach above a higher slat and below a lower slat, and are draw together to clamp the hanger to the slatwall. While this provides an effective method of securing the hanger, because the vertically opposed clamps are drawn together, the amount of vertical force exerted on the slats may be excessive, causing stress on a horizontal portion of the slat, and sometimes breaking the slat even before any load is applied by the hanger.
[0006] With very heavy loads and long lever arms, the stress on the slat can be excessive. This coupled with the stress from the opposing clamps makes the slat the weak link in the assembly.
[0007] Because installations may require a large number of hangers, clamps and clips to be attached to the slatwall, the horizontal portion of the slats can not be made thicker. Therefore, a need exists for a hanger which reduces that stress on a standard slatwall structure.
BRIEF SUMMARY OF THE INVENTION
[0008] The present invention addresses the above and other needs by providing a display mount which is attached to a slatwall using an improved slatwall hanger. The display mount includes vertically pivoting arms providing forward and rearward movement of the display with only slight vertical movement. The slatwall hanger is attached to the slatwall by sandwiching at least one vertical face of a slat between a cover and a clamping member. The cover includes at least one outer lip residing against the front of the vertical face and the clamping member includes at least one inner lip residing against the rear of the vertical face. The clamping member is biased away from the cover by a spring to facilitate insertion of the inner lips between open spaces between consecutive slats. Screws connect the clamping member to the cover and are tightened to grasp the vertical slat face between the lips.
[0009] In accordance with one aspect of the invention, there is provided a Touch Entry Device (TED) mount having parallel pivoting on horizontal axles providing maximum stability and minimizing the mounting envelope and provide a tighter compresses length that slides. The parallel arms pivot in a vertical plane from a rearward reposition, to a vertical position, to a forward position, holding a moveable carrier parallel to a fixed hanger. The arms pivot through small angles minimizing vertical carrier motion while providing adequate horizontal motion. The weight of the arms, carrier, and monitor applies torque to pin and sleeve assemblies of the horizontal axle pairs pushing to each pin and sleeve of each axle pair to opposite sides creating rotational friction in the axles, rather than sliding friction, provides a rigid yet smooth feel through the stroke.
[0010] In accordance with another aspect of the invention, there is provided a TED mount having arms only be slightly wider than the pivoting mechanism in order to rotate a monitor without interference. The horizontal axles allow having an arm width is only limited by our mounting envelope. Vertical axles would allow a greater vertical size requires a narrower arm width. The wider arm allowed by the horizontal axle provides better left-to-right stability and the geometry of the arms provides more than adequate vertical stability because the weight of the assembly, including the monitor, is holding the parallel arm in a rested position.
[0011] In accordance with yet another aspect of the invention, there is provided a TED mount having arms comprising opposing C-channels which partially overlapping but do not touch. The C-channel arm design provides greater strength than blades blade, overlap to eliminate pinch points, and are opposing to create a closed box look. The front arm includes inset lips with enter the rear arm, allowing the front arm to ride inside the rear arm, and eliminating pinch points. As the arms swing their separation changes, but the inset lips fill the gap over the range of arm motion. The inset lips of the front arm allows the bodies of the front and rear arms to be the same width and use the same pivot hardware used with the other axles of the TED mount, and still closes off the box, eliminating the pinch points.
[0012] In accordance with still another aspect of the invention, there is provided a TED mount having a hanger and carrier which are closed boxes for strength and aesthetics, and include ribs which provide stops to limit forward and rearward motion of the arms.
[0013] In accordance with another aspect of the invention, there is provided a TED mount having a triangular shaped hanger to act as a gusset, maximizing strength at the TED mount while minimizing the vertical height at the front where the equipment boxes are pivoting.
[0014] In accordance with yet another aspect of the invention, there is provided a TED mount having a hanger and carrier including reliefs cut into the hanger and carrier above and below the axles. The reliefs allow the interior dimensions of the hanger and carrier to be somewhat greater than the axle sleeves while allowing axle attachment portions of the hanger and carries to be compressed against the sleeves when the axle bolts are tightened—eliminating the twisting of the hanger and carrier which would otherwise occur.
[0015] In accordance with another aspect of the invention, there is provided a TED mount having rotating cable ties. The rotating ties allow cables to rotate when the carrier is moved to reduce stress on the cables.
[0016] In accordance with another aspect of the invention, there is provided a slatwall hanger which eliminate stress created by known clamp on hangers. The slat wall hanger includes opposing inner and outer lips which sandwich vertical faces of the slats and do not apply vertical forces to the slats. The inner lips are inserted between the vertical slat members and dropped into position behind the vertical slat members. The inner and outer lips are then drawn together to horizontally sandwich the vertical slat members, applying no vertical clamping force on the slats. Such sandwiching the vertical slat members eliminates of the stress on the slat that's associated with the known clamping action. As a result, the slats can carry more weight without making the slats physically larger to increase strength, with a resulting loss in the number of hangers which may be attached to the slatwall.
[0017] In accordance with another aspect of the invention, there is provided a slatwall hanger which sandwiches the vertical slat members between inner and outer lips rather than grasping vertically spaced apart slats. Rubber bumpers and/or rubber stick-on pads are attached to the outer lips to protect vertical faces of the slats from scratches.
[0018] In accordance with still another aspect of the invention, there is provided a slatwall hanger having inner and out lips biased apart. In order to engage the slatwall, the inner lip has to be pushed inward between adjacent slats. The larger the slatwall hanger, the more difficult this installation method is. To improve the ease of installation, a spring is incorporated biasing the inner and outer lips apart, making it easier to engage the slatwall hanger with the slatwall. After positioning the slatwall hanger on the slatwall, the lips are drawn together using screw, levers, or other mechanical apparatus.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
[0019] The above and other aspects, features and advantages of the present invention will be more apparent from the following more particular description thereof, presented in conjunction with the following drawings wherein:
[0020] FIG. 1 shows a perspective view of a slat wall and two embodiments of controlled stress hangers according to the present invention.
[0021] FIG. 2 is a cross-sectional view of the second embodiment of the controlled stress hanger according to the present invention taken along line 2 - 2 of FIG. 1 .
[0022] FIG. 3 shows cover and clamping members of the first embodiment of the controlled stress hanger according to the present invention.
[0023] FIG. 4A shows a front view of the first embodiment of the controlled stress hanger according to the present invention.
[0024] FIG. 4B shows a rear view of the first embodiment of the controlled stress hanger according to the present invention.
[0025] FIG. 5 shows cover and clamping members of the second embodiment of the controlled stress hanger according to the present invention.
[0026] FIG. 6A shows a front view of the second embodiment of the controlled stress hanger according to the present invention.
[0027] FIG. 6B shows a rear view of the second embodiment of the controlled stress hanger according to the present invention.
[0028] FIG. 7A shows a narrow version of the clamping member of the first embodiment of the controlled stress hanger according to the present invention.
[0029] FIG. 7B shows a wide version of the clamping member of the first embodiment of the controlled stress hanger according to the present invention.
[0030] FIG. 7C shows a short version of the clamping member of the first embodiment of the controlled stress hanger according to the present invention.
[0031] FIG. 7D shows a tall version of the cover member of the first embodiment of the controlled stress hanger according to the present invention.
[0032] FIG. 8A shows a cover member of the second embodiment of the controlled stress hanger according to the present invention having inward reaching vertical right and left outer lips according to the present invention.
[0033] FIG. 8B shows a cover member of the second embodiment of the controlled stress hanger according to the present invention having the inward reaching vertical right and left outer lips and an inward reaching bottom inner lip according to the present invention.
[0034] FIG. 8C shows a cover member of the second embodiment of the controlled stress hanger according to the present invention having the inward reaching vertical right and left outer lips and the inward reaching bottom inner lip and an inward reaching top inner lip according to the present invention.
[0035] FIG. 8D shows a cover member of the second embodiment of the controlled stress hanger according to the present invention having the inward reaching vertical right and left outer lips and outward reaching top and bottom outer lips according to the present invention.
[0036] FIG. 9A shows a clamping member having notches on opposite ends of top and bottom inner lips according to the present invention.
[0037] FIG. 9B shows a clamping member having notches on opposite ends of the top inner lip only, according to the present invention.
[0038] FIG. 9C shows a clamping member without notches on opposite ends of the inner lips, according to the present invention.
[0039] FIG. 10 shows a perspective view of a spring member for biasing the cover and clamping members apart, according to the present invention.
[0040] FIG. 11A shows a front view of the spring member according to the present invention.
[0041] FIG. 11B shows a side view of the spring member according to the present invention.
[0042] FIG. 11C shows a top view of the spring member according to the present invention.
[0043] FIG. 12 is a perspective view of a Touch Entry Device (TED) mount according to the present invention in a rearward position.
[0044] FIG. 13A is a front of the TED mount according to the present invention in a rearward position.
[0045] FIG. 13B is a side of the TED mount according to the present invention in a rearward position.
[0046] FIG. 14 is a perspective view of the TED mount according to the present invention in a forward position.
[0047] FIG. 15A is a front of the TED mount according to the present invention in a forward position.
[0048] FIG. 15B is a side of the TED mount according to the present invention in a rearward forward position.
[0049] FIG. 16 is a perspective view of a hanger element and equipment box of the TED mount according to the present invention.
[0050] FIG. 17A is a front view of the hanger element and the equipment box of the TED mount according to the present invention.
[0051] FIG. 17B is a side view of the hanger element and the equipment box of the TED mount according to the present invention.
[0052] FIG. 18A is a front view of the equipment box of the TED mount according to the present invention.
[0053] FIG. 18B is a side view of the equipment box of the TED mount according to the present invention.
[0054] FIG. 18C is a rear view of the equipment box of the TED mount according to the present invention.
[0055] FIG. 18D is a top view of the equipment box of the TED mount according to the present invention.
[0056] FIG. 19A is a front view of the carrier and pivot arms of the TED mount according to the present invention.
[0057] FIG. 19B is a side view of the carrier and pivot arms of the TED mount according to the present invention.
[0058] FIG. 20 is a cross-sectional view of the pivot arms of the TED mount according to the present invention taken along line 20 - 20 of FIG. 19B .
[0059] FIG. 21A is a front view of a carrier, the pivot arms, and the hanger of the TED mount according to the present invention.
[0060] FIG. 21B is a side view of the carrier, the pivot arms, and the hanger of the TED mount according to the present invention.
[0061] FIG. 21C is a top view of the carrier, the pivot arms, and the hanger of the TED mount according to the present invention.
[0062] FIG. 22 is a cross-sectional view of the carrier, the pivot arms, and the hanger of the TED mount according to the present invention taken along line 22 - 22 of FIG. 21A .
[0063] FIG. 23 is a perspective view of the carrier, the equipment box, the front pivot arm, and a front arm pivot axle of the TED mount according to the present invention.
[0064] FIG. 24A is a front view of the carrier, the equipment box, the front pivot arm, and the front arm pivot axle of the TED mount according to the present invention.
[0065] FIG. 24B is a side view of the carrier, the equipment box, the front pivot arm, and the front arm pivot axle of the TED mount according to the present invention.
[0066] FIG. 26A is a front view of a display housing according to the present invention.
[0067] FIG. 25 is a detailed view of an adjustable axle according to the present invention.
[0068] FIG. 26B is a side view of the display housing and pivot block according to the present invention.
[0069] FIG. 26C is a rear view of the display housing and pivot block according to the present invention.
[0070] FIG. 26D is a top view of the display housing and pivot block according to the present invention.
[0071] Corresponding reference characters indicate corresponding components throughout the several views of the drawings.
DETAILED DESCRIPTION OF THE INVENTION
[0072] The following description is of the best mode presently contemplated for carrying out the invention. This description is not to be taken in a limiting sense, but is made merely for the purpose of describing one or more preferred embodiments of the invention. The scope of the invention should be determined with reference to the claims.
[0073] A perspective view of a slat wall 10 and two embodiments of controlled stress hangers 12 and 14 according to the present invention are shown in FIG. 1 , and a cross-sectional view of the slatwall 10 and the controlled stress hanger 14 taken along line 2 - 2 of FIG. 1 is shown in FIG. 2 . The slatwall 10 includes a multiplicity of parallel vertically spaced apart slats 11 . Each slat 11 includes a vertical face 11 a and a horizontal standoff 11 b . Open spaces 13 between consecutive slats 11 allow attachment of the controlled stress hangers 12 and 14 to the slat wall 10 . The controlled stress hangers 12 and 14 include outer and inner lips 16 and 18 respectively which sandwich the vertical faces 11 a of the slats 11 to attach the controlled stress hangers 12 and 14 to the slatwall 10 . Such attachment does not create vertical clamping forces on the slats 11 , which when combined with the weight of accessories attached to the controlled stress hangers 12 and 14 , may damage the slats 11 .
[0074] A separated cover 12 a and clamping member 12 b of the controlled stress hanger 12 are shown in FIG. 3 , a front view of the controlled stress hanger 12 is shown in FIG. 4A , and a rear view of the controlled stress hanger 12 is shown in FIG. 4B . The biasing spring 22 is attached to the clamping member 12 b and resides between the cover 12 a and clamping member 12 b biasing the cover 12 a and clamping member 12 b apart. The biasing spring 22 may also be attached to the cover 12 a . Such biasing separates the inner and outer lips 16 and 18 during positioning of the controlled stress hanger 12 on the slatwall 10 . The spring 22 may be a leaf spring, a coil spring, any compressible material which biases the cover 12 a and clamping member 12 b apart which may be compressed to allow sandwiching (or clamping) the vertical face 11 between the inner and outer lips 16 and 18 to attach the controlled stress hanger 12 to the slatwall.
[0075] The cover 14 a and clamping member 14 b of the controlled stress hanger 14 are shown separated in FIG. 5 , a front view of the controlled stress hanger 14 is shown in FIG. 6A , and a rear view of the controlled stress hanger 14 is shown in FIG. 6B . The cover 14 a and clamping member 14 b are attached by screws 20 or the like, and the screws 20 are tightened after the inner lips 18 are inserted between the slats 11 to attached the controlled stress hanger 14 to the slatwall 10 . The controlled stress hanger 14 is thus attached by sandwiching the vertical face 11 a , not by exerting vertical clamping force on vertically spaced apart slats 11 .
[0076] A narrow version of the clamping section 12 b is shown in FIG. 7A , a wide version of the clamping section 12 b is shown in FIG. 7B , a short version of the clamping section 14 b is shown in FIG. 7C , and a tall version of the clamping section 14 b is shown in FIG. 7D . The narrow and short versions of the clamping section include a single spring 22 , and the wide and tall versions of the clamping section include two single springs 22 .
[0077] A cover member 14 a of the controlled stress hanger 14 having inward reaching vertical right and left outer lips 16 is shown in FIG. 8A , a cover member 14 a having the inward reaching vertical right and left outer lips 16 and an inward reaching bottom outer lip 16 is shown in FIG. 8B , a cover member 14 a having the inward reaching vertical right and left outer lips 16 and the inward reaching bottom outer lip 16 and an inward reaching top outer lip 16 is shown in FIG. 8C , and a cover member 14 a having the inward reaching vertical right and left outer lips 16 and outward reaching top and bottom outer lips 16 is shown in FIG. 8D . The various configurations of outer lips are generally interchangeable, but some may be preferred in specific embodiments of the present invention.
[0078] A clamping member 14 b having notches 19 on opposite ends of top and bottom inner lips 18 is shown in FIG. 9A , a clamping member 14 b having notches 19 on opposite ends of the top inner lips 18 is shown in FIG. 9B , and a clamping member 14 b without notches 19 on opposite ends of the inner lips 18 is shown in FIG. 9C . The notches 19 are provided to allow wider spacing of the screws 20 (see FIGS. 5 , 6 A, and 6 B).
[0079] A perspective view of the spring member 22 for biasing the cover 12 a , 14 a and clamping members 12 b , 14 b apart is shown in FIG. 10 , a front view of the spring member 22 is shown in FIG. 11A , a side view of the spring member 22 is shown in FIG. 11B , and a top view of the spring member 22 is shown in FIG. 11C .
[0080] A perspective view of a Touch Entry Device (TED) mount 30 according to the present invention in a rearward position is shown in FIG. 12 , a front view of the TED mount 30 in a rearward position is shown in FIG. 13A , and a side view of the TED mount 30 in a rearward position is shown in FIG. 13B . The TED mount 30 includes five major elements, a hanger 36 , a carrier 38 , a equipment box 32 , a display housing 34 , and front and rear vertically pivoting arms 40 a and 40 b respectively. The equipment box 32 is attached to the hanger 36 by a first pivot block 50 a and the display housing is attached to the carrier 36 by a second pivot block 50 b . Cables 52 are attached to the hanger 36 , front arm 40 a , and carrier 36 by clips 54 . The vertically pivoting arms 40 a and 40 b pivot on horizontal axles 60 (see FIGS. 23 , 24 a , and 25 ).
[0081] The TED mount 30 is preferably mounted to the slatwall 10 using the clamping member 14 , but may be mounted to the slatwall 10 using any mounting, and may be mounted to other support structure, and a TED mount 30 mounted to any support using any mounting is intended to come within the scope of the present invention.
[0082] A perspective view of the TED mount 30 according to the present invention in a forward position is shown in FIG. 14 , a front of the TED mount 30 in a forward position is shown in FIG. 15A , and a side of the TED mount 30 in a forward position is shown in FIG. 15B . The vertically pivoting geometry of the pivot arms 40 a , 40 b allows the display housing 34 to be moved forward and rearward, with negligible vertical movement because the pivot arms 40 a , 40 b pivot between very small angles. Other mounts, such as a slide mount and a horizontally pivoting mount, were considered, but neither provides the strength or stability of the pivot arms 40 a , 40 b . The arms 40 a , 40 b pivot through a vertical position moving from the rearward position in FIG. 13B to the forward position in FIG. 15B .
[0083] The hanger 36 includes a pair of stops 72 a to limit the movement of the arms 40 a and 40 b . The stops 72 a preferably include rubber bumpers for contact with the arms 40 a and 40 b . The carrier 38 similarly includes stops 72 b . A first pivot stop 70 a resided in front of pivot block 50 a to limit vertical movement of the equipment box 32 and a second pivot stop 70 b resided above pivot block 50 b to limit vertical movement of the display housing 34 .
[0084] A perspective view of the hanger 36 and equipment box 32 of the TED mount 30 is shown in FIG. 16 , a front view of the hanger 36 and equipment box 32 of the TED mount 30 is shown in FIG. 17A , and a side view of the hanger 36 and equipment box 32 of the TED mount 30 is shown in FIG. 17B . Front, side, rear, and top views of the equipment box 32 are shown in FIGS. 18A-18D respectively. The equipment box 32 is connected to the hanger 36 by the pivot block 50 a providing both rotation (see FIG. 18D ) and tilt (see FIG. 18B ) of the equipment box 32 . A vertical axle of the pivot block 50 a is composed of a threaded rod 62 v , a pair of plain bearings 64 v and a pair of flange barrel nuts 66 v . The flange barrel nuts 66 v provide axial bearings and the friction adjustments for the pivot block 50 a . Similarly, the horizontal axle of the pivot block 50 a is composed of a threaded rod 62 h , a pair of plain bearings 64 h and a pair of flange barrel nuts 66 h . The pivot block 50 b has similar construction. Additional details of an adjustable axle according to the present invention are shown in FIG. 25 .
[0085] A front view of the carrier 36 and pivot arms 40 a and 40 b of the TED mount 30 is shown in FIG. 19A , a side view of the carrier 36 and pivot arms 40 a and 40 b of the TED mount 30 is shown in FIG. 19B , and a cross-sectional view of the carrier 36 and pivot arms 40 a and 40 b of the TED mount 30 taken along line 20 - 20 of FIG. 19B is shown in FIG. 20 . The arms 40 a and 40 b are parallel and the arm 40 a includes lips 42 overlapped by the arm 40 b preventing material from entering the space between the arms 40 a and 40 b.
[0086] A front view of the carrier 38 , the pivot arms 40 a and 40 b , and the hanger 36 of the TED mount 30 is shown in FIG. 21A , a side view of the carrier 38 , the pivot arms 40 a and 40 b , and the hanger 36 of the TED mount 30 is shown in FIG. 21B , a top view of the carrier 38 , the pivot arms 40 a and 40 b , and the hanger 36 of the TED mount 30 is shown in FIG. 21C , and a cross-sectional view of the carrier 38 , the pivot arms 40 a and 40 b , and the hanger 36 of the TED mount 30 taken along line 22 - 22 of FIG. 21A is shown in FIG. 22 . Arcs 56 are cut into sides of the carrier 38 and hanger 36 on opposite side of axles (see FIGS. 23 , 24 A, and 24 B) to allow axle stays 44 to be adjusted to control motion of the TED mount 30 .
[0087] A perspective view of the carrier 38 , the equipment box 32 , the front pivot arm 40 a , and a front arm pivot axle 48 of the TED mount 30 is shown in FIG. 23 , a front view of the carrier 38 , the equipment box 32 , the front pivot arm 40 a , and a front arm axle 60 (see FIG. 25 ) of the TED mount 30 is shown in FIG. 24A , and a side view of the carrier 38 , the equipment box 32 , the front pivot arm 40 a , and the front arm axle 60 of the TED mount 30 is shown in FIG. 24B . A more detailed view of an axle 60 according to the present invention is shown in FIG. 25 . The axle 60 comprises a threaded rod 62 , a pair of plain bearings 64 and a pair of flange barrel nuts 66 . The flange barrel nuts 66 may be tightened or loosened on the threaded rod 62 to increase or decrease resistance of movement of the arms 40 a , 40 b . For example, the flange barrel nuts 66 may be configured for a slot screwdriver, a phillips screw driver, and allen wrench, a square drive, or any tightening tool. The axles at the lower end of the arms 40 a and 40 b , and in the pivot block 50 a , 50 b are preferably of similar design having the same function, only varying in dimensions.
[0088] A front view of a display housing 34 is shown in FIG. 26A , a side view of a display housing 34 is shown in FIG. 26B , a rear view of a display housing 34 is shown in FIG. 26C , and a top view of a display housing 34 is shown in FIG. 26D . The display housing 34 is connected to the carrier 38 by the pivot block 50 b allowing rotation (see FIG. 2D ) and tilt (see FIG. 26B ) of the equipment box 32 .
[0089] While the invention herein disclosed has been described by means of specific embodiments and applications thereof, numerous modifications and variations could be made thereto by those skilled in the art without departing from the scope of the invention set forth in the claims.
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A display mount is attached to a slatwall using an improved slatwall hanger. The display mount includes vertically pivoting arms providing forward and rearward movement of the display with only slight vertical movement. The slatwall hanger is attached to the slatwall by sandwiching at least one vertical face of a slat between a cover and a clamping member. The cover includes at least one outer lip residing against the front of the vertical face and the clamping member includes at least one inner lip residing against the rear of the vertical face. The clamping member is biased away from the cover by a spring to facilitate insertion of the inner lips between open spaces between consecutive slats. Screws connect the clamping member to the cover and are tightened to grasp the vertical slat face between the lips.
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CROSS-REFERENCES TO RELATED APPLICATIONS
[0001] This application claims the priority of German Patent Application, Serial No. 10 2007 033 629.4, filed Jul. 17, 20071, pursuant to 35 U.S.C. 119(a)-(d), the content of which is incorporated herein by reference in its entirety as if fully set forth herein.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to a method and apparatus for drying particles of bulk material.
[0003] Nothing in the following discussion of the state of the art is to be construed as an admission of prior art.
[0004] Examples of bulk material involved here include gravel, stone chips, and like materials. After being collected, these materials can be used for a wide variety of applications. Typically, particles can be used only when their particle size remains within predefined ranges. After being collected, chunks of these materials are initially comminuted by crushers and then classified according to grain size by a screen. Samples are hereby taken and tested in a laboratory with an analyzer to determine whether their grain size is within the accepted range. As the materials being screened are very moist right after their retrieval or after outdoor storage, the samples have to be dried before being analyzed because particles, in particular those of smaller grain size range, tend to agglomerate, i.e. adhere to one another. In other words, the analysis becomes flawed and may result in claims for damages by the supplier because in a wide variety of cases the grain size must be within a certain range.
[0005] Agglomeration can be prevented when drying the particles before undergoing the analysis, i.e. to substantially decrease the moisture content so as to be considered dry. Drying chambers have been used which can be heated up to a temperature of for example about 100° C. The drying time is, however, very long and may last 24 hours for example. This is disadvantageous because the analysis takes place at a much later time than the extraction of a sample from the screening device. Before being able to intervene in the screening operation, a large amount of material has already been processed. As a result, the use of drying chambers has been discarded for situations that require rapid drying.
[0006] To address these problems, it has been proposed to introduce the particles to be analyzed in a vessel which is then heated by a gas flame. While this may address the time factor, the drying process is too uneven to be considered for laboratory application.
[0007] German Offenlegungsschrift DE 29 21 156 A1 describes a high throughput facility for drying, heating and cooling bulk material. The facility uses a treatment gas which acts on the bulk material supplied to the oscillating conveyor in free fall. Subsequently, bulk material transported by the oscillating conveyor is again exposed to the treatment gas from top to bottom and through the conveyor bottom. As the treatment gas passes through the bulk material, heating or cooling is inadequate. In addition, particles of the bulk material stream that have grain sizes which are smaller than the openings of the conveyor bottom fall through the conveyor bottom. These particles of the particle stream represent waste, rendering the overall process inefficient.
[0008] It would therefore be desirable and advantageous to address these prior art problems and to obviate other prior art shortcomings.
SUMMARY OF THE INVENTION
[0009] According to one aspect of the present invention, a method of drying particles of bulk material for subsequent transfer to an analyzer for determining a grain size of the particles includes the steps of forming a free-flowing particle stream of particles to be dried, advancing the particle stream in a transport direction through a drying zone, and exposing the particle stream in the drying zone to an air flow, generated by a fan and heated by an air heater.
[0010] The present invention resolves prior art problems by the formation of a free-flowing particle stream which is exposed to a heated air flow as it moves through the drying zone. The air flow, generated by a fan, can be heated by the air heating system to a temperature that enables optimum drying results. The particle stream is exposed to the heated air flow as it advanced through the drying zone so as to have residual moisture which allows a separation of the particles even of those particles in the lower grain size range. The air flow may be divided into several single air flows, whereby each single air flow flows through its dedicated air heater. In this way, an even exposure of the particle stream to heated air is ensured.
[0011] According to another feature of the present invention, the heating capacity and thus the temperature of each of the single air flows may be controlled independently from one another. As a result, the temperatures of the single air flows may differ, thereby further optimizing the drying process.
[0012] According to another feature of the present invention, the particle stream may advance continuously through the drying zone. This ensures a constant exposure of the particle stream with heated air.
[0013] According to another feature of the present invention, dividing the particle stream, in particular of particles in the lower range of the grain size, can be enhanced by causing the particle stream to vibrate. This is easy to implement through proper configuration of the conveyor.
[0014] According to another feature of the present invention, a continuous jet of compressed air or an intermittent jet of compressed air at ambient temperature may be directed in transport direction upon the particle stream. In this way, moist particles of smaller grain size are prevented from sticking to the conveyor duct. As a result, all particles of the bulk material, regardless of grain size, can be evenly transported and dried.
[0015] According to another aspect of the present invention, an apparatus for drying particles of bulk material includes a feed container for discharge of particles, a conveyor disposed adjacent to the feed container for advancing the particles received from the feed container in a transport direction, an air heating system placed above the conveyor, and a fan in flow communication with the air heating system for generating an air flow.
[0016] The feed container is constructed to allow control of throughput per time unit with respect to the particle stream and to attain an even particle stream. The particles may be poured into the feed container by hand using a vessel. Of course, loading by means of a conveyor is conceivable as well. The formation of an even particle stream enables optimum drying results as the conveyor moves the particle stream through the drying zone. Positioning the air heating system above the conveyor enables the air flows to directly act on the particle stream, further contributing to an optimum drying effect. The fan may be positioned at any suitable spot within the apparatus, thereby attaining an overall compact structure. The flow connection between fan and air heating system may be realized in any way known to the artisan, for example by a conduit or hose.
[0017] According to another feature of the present invention, the conveyor may be constructed as an oscillating conveyor with a metering duct. The transport speed of the particle stream can then be controlled by changing the frequency of the vibration.
[0018] According to another feature of the present invention, a discharge element may be provided downstream of the conveyor in the transport direction to ensure a reliable collection of dried particles. The discharge element may be constructed in many ways so long as it is capable of catching the particle stream in a vessel. The discharge element may simply be a slide movable in a vertical direction, or a swingable flap, or an inclined discharge duct. Configuration of the discharge element in the form of a slide or flap leads to a desired heat accumulation. The discharge element may, however, also be configured as a conveyor which can be linked to the analyzer for determining grain sizes. Analyzers of a type involved here are known in the field as CPA (computer-assisted particle analysis).
[0019] According to another feature of the present invention, the air heating system may include a plurality of continuous air heaters arranged behind one another and flowed through by the air stream generated by the fan and then divided in single air streams. The number of continuous air heaters depends on the length of the drying zone. The air heaters may be provided with an electric resistance heating. Moreover, the air heaters are constructed to expose the particle stream continuously to the heated air. Therefore, the outlet of each air heater is configured in the shape of a pyramid or cone, with the outlet ports having a greatest cross section.
[0020] According to another feature of the present invention, a control unit may be provided for controlling a heating capacity of the air heaters to thereby control a temperature of the single air flows. As a result, the exiting single air flows may have different temperatures. Suitably, the heating capacity and thus the temperatures of the single air flows may be controlled independently from one another. Suitably, a control circuit is provided for controlling the transport speed of the particle stream, the adjustment of the heating capacity of each air heater, and optionally also the feeding of the bulk material. Providing displays for indicating the temperatures of the single air flows facilitate operation of the apparatus for the operator.
[0021] As described above, particles being dried are extracted as samples by a machine for processing bulk material, such as a screening machine. In order to change the setting of the processing machine in dependence on the grain sizes of the particle stream being analyzed later, it is provided to operate the apparatus as evaluation unit and to couple it directly or online with a viewing device of the associated processing machine, or to equip the apparatus with at least one display to indicate for example settings of the processing machine.
[0022] According to another feature of the present invention, a compressed air generator interacts with the conveyor and produces a continuous or intermittent jet of compressed air directed at the particle stream that passes by in transport direction. This prevents moist particles, in particular those of lower grain size, to stick to the conveyor element of the conveyor or conveyor duct, which would cause an alteration of the screening line of the material sampling. The compressed air jet provides assistance to the conveyor element of the oscillating conveyor so that a combination of oscillating conveyor and pneumatic conveyor is effectively realized.
[0023] According to another feature of the present invention, the conveyor or conveyor duct may have an airtight bottom. Thus, the heated air flow is prevented from flowing through the particle stream, resulting in heat accumulation that further enhances the drying effect.
BRIEF DESCRIPTION OF THE DRAWING
[0024] Other features and advantages of the present invention will be more readily apparent upon reading the following description of currently preferred exemplified embodiments of the invention with reference to the accompanying drawing, in which the sole FIGURE shows a perspective view of an apparatus for drying particles of bulk material in accordance with the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0025] The depicted embodiment is to be understood as illustrative of the invention and not as limiting in any way. It should also be understood that the FIGURE is not necessarily to scale and that the embodiment is sometimes illustrated by graphic symbols, phantom lines, diagrammatic representations and fragmentary views. In certain instances, details which are not necessary for an understanding of the present invention or which render other details difficult to perceive may have been omitted.
[0026] Turning now to FIG. 1 , there is shown a perspective view of an apparatus for drying particles of bulk material in accordance with the present invention. The apparatus has a substantially closed housing 11 which accommodates an unillustrated conveyor, for example an oscillating conveyor. The housing 11 is mounted on a stand comprised of vertical columns 12 and upper and lower struts 13 , 14 to connect the columns 12 . Mounted to one side (left side in FIG. 1 ) of the stand adjacent to the housing 11 is a feed hopper or feed container 15 positioned upstream the conveyor and provided on its conveyor-proximal side with a slide 16 for adjustment of the volume flow and bed height.
[0027] Mounted to a top wall of the housing 11 are a plurality (here three by way of example) continuous air heaters 14 arranged behind one another in movement direction of the conveyor. A further continuous air heater 17 is mounted to the conveyor-distal end of the feed container 15 . All air heaters 17 are equipped with an electric resistance heating to heat single air flows flowing through the housing 11 to temperatures between 200 and 300° C. A fan (not shown), e.g. a high pressure fan, is fluidly connected to the air heaters 17 via conduits or hoses. The operating pressure of the fan ranges between 1.3 and 1.5 bar.
[0028] Attached to one side of the stand is a cubicle 18 for accommodating the electric and/or electronic components. A main switch 19 is mounted to the outer wall of the cubicle 18 to supply the apparatus with electric energy and to disconnect the apparatus from the power supply. Further integrated in an upper portion of the outer wall of the cubicle 18 are four temperature displays 20 to allow an operator to suitably adjust the temperature of the single air flows. Placed below the temperature displays 20 are control lamps 21 to indicate error messages, malfunctions, and the like, especially with respect to the heating capacity of the air heaters 17 and control of the conveyor. The housing 11 is provided on its side distal to the feed container 15 with a discharge element 22 which is constructed in the non-limiting example shown here in the form of a slide that is movable in a vertical direction. As an alternative, the discharge element 22 may also be constructed in the form of a swingable flap or discharge duct.
[0029] In operation, controlled amounts of particles of bulk material are transferred from the feeding container 15 in the form of a particle stream onto the conveyor by which the particles are transported along a drying or heating zone inside the housing 11 to the other end where the particles exit via the discharge element 22 for collection in an unillustrated container for subsequent transfer to an analyzer for determination of a grain size. As the particles advance through the housing, air generated by the fan and passing through the air heaters 17 is heated for heating the particles. The heating capacity of each air heater 17 can hereby be adjusted to the need at hand. In other words, the temperature to which the passing particles are exposed can be individually adjusted by separately controlling the air heaters 17 so that the single air flows released by the air heaters 17 can have different temperatures. During passage of the particles, the conveyor may be acted upon by a continuous or intermittent jet of compressed air which is directed in movement direction of the conveyor upon the particles to prevent any agglomeration of particles.
[0030] While the invention has been illustrated and described in connection with currently preferred embodiments shown and described in detail, it is not intended to be limited to the details shown since various modifications and structural changes may be made without departing in any way from the spirit of the present invention The embodiments were chosen and described in order to best explain the principles of the invention and practical application to thereby enable a person skilled in the art to best utilize the invention and various embodiments with various modifications as are suited to the particular use contemplated.
[0031] What is claimed as new and desired to be protected by Letters Patent is set forth in the appended claims and includes equivalents of the elements recited therein:
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In a method of drying particles of bulk material for subsequent transfer to an analyzer for determining a grain size of the particles, a free-flowing particle stream of particles to be dried is formed to move in a transport direction through a drying zone. As it moves through the drying zone, the particle stream is exposed to an air flow which is generated by a fan and heated by an air heater.
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This is a continuation-in-part of U.S. patent application Ser. No. 08/205,512, filed Mar. 3, 1994, now abandoned, the entirety of which is hereby incorporated herein.
FIELD OF THE INVENTION
The invention generally relates to delivering an occlusion device to a desired site in a mammal to facilitate the formation of mechanical blockage or thrombi in arteries, veins, aneurysms, vascular malformations, and arteriovenous fistulas. More specifically, the invention involves a method and apparatus for detecting electrolytic separation of an endovascular occlusion device from a delivery member after the device has been delivered to the desired site and the coupling between the device and delivery member subjected to an electrolytic environment.
BACKGROUND OF THE INVENTION
Approximately 25,000 intracranial aneurysms rupture each year in North America. The primary purpose of treatment for a ruptured intracranial aneurysm is to prevent rebleeding. There are a variety of ways to treat ruptured and non-ruptured aneurysms.
Possibly the most widely known of these procedures is an extravascular approach using surgery or microsurgery. This treatment is common with intracranial berry aneurysms. The method comprises a step of clipping the neck of the aneurysm, performing a suture ligation of the neck, or wrapping the entire aneurysm. Each of these procedures is formed by intrusive invasion into the body and performed from the outside of the aneurysm or target site. General anesthesia, craniotomy, brain retraction, and placement of a clip around the neck of the aneurysm are typically required in these surgical procedures. The surgical procedure is often delayed while waiting for the patient to stabilize medically. For this reason, many patients die from the underlying disease or defect prior to the initiation of the procedure.
Another procedure--the extra-intravascular approach--involves surgically exposing or stereotactically reaching an aneurysm with a probe. The wall of the aneurysm is then perforated from the outside and various techniques are used to occlude the interior in order to prevent it from rebleeding. The techniques used to occlude the aneurysm include electrothrombosis, adhesive embolization, hog hair embolization, and ferromagnetic thrombosis. These procedures are discussed in U.S. Pat. No. 5,122,136 to Guglielmi et al., the entirety of which is incorporated herein by reference.
A still further approach, the least invasive, is described in Guglielmi et al. It is the endovascular approach. In this approach, the interior of the aneurysm is entered by use of a catheter such as those shown in Engelson (Catheter Guidewire), U.S. Pat. No. 4,884,579 and also in Engelson (Catheter for Guidewire Tracking), U.S. Pat. No. 4,739,768. These patents describe devices utilizing guidewires and catheters which allow access to an aneurysm from remote portions of the body. Specifically, by the use of catheters having very flexible distal regions and guidewires which are steerable to the region of the aneurysm, embolic devices which may be delivered through the catheter are an alternative to the extravascular and extra-intravascular approaches.
The endovascular approach typically includes two major steps. The first step involves the introduction of the catheter to the aneurysm site using devices such as shown in the Engelson patents. The second step often involves filling the aneurysm in some fashion or another. For instance, a balloon may be introduced into the aneurysm from the distal portion of the catheter where it is inflated, detached, and left to occlude the aneurysm. In this way, the parent artery is preserved. Balloons are becoming less in favor because of difficulty in introducing the balloon into the aneurysm sac, the possibility of an aneurysm rupture due to overinflation of the balloon within the aneurysm or due to stress placed on the nonspherically shaped aneurysm by the spherical balloon, and the risk associated with traction produced when detaching the balloon.
A highly desirable embolism-forming device that may be introduced into an aneurysm using endovascular placement procedures, is found in U.S. Pat. No. 4,994,069, to Ritchart et al. The device--typically a platinum/tungsten alloy coil having a very small diameter--may be introduced into an aneurysm through a catheter such as chose described in Engelson above. These coils are often made of wire having a diameter of 2-6 mils. The coil diameter may be 10-30 mils. These soft, flexible coils may be of any length desirable and appropriate for the site to be occluded. For instance, the coils may be used to fill a berry aneurysm. Within a short period of time after the filling of the aneurysm with the embolic device, a thrombus forms in the aneurysm and is shortly thereafter complemented with a collagenous material which significantly lessens the potential for aneurysm rupture.
Coils such as seen in Ritchart et al. may be delivered to the vasculature site in a variety of ways including, e.g., mechanically detaching them from the delivery device as is shown in U.S. Pat. No. 5,250,071, to Palermo or by electrolytic detachment as is shown in Guglielmi et al. (U.S. Pat. No. 5,122,136), discussed above.
Guglielmi et al. shows an embolism-forming device and procedure for using that device. Specifically, the Guglielmi device fills a vascular cavity (such as an aneurysm) with an embolic device, typically a platinum coil, that has been endovascularly delivered. The coil is then severed from its insertion tool by the application of a small electric current. Desirably, the insertion device involves a guidewire which is attached at its distal end to the embolic device by a sacrificial joint that is electrolytically dissolvable. Guglielmi et al. suggests that when the embolic device is a platinum coil, the platinum coil may be 1-50 cm. or longer as is necessary. Proximal of the embolic coil is a guidewire, often stainless steel in construction. The guidewire is used to push the platinum embolic coil, obviously with great gentleness, into the vascular site to be occluded. The patent shows a variety of ways of linking the embolic coil to the pusher guidewire. For instance, the guidewire is tapered at its distal end and the distal tip of the guidewire is soldered into the proximal end of the embolic coil. Additionally, a stainless steel coil is wrapped coaxially about the distal tapered portion of the guidewire to provide column strength to the guidewire. This coaxial stainless steel wire is joined both to the guidewire and to the embolic coil. Insulation may be used to cover a portion of the strength-providing stainless steel coil. This arrangement provides for two regions which must be electrolytically severed before the embolic coil is severed from the guidewire.
U.S. Pat. No. 5,423,829 Nov. 3, 1993, describes a variation of the Guglielmi detachable coil using an improved sacrificial link between the guidewire and the coil. The size of the sacrificial link is limited to allow more precise placement of the embolic device and facile, quick detachment. The focussed electrolysis found at the sacrificial site reduces the overall possibility of occurrence of multiple electrolysis sites and liberation of large particles from those sites.
Previous attempts to detect coil detachment generally involved a DC constant current circuit with a DC voltage monitor (the DC current electrolytically dissolves the sacrificial link). The circuit generally included a DC constant current power source having its positive terminal coupled to the sacrificial link via a guidewire, for example. As discussed above, the link coupled the occlusion device to the guidewire. The negative terminal of the power source typically was coupled to the patient's skin via a large skin electrode (e.g., a ground pad or needle). Other grounding arrangements include providing, an embolic device delivery microcatheter with a cathode that is electrically coupled to the negative terminal of the power source (see U.S. Pat. No. 5,354,295 to Guglielmi et al.). However, the actual moment of detachment of the occlusion device using these schemes may go undetected because detachment of the coil can occur without a corresponding significant increase in DC impedance.
Applicants believe that the electrolytic phenomenon creates the lowest impedance path between the link and ground. This is consistent with certain properties of the coil and sacrificial link, which typically are platinum and stainless steel, respectively. Although the conductivity of stainless steel and platinum are fairly similar under non-reactive environmental conditions, applicants have found that the difference in conductivity between these two materials significantly increases in an electrolytic environment. That is, it takes significantly more voltage for platinum to conduct in the electrolytic solution as compared to stainless steel. More specifically, most of the DC current flows only through the link to the negative electrode. The embolic coil is effectively out of the circuit. As a result, detachment of the coil may go undetected unless the detachment point is at the most proximal point on the sacrificial link.
Applicants have found that the detachment point (i.e., where etching through the link occurs) often is distal from the most proximal point on the link. It is believed that when the electrolysis causes a break in the link downstream from this point, the current still flows through the remaining upstream (proximal) portion of the link and through the body to ground. Since the current continues to flow from the etch site on the linking member, there is no sudden increase in DC impedance at the time of such separation. However, such increase in DC impedance may be detected when all of the upstream (proximal) portion of the sacrificial link finally disintegrates some time considerably later.
In sum, a DC constant current scheme that monitors DC voltage feedback may not detect the precise moment of detachment if the detachment does not occur exactly at the most proximal point on the sacrificial link. Thus, these schemes do not provide the desired repeatability or accuracy in detecting detachment. When detachment goes undetected, one is unable to precisely determine when the system's power should be shut down. The time required for the procedure may be unintentionally increased. In addition, particles may be liberated into the blood stream after coil detachment has occurred.
Thus, there is a need for a system that can accurately detect electrolytic separation of an occlusion device and interrupt the power input in response to detachment detection to discontinue further electrolysis.
SUMMARY OF THE INVENTION
The present invention involves a method and system for detecting electrolytic separation of an occlusion device. The system constructed according to the principles of the present invention comprises a mammalian implant, a delivery member for delivering the implant to a selected site and a link coupling the delivery member to the implant. The system further includes a power supply for supplying DC power with AC superposition to the link. More specifically, the system includes a conductive path and the power supply and link are in that path. The system further includes an AC impedance monitoring circuit also coupled to the path. With this construction, the AC current flows through both the sacrificial link and occlusion device during electrolysis. Accordingly, any sudden or significant change in the monitored AC impedance provides an accurate indication that an open has formed somewhere along the link and the occlusion device has become detached from the delivery member. Thus, unlike a DC voltage monitor, the AC voltage monitor detects separation anywhere along the length of the linking member.
According to another aspect of the invention, the DC power supply to the sacrificial link is interrupted when a sudden change in the monitored AC impedance occurs. In this manner, post detachment electrolysis of the linking member is minimized or avoided.
According to a particular embodiment of the invention, the impedance (as measured by the amplitude of the AC signal) is averaged over time. When a change from the averaged value in excess of 20% is detected, the power input to the sacrificial link is shut off. Changes below this value may be caused by factors other than dissolution of the linking member, which would result in a false indication of detachment. On the other hand, a system that requires more than 40% change may not detect all detachments.
The method for detecting electrolytic separation of an occlusion device according to the present invention includes the steps of (a) providing a delivery member (e.g., a guidewide) and an occlusion device coupled to the delivery member via a link; (b) delivering the occlusion device to a desired site in a mammal via the delivery member; (c) supplying DC power with a superimposed AC signal to the link; and (d) monitoring the amplitude of the superimposed AC signal.
With this method DC power with superposed AC can be interrupted when a sudden change in the amplitude of the superposed AC signal occurs as discussed above. As discussed above, a change of at least about 20% is preferred before triggering power interruption.
The above is a brief description of some of the features and advantages of the present invention. Other features, advantages and embodiments of the invention will be apparent to those skilled in the art from the following description, accompanying drawings and appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of a power drive delivery and detection circuit for detecting electrolytic separation of an occlusion device in accordance with the principles of the present invention.
FIG. 2 is a side view of an electrolytically susceptible, sacrificial link between a core wire and an occlusion device for use in conjunction with the present invention.
FIG. 3 is a side view of a typical corewire assembly for use with the present invention.
FIGS. 4 and 5 schematically depict the method for deploying an occlusion device according to the present invention.
FIG. 6 is a block diagram showing the system of FIG. 1 integrated with a power supply controller according to a preferred embodiment of the invention.
FIG. 7 is a schematic representation of the block diagram of FIG. 1.
FIGS. 8A and 8F are equivalent circuit diagrams for the DC and AC flow paths within a mammal.
FIG. 9 is a block diagram of an alternative power delivery and detection circuit.
FIG. 10 is a block diagram showing the system of FIG. 9 integrated with a power supply controller as in FIG. 6.
FIG. 11 is a schematic representation of the block diagram of FIG. 9.
FIGS. 12A and 12B together are table containing a histogram. The information included therein describes release times for the inventive device.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1, a constant current drive circuit and feedback loop 310 and an embolic device detection circuit (EDDC) 319 for detecting the electrolytic separation of an occlusion device from a delivery member or guidewire are shown in accordance with the principles of the present invention. The EDDC includes an AC impedance monitoring circuit and a circuit for detecting changes in the monitored impedance which can comprise microprocessor 300 as will be described in more detail below. The apparatus or system diagrammatically shown in FIG. 1 can be used in conjunction with various occlusion devices such as those described in U.S. Pat. No. 5,122,136 to Guglielmi et al., the entirety of which patent is incorporated herein by reference. A discussion of the electrolytic separation of such devices will be described and followed by description of the preferred power delivery and detection circuits according to the present invention.
Electrolytic separation of a device from a guidewire may be facilitated by means of the assembly 100 shown in FIG. 2. The assembly 100 is made up generally of a guidewire 102 which tapers at its distal end to a point which is soldered into the proximal end of an occlusion device such as vasoocclusive device 104, which in this case is a coil and is of a radiopaque physiologically compatible material such as platinum, tungsten, gold, iridium or alloys of these. All of the guidewire 102 is covered with an insulating material such as Teflon®, polyurethane, polyethylene, polypropylene, or other suitable polymeric material, except the most distal exposed joint or sacrificial link 106. Link 106 is not coated with an electrical insulator and is of a material such as stainless steel, which is susceptible to electrolytic dissolution in blood. Stainless steel guidewire 102 typically is approximately 10-30 mils. in diameter. Often the guidewire is 50-300 cm. in length, that is to say, from the entry site outside the body to sacrificial link 106.
Sacrificial link 106 is a discrete link. By discrete we mean to say preferably that the joint is substantially dissolved upon release of the vasoocclusive device 104. Alternatively, "discrete" may mean that the length of the link 106 is no greater than the diameter of the sacrificial link 106 or that the electrolytic surface present after the vasoocclusive device is released is not substantially greater than would be a circle having the diameter of the sacrificial link 106. Although the latter reduces the likelihood of multiple etch sites, it may still be possible for etching to occur on the remaining exposed section of the link after the vasoocclusive device has been released.
Also shown in FIG. 2 is a coil 108 which is soldered at its proximal end and, typically, is designed to provide some column strength to the guidewire assembly while not detrimentally affecting the flexibility of the tapered portion of the guidewire 102. Obviously, in the area where the support coil 108 is soldered to guidewire 102, the coating on 102 is not present, allowing the solder to adhere to metal surfaces. Further, on the distal tip of core wire 102 may be found a pair of insulators: sleeve 110 and end plug 112 which serve to further remove the stainless steel coil 108 from contact with the blood while the step of electrolytic detachment is carried out. Preferably, the end plug 112 and sleeve 110 are adhesively attached to each other to form an electrically insulating or electrolysis-tight housing about coil 108. The end plug 112 and sleeve 110 form a planar surface which is generally planar and perpendicular to the axis of the core wire 102 (FIG. 2). The shape of the surface is not critical except to the extent it allows reasonably free access of the blood to the sacrificial link 106. Curved, slotted, and other variations of the end surface are also contemplated to be used in this invention.
As noted above, the distal end of the guidewire 102 is inserted into the solder joint 114 forming the proximal end of vasoocclusive device 104. As will be discussed in more detail below, the discrete sacrificial link 106 is completely or substantially completely dissolved during electrolysis.
Vasoocclusive device 104 is shown to be a coil. It may be a coil or a braid or other vasoocclusive device as is already known. The vasoocclusive device may be covered or connected with fibrous materials tied to the outside of the coil or braided onto the outer cover of the coil as desired. Such fibrous adjuvants may be found in U.S. Pat. No. 5,382,259, to Phelps et al, or in U.S. Pat. No. 5,226,911, entitled "Vasoocclusion Coil with Attached Fibrous Elements", the entirety of which are incorporated by reference.
FIG. 3 shows a typical layout involving the sacrificial link 106 as was generally shown in FIG. 2 above. In FIG. 3, a somewhat conventionally Teflon® laminated or similarly insulated stainless steel guidewire 102 may be placed within a protective catheter. As was noted above, stainless steel guidewire 102 may have a diameter of approximately 10-30 mils. In the embodiment illustrated in FIG. 3, a guidewire assembly 140 is shown as including guidewire 102 which is tapered at its distal end to form a conical section 142 which joins a further section 144 which extends along a length of the guidewire designated with reference numeral 146. Section 144 then gradually narrows down to a thinner section 148. The guidewire assembly 140, as noted above, may be placed within a catheter body and is typically 50-200 cm. in length down to sacrificial link 106. As was shown in FIG. 2, the distal section of guidewire assembly 140 has an outer Teflon® sleeve 110 (or sleeve of other appropriate insulating material), which is shown somewhat longer than the sleeve 110 in. FIG. 2. Furthermore, it has an end plug 112 to permit isolation of the guidewire electrically from the blood except at sacrificial discrete link 106. The proximal end of vasoocclusive device 104 is typically a soldered tip or a joint 114. Preferably, vasoocclusive device 104, when a coil, forms a secondary loop after it emanates from the end of the catheter. The distal end of vasoocclusive device 104 may also have an end plug or tip 154 to prevent punctures of the aneurysm when introduced into the aneurysm sac.
Coil or vasoocclusive device 104 may be prebiased to form a cylinder or conical envelope. However, the vasoocclusive device 104 is extremely soft and its overall shape is easily deformed. When inserted within the catheter (not shown), the vasoocclusive device 104 is easily straightened to lie axially within the catheter. Once ejected from the tip of the catheter, vasoocclusive device 104 may form a shape shown in FIG. 3 or may be loosely deformed to conform to the interior shape of the aneurysm.
FIG. 4 shows the placement of an occlusion device described above within an aneurysm. The process of placing an embolic device is typically practiced under fluoroscopic control with local anesthesia. A transfemoral catheter is utilized to treat a cerebral aneurysm and is usually introduced at the groin. The physician guides the distal tip of the catheter to the target site. The embolic device is then inserted into the catheter. Using a fluoroscope, the physician guides the device to the desired position before separation is initiated. When the vasoocclusive device 104 is platinum, it is not effected by electrolysis. When the guidewire and pertinent portions of the supporting coils at the distal tip of the guidewire are adequately coated with insulating coverings, only the exposed portion at the sacrificial link 106 is effected by the electrolysis.
Returning to FIG. 4, catheter 158 is positioned in a vessel 156 with the tip of catheter 158 placed near neck 160 of aneurysm 162. A vasoocclusive device, such as device 104, is fed into aneurysm 162 at least until sacrificial link 106 is exposed beyond the distal tip of the catheter 158. A positive electric current of approximately 0.1-10 milliamps, preferably about 1 milliamp, at 0.1-6 volts, is applied to guidewire 102 (shown in dashed line) to form a thrombus within aneurysm 162 and dissolve sacrificial link 106. Power supply 170 provides DC power with AC superposition as will be discussed in more detail below.
Referring to FIGS. 4 and 5, the positive terminal of power supply 170 is attached to the proximal end of guidewire 102. A negative or return electrode 168 is coupled to the negative terminal of power supply 170. Electrode 168 is typically placed in electrical contact with the skin. Alternatively, the electrode can comprise a ground wire with a skin patch located behind the shoulder of the patient may be used.
After a vasoocclusive device has been properly placed inside the aneurysm 162, the device 104 is detached from guidewire 102 by electrolytic disintegration of sacrificial link 106. After sacrificial link 106 is completely dissolved by electrolytic action, typically within 1-10 minutes, the guidewire 102 is removed from catheter 158 and from vessel 156. Additional vaso-occlusive devices may be placed in aneurysm 162 along with previously detached devices 104 until aneurysm 162 is occluded as shown in FIG. 5. At this point, guidewire 102 and catheter 158 are withdrawn.
Referring to FIG. 6, a block diagram shows the power drive and detection circuits of FIG. 1 integrated with a power supply controller. A description of the diagram, including description of particular features such as display characteristics follows. However, it should be understood that this description is provided for exemplary purposes and not to limit the invention to particular elements or arrangements discussed below. The voltage display 302, which can be a three digit red LED readout, displays the voltage required to maintain the current flowing through the linking member and the patient. In the preferred embodiment, the fixed-decimal display shows voltages from 0.00 to 9.99 volts DC. In Pause Mode, that is, when electrolytic separation has occurred, and the unit has shut off power to the guidewire, the display shows the voltage immediately prior to coil detachment. The current display 303, which can be a conventional three digit red LED readout, displays the actual current flowing through the linking member and the patient. In the preferred embodiment, the fixed-decimal display shows current from 0.00 to 1.25 mA DC. In addition, the display briefly flashes the new current setting when the current select switch 308 is pressed or when power-up occurs, and then returns to the continuous display of actual current. In Pause Mode, the display shows the current immediately prior to coil detachment. In Normal Mode, the current-select switch 308 is used to change the current setting. When the power supply is turned on, the current is automatically set to 1.00 milliamps. Pressing the current-select switch one time changes the setting to 0.50 milliamps, pressing it a second time changes it to 0.75 milliamps and pressing it a third time returns the setting to 1.00 milliamps. The current may be changed by the physician at any time. Each time the switch is pressed, the current display 303 briefly flashes the new current setting. In Pause Mode, pressing the current-select switch 308 will resume Normal Mode. The current and voltage displays 303 and 302 resume the real-time display of these parameters and the elapsed time display 304 resumes counting from where it was paused.
The elapsed time display 304, which can be a four digit red LED readout, displays the elapsed time in minutes and seconds from the start of the procedure. The flashing colon display shows elapsed time from 00:00 to 59:59. The check indicator 305, which can be a yellow LED indicator, turns on when the microprocessor and EDDC electronics determine that coil detachment has occurred, and indicates that the power supply has entered Pause Mode. The detach indicator 306, which can be a red LED, flashes when the power supply is in Pause Mode after detecting a coil detachment. In each case, the physician is instructed to check detachment using fluoroscopy. In Pause Mode, the display shows the amount of time required to detach the coil.
In the embodiment of FIG. 1, CPU 300, preferably a Motorola MC68HC811E2FN single-chip microcontroller with 2048 bytes of EEPROM, 256 bytes of RAM, an 8 channel 8-bit A/D converter, and three 8-bit I/O ports which control and monitor vital functions of the power supply. However, other processors may be used as would be apparent to one of ordinary skill. In the illustrated embodiment, CPU 300 is shown responsible for monitoring, output DC voltage and current, elapsed time, and requests for changing the DC current. The CPU is outside the critical path of the current control loop, which is implemented in hardware. The CPU manages the LED displays, status indicators and beeper, runs self-diagnostic tests at power-on, issues current setting changes and the fail-safe current enable signal, monitors the EDDC signal to determine when coil detachment has occurred, and monitors the current-select switch.
Referring to FIG. 1, the constant current drive circuit 310 utilizes a feedback loop to maintain the steady current through the patient. The embolic device detection circuit 319, a feedback loop, identifies separation of the embolic device, as reflected in changes in the amplitude of the AC signal from the constant-current source. The AC signal is amplified and rectified by the embolic device detection circuit (EDDC) and is then sent to the CPU for analysis. Although a particular microprocessor has been described, it should be understood that other circuits and topologies (including analog or other nondigital circuits) can be used to monitor and analyze the AC signal to detect changes therein.
In sum, the present invention involves placing an occlusion device, having a sacrificial link coupling the occlusion device to a delivery member (such as a guidewire) at a desired site in a mammal, supplying DC power with AC superposition to the sacrificial link, monitoring the amplitude of the AC signal and detecting any sudden change in that signal. The invention further involves interrupting the DC power input in response to detecting such a sudden change in the AC signal. A preferred embodiment of the embolic device detection circuit (EDDC) is described below with reference to FIG. 7.
The construction of a preferred embodiment of the EDDC is shown in FIG. 7. It is desired to maintain the output of amplifier 330 at a constant current. Amplifier 330 is preferably a National Semiconductor LMC660CN. This device was chosen because of its ability to operate on a single (positive) power supply and because it has a high voltage gain of 126 decibels (dB) and a Gain Bandwidth Product of 1.4 Megahertz (MHz). When the constant current amplifier 330 has achieved equilibrium--when the output current exactly matches the setpoint present at the non-inverting input terminal--the amplifier will oscillate at approximately 20 to 24 kilohertz (kHz) at an amplitude of several hundred millivolts due to a lagging error correction signal (out-of-phase feedback). That is, the amplifier provides constant DC current with AC superposition. The amplitude of this AC signal is dependent on the band-width characteristics of the constant current amplifier and the AC impedance of the steel and the platinum coil and of the patient's body. Capacitor 344, a 4.7 microfarad tantalum capacitor, is used to reduce the amplitude of the self-oscillation voltage to between about 40 to 60 millivolts AC while maintaining a rapid DC response.
Accordingly, a reference voltage 333 is held constant, in this case from 0.166 to 0.332 volts. These voltages represent a constant current output of between 0.5 and 1 milliamp. Resistor 342, with a resistance in this instance of 332 ohms, is connected between the inverting input terminal of amplifier 330 and ground and ensures the maintenance of the constant current flow from amplifier 330.
The constant current flowing out of amplifier 330 flows through the guidewide and to the embolic device. The resistance of the patient's body between the occlusion device and the negative electrode, is generally in the range of 1000 to 4000 ohms and typically about 2000 ohms. Equivalent circuit diagrams of the DC and AC paths are shown in FIGS. 8A and 8B.
Referring to the illustrative example in FIG. 8A, the impedance (Z) values shown are for a constant voltage input of 2.5V DC or a constant current input of 1.0 mA DC. Although link 106 and embolic device 104 are physically connected in series, immersion in an electrolytic solution provides two parallel DC current paths through the body to ground. The DC current path from link 106 towards ground is caused by ion flow away from the stainless steel link during electrolysis. The current flows in from the left side of guidewire 102 and arrives at the branch of the link 106 and coil 104. More than 99% of the DC current flows through the link 106 with less than 1% flowing through coil 104. Thus, if coil 104 becomes detached and a portion of link 106 remains attached to guidewire 102, the main DC current path remains virtually unchanged.
Referring to the illustrative example in FIG. 8B, the impedance (Z) values shown are for a constant voltage input of 2.0V AC at a frequency of 31.25 kHz. As in FIG. 8A, link 106 and coil 104 are physically connected in series. However, immersion in an electrolytic solution does not significantly alter the AC current path so that current flow through the coil can be detected until the coil becomes detached from the guidewire.
In the EDDC (FIG. 7), the AC feedback signal through the patient's body is selectively passed through capacitor 340, in this case, a 0.1 microfarad monolithic capacitor. The AC signal is then amplified in the AC signal amplifier 320, rectified in the AC to DC rectifier 321 and the resulting DC signal is further amplified in DC amplifier 322. The amplified DC signal, the level of which is representative of the amplitude of the error correction voltage of constant current amplifier 330 is then sent to the microprocessor (CPU) 300 for monitoring and analysis as described below. The AC signal, which in illustrated embodiments is a voltage, is monitored by monitoring the level of the amplified DC signal every 10 to 250 milliseconds, preferably every 50 to 200 milliseconds, and constantly averaging the signal every 5 to 50 samples, preferably every 10-20 samples or every 0.5-10 seconds, preferably every 2-6 seconds. In this manner, the CPU can accurately determine the instant the embolic device detaches. When the embolic device detaches, constant current amplifier 330 is no longer in equilibrium and instantly reacts to the change in AC impedance. During the next several dozen milliseconds, amplifier 330 makes large corrections to the DC output voltage to maintain the set current, which disrupts the stable self-oscillation feedback. In other words, the change in AC impedance upsets the balance of the amplifier circuit, and the amplitude of the self-oscillation signal is affected. During this period the amplified EDDC signal will show a sudden voltage drop of greater than 10%, preferably a drop of greater than 20% of the average level for the procedure. This sudden voltage drop reliably detects the dissolution of the junction between the embolic device and the guidewire.
When the sudden voltage drop is detected, the microprocessor immediately halts current flow, energizes the patient isolation relay, freezes the voltage, current and time displays, and emits five beeps to indicate to the physician that coil detachment has occurred. When the power supply is in Pause Mode, no further electrolysis can occur. Using fluoroscopy, the physician can verify that detachment has occurred. If detachment is incomplete and further electrolysis is necessary, the procedure can be resumed by pressing the current-select switch 308 on the front panel. If detachment is verified, the physician can turn off the power supply and withdraw the guidewire. If necessary, another coil can be placed at the site and the power supply started again. If no action is taken, the power supply will automatically turn itself off after 15 minutes.
Referring to FIGS. 9-11, a further preferred embodiment of the invention is shown. Referring to FIG. 9, the power supply and detection circuit 310' and 319' differ from that shown in FIG. 1 in that an external AC signal source 400 has been added, an AC and DC feedback loop 402 has been substituted for the DC feedback loop (FIG. 1), DC level amplifier 322 has been deleted, and the input to AC signal amplifier 320 comes from the output of the power delivery amplifier (as opposed to from the DC feedback loop of 310). With this arrangement, one can directly monitor the AC impedance by observing the reaction of amplifier 330' in response to the change in AC impedance.
In this embodiment, it is important that the power delivery amplifier remain stable when configured as a constant current source so as not to generate a self-oscillating signal as in the embodiment of FIG. 1. In the embodiment shown in FIG. 1, amplifier 330 oscillated on its own, which allowed the monitoring of the AC impedance by the EDDC. However, there were variations in the self-oscillation signal from unit to unit. This preferred embodiment utilizes an external AC source to ensure all units will show the identical response to changes in AC impedance. Since it is desirable to have the amplifier respond exactly to the AC source, the amplifier must not produce any self-oscillating signal of its own. That is, it must remain stable under constant current conditions. Accordingly, the amplifier shown in FIG. 9 is designated with reference to numeral 330'. One suitable amplifier is a TI2274N amplifier manufactured by Texas Instruments. A constant current source is generally preferred for safety purposes when introducing electricity into a patient.
FIG. 10 shows the additional preferred embodiment of 310' and 319' integrated with the power supply controller as in FIG. 6. The operation of the power supply controller in FIG. 8 is as described for FIG. 6.
Referring to FIG. 11, AC signal source 400 is coupled to the reference input of amplified 330' so as to modulate the output current (i.e., provide AC superposition on the DC current). For purposes of example, a 31.25 kHz 100 mV peak-to-peak sine wave has been found to be a suitable input to the amplifier. Capacitor 401 (FIG. 10) is provided between AC signal source 400 and amplifier 330' to isolate DC bias from the AC signal input. The operation of the constant current source (schematically shown in FIG. 11) is the same as that described with reference to FIG. 7.
In operation, an AC signal is provided to the non-inverting input of amplifier 330' where it is summed with the DC current reference. DC current with AC superposition is output from amplifier 330' and sent to the sacrificial link (e.g., link 106). The DC and AC current paths branch as described above with reference to FIGS. 8A, B. These current paths rejoin at the patient return electrode and continue to AC and DC feedback loop 402. The AC signal is monitored at the output of the constant current amplifier where a measurement of AC impedance can be made through EDDC 319'.
One advantage of the position of this AC signal monitoring point is that the amplitude of the AC signal is higher than in the arrangement of FIG. 1, therefore eliminating the need for additional amplification by amplifier 322.
Referring to FIGS. 9 and 11, the AC signal is monitored at a location upstream from the patient's body. More specifically, the amplitude of the AC signal is monitored through pick-off capacitor 340, in this case, a 0.1 microfarad monolithic capacitor. The AC signal from capacitor 340 is then amplified in the AC signal amplifier 320, and is rectified and peak detected in the AC to DC rectifier 321. The DC signal, the level of which is representative of the amplitude of the AC voltage of constant current amplifier 330 is then sent to the microprocessor (CPU) 300 for monitoring and analysis as described below.
The AC signal, which in the illustrated embodiments is voltage, is monitored by sampling the level of the amplified DC signal every 10 to 250 milliseconds, preferably every 50 to 200 milliseconds, and constantly averaging the signal every 5 to 50 samples, preferably every 10-20 samples or every 0.5-10 seconds, preferably every 2-6 seconds. In this manner, the CPU can accurately determine the instant the occlusion device detaches as discussed below.
When the occlusion device detaches, constant current amplifier 330' instantly reacts to the change in AC impedance. The amplitude of the AC waveform increases in an attempt to maintain the constant AC current set at the non-inverting input. During this period the amplified EDDC signal will show a sudden voltage increase of greater than 20%, preferably an increase of greater than 30% of the average level for the procedure. This sudden voltage increase reliably detects the dissolution of the junction between the embolic device and the guidewire.
When the sudden voltage increase is detected, the microprocessor immediately halts current flow, energizes the patient isolation relay, freezes the voltage, current and time displays, and emits five beeps to indicate to the physician that coil detachment has occurred. When the power supply is in Pause Mode, no further electrolysis can occur. Using fluoroscopy, the physician can verify that detachment has occurred. If detachment is incomplete and further electrolysis is necessary, the procedure can be resumed by pressing the current-select switch on the front panel. If detachment is verified, the physician can turn off the power supply and withdraw the guidewire. If necessary, another coil can be placed at the site and the power supply started again. If no action is taken, the power supply will automatically turn itself off after 15 minutes.
The following Example is intended to illustrate but not to limit the invention in any manner.
EXAMPLE
Detachment time studies were run in a preclinical setting Using the Guglielmi Detachable Coil (GDC) as described in Guglielmi et al. with the power delivery and detection circuit of FIG. 1 (see FIGS. 12A and 12B). Thirty pigs were anesthetized and catheterized such that a platinum coil was positioned inside the internal carotid artery. The time of coil detachment was determined using the EDDC. For 28 of the samples, at time 0, the 1 milliamp of power was supplied, for one sample 0.5 milliamps of power was supplied and for one sample 0.75 milliamps of power was supplied. The constant current circuit was monitored as was the embolic device detection circuit. As reflected in FIGS. 12A and 12B, detachment occurred in all cases within 6 minutes of supplying power supply and the majority of detachments occurred within 2 minutes.
The above is a detailed description of particular embodiments of the invention. It is recognized that departures from the disclosed embodiment may be made within the scope of the invention and that many alterations and modifications may be made by those having ordinary skill in the art without departing from the spirit and scope of the invention set out in the claims. The full scope of the invention is set out in the claims that follow and their equivalents. For example, although constant current power delivery circuits have been described above with AC voltage monitoring, constant voltage power delivery circuits also can be used and the AC current monitored. The material selection for the guidewire and occlusion device may vary as would be apparent to one of ordinary skill in the art.
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This invention is a method for ensuring for endovascular occlusion through the formation of thrombi in arteries, veins, aneurysms, vascular malformations, and arteriovenous fistulas. In particular, it deals with a method to predictably determine the instant of electrolytic detachment of an embolic device which is introduced to and is intended to remain at the desired thrombus formation site. The invention further includes a method for delivering an embolic device and detecting its electrolytic separation. According to the present invention, DC power with AC superposition is delivered to the sacrificial link that couples a delivery member (e.g., a guidewire) to an occlusion device. The impedance (as measured by the amplitude of the superposed AC) is monitored. When a predetermined change in that impedance (or amplitude occurs), which indicates coil detachment, the DC power is interrupted to minimize or avoid further electrolysis.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a data carrier with a data processing device as well as to an electronic component with a data processing device for such a data carrier.
2. Description of the Related Art
Recently doubts have arisen as regards the security of data carriers, it being claimed that security-relevant data can be discovered by observation of the power consumption of such a data carrier.
SUMMARY OF THE INVENTION
It is an object of the invention to ensure that such attempts cannot be successful.
This object is achieved according to the invention in that a data carrier with an external power supply is also provided with an internal power supply, at least one switching means being provided in the data carrier in order to realize temporary decoupling of the external power supply.
The advantage of the invention resides in the fact that the decoupling of the external power supply, preferably during security-relevant operations or at least partly during security-relevant operations of the data processing device, frustrates such attempts to fraud.
Advantageous embodiments of the invention are described in the dependent Claims.
The invention will be described in detail hereinafter.
Data carriers provided with data processing devices, for example so-called chip cards, incorporate a test function for the protection of security-relevant transactions, for example the dispensing of cash in money-dispensing machines; such a test function serves to test the authorization for the transaction. In order to establish proof of authorization, use is made of, for example so-called Personal Identification Numbers (PIN). The PIN can be tested in the data processing device of the data carrier while utilizing key algorithms. The power supply for the data carrier is customarily realized by way of contacts or by induction of alternating currents which are converted into a direct current in the data carrier.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a chip card.
FIG. 2 shows a schematic of the chip card FIG. 1 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a so called chip card 1 with a contact field 2 and an embedded chip 3 . The chip 3 is connected to the contact field 2 via internal wires 4 .
In order to preclude with certainty, at least during testing of the transaction authorization, the retrieval of information regarding the authorization key via the externally applied and hence measurable current consumption, or via the signals applied via the current leads, the supply leads to the external current source are decoupled by means of decoupling means, for example switches. In this manner it is prevented that signals which are produced by internal operations can reach the environment. An internal power supply source is used for the power supply of the data processing device at least for this period of time. Suitable for this purpose are, for example, rechargeable batters or a solar cell 10 (shown in FIG. 2 ), illuminated by a read apparatus, or capacitors which are proportioned so that the power supply is ensured at least during the decoupling time. Power supply beyond that time is not required so as to insure the intended decoupling step the duration of the decoupling for the purpose of disguising the operating time can be controlled not only by the data processing device itself but also, for example in a time-controlled manner or until the energy of the internal power supply source for has decreased to a given value.
FIG. 2 shows the internal structure of a preferred embodiment of a chip 3 . Inside the chip there is provided the data processing section 5 in which the security-relevant operations are carried out. To this end the data processing section 5 is connected to the contact field 2 , i.e. to the contacts used for transmitting data from and to the data processing section 5 . The current supply contact V of the contact field 2 is connected to a first switch 6 which is used as said decoupling device. The other end of the first switch 6 is connected to the power supply input of the data processing section 5 . Also connected to this power supply input of the data processing section 5 are a capacitor 7 which is used as said internal supply source and a second switch 8 which is used as a discharging device. The first and the second switch 6 , 8 are controlled by a power supply control circuit 9 . Preferably, the data processing section 5 , the first and the second switch 6 , 8 , the capacitor 7 and the power supply control circuit are arranged on a single chip so as to make it harder to deactivate parts of that arrangement by opening the chip card 1 .
When the internal power supply sources cannot be proportioned so as to enable complete execution of the security-relevant operations during a single decoupling period, the security-relevant operations are preferably subdivided into a number of sub-operations; the internal power supply should then be capable of providing the power supply for at least each sub-operation. The circuit elements fed by the internal power source are thus decoupled from the external power supply at least during such sub-operations.
For example, the decoupling is triggered by switching means which are preferably arranged in such a manner that only weak coupling capacitances occur between internal and external power supply leads.
Additionally, in order to cover any capacitively coupled small signals or small signals arising by irradiation, noise or masking or superposition signals can be applied via the leads connected to the external power supply.
When a capacitor is used as an internal power supply source, for example supporting and smoothing capacitors provided on the chip can be used. These capacitors are discharged during the sensitive internal operations or sub-operations and recharged between the sub-operations, or after the operation, via the external power supply. Preferably, prior to such recharging the internal power supply source is always adjusted to the same discharged state or to different charging states due to incidental power consumption. Thus, sensible information as regards the arithmetic operations performed during the decoupling phase cannot be derived either by measurement of the current required for the recharging.
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In a data carrier with a data processing device in which there is provided an external as well as an internal power supply, it is proposed to provide at least one switching means in which is accommodated in the data carrier in order to realize temporary decoupling of the external power supply, thus making the retrieval of sensitive data impossible.
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CO-PENDING APPLICATIONS
[0001] This is a Continuation of Ser. No. 10/102,697 filed on Mar. 22, 2002
[0002] Various methods, systems and apparatus relating to the present invention are disclosed in the following co-pending granted patents/applications filed by the applicant or assignee of the present invention: 6,428,133, 6,526,658, 09/575,108, 09/575,109.
[0003] The disclosures of these co-pending granted patents/applications are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0004] The following invention relates to a printhead assembly having a flexible printed circuit board to provide power and data to individual printhead modules in a printer.
[0005] More particularly, though not exclusively, the invention relates to a printhead assembly having a flexible printed circuit board for providing data and power connections to individual printhead modules in an A4 pagewidth drop on demand printhead capable of printing up to 1600 dpi photographic quality at up to 160 pages per minute. The flexible printed circuit board also has associated therewith a pair of busbars for carrying the power thereto.
[0006] The overall design of a printer in which the assembly can be utilized revolves around the use of replaceable printhead modules in an array approximately 8½ inches (21 cm) long. An advantage of such a system is the ability to easily remove and replace any defective modules in a printhead array. This would eliminate having to scrap an entire printhead if only one chip is defective.
[0007] A printhead module in such a printer can be comprised of a “Memjet” chip, being a chip having mounted thereon a vast number of thermo-actuators in micro-mechanics and micro-electromechanical systems (MEMS). Such actuators might be those as disclosed in U.S. Pat. No. 6,044,646 to the present applicant, however, might be other MEMS print chips.
[0008] In a typical embodiment, eleven “Memjet” tiles can butt together in a metal channel to form a complete 8½ inch printhead assembly.
[0009] The printhead, being the environment within which the assembly of the present invention is to be situated, might typically have six ink chambers and be capable of printing four color process (CMYK) as well as infra-red ink and fixative. An air pump would supply filtered air through a seventh chamber to the printhead, which could be used to keep foreign particles away from its ink nozzles.
[0010] Each printhead module receives ink via an elastomeric extrusion that transfers the ink. Typically, the printhead assembly is suitable for printing A4 paper without the need for scanning movement of the printhead across the paper width.
[0011] The printheads themselves are modular, printhead arrays can be configured to form printheads of arbitrary width.
[0012] Additionally, a second printhead assembly can be mounted on the opposite side of a paper feed path to enable double-sided high speed printing.
OBJECTS OF THE INVENTION
[0013] It is an object of the present invention to provide a printer assembly having a flexible printed circuit board and busbars for delivering power and data to printhead modules of the assembly.
[0014] It is a further object of the present invention to provide an improved printhead assembly.
SUMMARY OF THE INVENTION
[0015] The present invention provides a printhead assembly for a pagewidth drop on demand ink jet printer, comprising:
[0016] an array of printhead modules extending substantially across said pagewidth,
[0017] a flexible printed circuit board carrying data and power to said modules, the flexible printed circuit board also extending substantially across said pagewidth,
[0018] a pair of busbars electrically connected to the flexible printed circuit board and carrying power thereto, the busbars also extending substantially across said pagewidth.
[0019] Preferably said busbars are soldered to said flexible printed circuit board. Preferably said flexible printed circuit board contacts individual fine pitch flex PCBs on each printhead module.
[0020] Preferably said flexible printed circuit board has a series of gold plated, domed contacts which interface with contact pads on said fine pitch flex PCBs.
[0021] Preferably the flexible printed circuit board extends from one end of the assembly for data connection.
[0022] Preferably said printhead modules are fixed to an elongate channel and an elastomeric ink delivery extrusion is situated between the modules and the channel and the flexible printed circuit board is sandwiched between the elastomeric ink delivery extrusion and the channel and extends around one edge of the extrusion to carry power and data to the printhead modules.
[0023] Preferably the busbars are situated between the flexible printed circuit board and the elastomeric ink delivery extrusion.
[0024] Preferably said gold plated, domed contacts and said contact pads are located alongside said printhead modules and are biased into mutual contact by a resilient force exerted thereon by said channel.
[0025] Preferably said flexible printed circuit board is bonded to the channel.
[0026] As used herein, the term “ink” is intended to mean any fluid which flows through the printhead to be delivered to print media. The fluid may be one of many different colored inks, infra-red ink, a fixative or the like.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] A preferred form of the present invention will now be described by way of example with reference to the accompanying drawings wherein:
[0028] [0028]FIG. 1 is a schematic overall view of a printhead;
[0029] [0029]FIG. 2 is a schematic exploded view of the printhead of FIG. 1;
[0030] [0030]FIG. 3 is a schematic exploded view of an ink jet module;
[0031] [0031]FIG. 3 a is a schematic exploded inverted illustration of the ink jet module of FIG. 3;
[0032] [0032]FIG. 4 is a schematic illustration of an assembled ink jet module;
[0033] [0033]FIG. 5 is a schematic inverted illustration of the module of FIG. 4;
[0034] [0034]FIG. 6 is a schematic close-up illustration of the module of FIG. 4;
[0035] [0035]FIG. 7 is a schematic illustration of a chip sub-assembly;
[0036] [0036]FIG. 8 a is a schematic side elevational view of the printhead of FIG. 1;
[0037] [0037]FIG. 8 b is a schematic plan view of the printhead of FIG. 8 a;
[0038] [0038]FIG. 8 c is a schematic side view (other side) of the printhead of FIG. 8 a;
[0039] [0039]FIG. 8 d is a schematic inverted plan view of the printhead of FIG. 8 b;
[0040] [0040]FIG. 9 is a schematic cross-sectional end elevational view of the printhead of FIG. 1;
[0041] [0041]FIG. 10 is a schematic illustration of the printhead of FIG. 1 in an uncapped configuration;
[0042] [0042]FIG. 11 is a schematic illustration of the printhead of FIG. 10 in a capped configuration;
[0043] [0043]FIG. 12 a is a schematic illustration of a capping device;
[0044] [0044]FIG. 12 b is a schematic illustration of the capping device of FIG. 12 a, viewed from a different angle;
[0045] [0045]FIG. 13 is a schematic illustration showing the loading of an ink jet module into a printhead;
[0046] [0046]FIG. 14 is a schematic end elevational view of the printhead illustrating the printhead module loading method;
[0047] [0047]FIG. 15 is a schematic cut-away illustration of the printhead assembly of FIG. 1;
[0048] [0048]FIG. 16 is a schematic close-up illustration of a portion of the printhead of FIG. 15 showing greater detail in the area of the “Memjet” chip;
[0049] [0049]FIG. 17 is a schematic illustration of the end portion of a metal channel and a printhead location molding;
[0050] [0050]FIG. 18 a is a schematic illustration of an end portion of an elastomeric ink delivery extrusion and a molded end cap; and
[0051] [0051]FIG. 18 b is a schematic illustration of the end cap of FIG. 18 a in an out-folded configuration.
DETAILED DESCRIPTION OF THE INVENTION
[0052] In FIG. 1 of the accompanying drawings there is schematically depicted an overall view of a printhead assembly. FIG. 2 shows the core components of the assembly in an exploded configuration. The printhead assembly 10 of the preferred embodiment comprises eleven printhead modules 11 situated along a metal “Invar” channel 16 . At the heart of each printhead module 11 is a “Memjet” chip 23 (FIG. 3). The particular chip chosen in the preferred embodiment being a six-color configuration.
[0053] The “Memjet” printhead modules 11 are comprised of the “Memjet” chip 23 , a fine pitch flex PCB 26 and two micromoldings 28 and 34 sandwiching a mid-package film 35 . Each module 11 forms a sealed unit with independent ink chambers 63 (FIG. 9) which feed the chip 23 . The modules 11 plug directly onto a flexible elastomeric extrusion 15 which carries air, ink and fixitive. The upper surface of the extrusion 15 has repeated patterns of holes 21 which align with ink inlets 32 (FIG. 3 a ) on the underside of each module 11 . The extrusion 15 is bonded onto a flex PCB (flexible printed circuit board).
[0054] The fine pitch flex PCB 26 wraps down the side of each printhead module 11 and makes contact with the flex PCB 17 (FIG. 9). The flex PCB 17 carries two busbars 19 (positive) and 20 (negative) for powering each module 11 , as well as all data connections. The flex PCB 17 is bonded onto the continuous metal “Invar” channel 16 . The metal channel 16 serves to hold the modules 11 in place and is designed to have a similar coefficient of thermal expansion to that of silicon used in the modules.
[0055] A capping device 12 is used to cover the “Memjet” chips 23 when not in use. The capping device is typically made of spring steel with an onsert molded elastomeric pad 47 (FIG. 12 a ). The pad 47 serves to duct air into the “Memjet” chip 23 when uncapped and cut off air and cover a nozzle guard 24 (FIG. 9) when capped. The capping device 12 is actuated by a camshaft 13 that typically rotates throughout 180°.
[0056] The overall thickness of the “Memjet” chip is typically 0.6 mm which includes a 150 micron inlet backing layer 27 and a nozzle guard 24 of 150 micron thickness. These elements are assembled at the wafer scale.
[0057] The nozzle guard 24 allows filtered air into an 80 micron cavity 64 (FIG. 16) above the “Memjet” ink nozzles 62 . The pressurized air flows through microdroplet holes 45 in the nozzle guard 24 (with the ink during a printing operation) and serves to protect the delicate “Memjet” nozzles 62 by repelling foreign particles.
[0058] A silicon chip backing layer 27 ducts ink from the printhead module packaging directly into the rows of “Memjet” nozzles 62 . The “Memjet” chip 23 is wire bonded 25 from bond pads on the chip at 116 positions to the fine pitch flex PCB 26 . The wire bonds are on a 120 micron pitch and are cut as they are bonded onto the fine pitch flex PCB pads (FIG. 3). The fine pitch flex PCB 26 carries data and power from the flex PCB 17 via a series of gold contact pads 69 along the edge of the flex PCB.
[0059] The wire bonding operation between chip and fine pitch flex PCB 26 may be done remotely, before transporting, placing and adhering the chip assembly into the printhead module assembly. Alternatively, the “Memjet” chips 23 can be adhered into the upper micromolding 28 first and then the fine pitch flex PCB 26 can be adhered into place. The wire bonding operation could then take place in situ, with no danger of distorting the moldings 28 and 34 . The upper micromolding 28 can be made of a Liquid Crystal Polymer (LCP) blend. Since the crystal structure of the upper micromolding 28 is minute, the heat distortion temperature (180° C.-260° C.), the continuous usage temperature (200° C.-240° C.) and soldering heat durability (260° C. for 10 seconds to 310° C. for 10 seconds) are high, regardless of the relatively low melting point.
[0060] Each printhead module 11 includes an upper micromolding 28 and a lower micromolding 34 separated by a mid-package film layer 35 shown in FIG. 3.
[0061] The mid-package film layer 35 can be an inert polymer such as polyimide, which has good chemical resistance and dimensional stability. The mid-package film layer 35 can have laser ablated holes 65 and can comprise a double-sided adhesive (ie. an adhesive layer on both faces) providing adhesion between the upper micromolding, the mid-package film layer and the lower micromolding.
[0062] The upper micromolding 28 has a pair of alignment pins 29 passing through corresponding apertures in the mid-package film layer 35 to be received within corresponding recesses 66 in the lower micromolding 34 . This serves to align the components when they are bonded together. Once bonded together, the upper and lower micromoldings form a tortuous ink and air path in the complete “Memjet” printhead module 11 .
[0063] There are annular ink inlets 32 in the underside of the lower micromolding 34 . In a preferred embodiment, there are six such inlets 32 for various inks (black, yellow, magenta, cyan, fixitive and infrared). There is also provided an air inlet slot 67 . The air inlet slot 67 extends across the lower micromolding 34 to a secondary inlet which expels air through an exhaust hole 33 , through an aligned hole 68 in fine pitch flex PCB 26 . This serves to repel the print media from the printhead during printing. The ink inlets 32 continue in the undersurface of the upper micromolding 28 as does a path from the air inlet slot 67 . The ink inlets lead to 200 micron exit holes also indicated at 32 in FIG. 3. These holes correspond to the inlets on the silicon backing layer 27 of the “Memjet” chip 23 .
[0064] There is a pair of elastomeric pads 36 on an edge of the lower micromolding 34 . These serve to take up tolerance and positively located the printhead modules 11 into the metal channel 16 when the modules are micro-placed during assembly.
[0065] A preferred material for the “Memjet” micromoldings is a LCP. This has suitable flow characteristics for the fine detail in the moldings and has a relatively low coefficient of thermal expansion.
[0066] Robot picker details are included in the upper micromolding 28 to enable accurate placement of the printhead modules 11 during assembly.
[0067] The upper surface of the upper micromolding 28 as shown in FIG. 3 has a series of alternating air inlets and outlets 31 . These act in conjunction with the capping device 12 and are either sealed off or grouped into air inlet/outlet chambers, depending upon the position of the capping device 12 . They connect air diverted from the inlet slot 67 to the chip 23 depending upon whether the unit is capped or uncapped.
[0068] A capper cam detail 40 including a ramp for the capping device is shown at two locations in the upper surface of the upper micromolding 28 . This facilitates a desirable movement of the capping device 12 to cap or uncap the chip and the air chambers. That is, as the capping device is caused to move laterally across the print chip during a capping or uncapping operation, the ramp of the capper cam detail 40 serves to elastically distort and capping device as it is moved by operation of the camshaft 13 so as to prevent scraping of the device against the nozzle guard 24 .
[0069] The “Memjet” chip assembly 23 is picked and bonded into the upper micromolding 28 on the printhead module 11 . The fine pitch flex PCB 26 is bonded and wrapped around the side of the assembled printhead module 11 as shown in FIG. 4. After this initial bonding operation, the chip 23 has more sealant or adhesive 46 applied to its long edges. This serves to “pot” the bond wires 25 (FIG. 6), seal the “Memjet” chip 23 to the molding 28 and form a sealed gallery into which filtered air can flow and exhaust through the nozzle guard 24 .
[0070] The flex PCB 17 carries all data and power connections from the main PCB (not shown) to each “Memjet” printhead module 11 . The flex PCB 17 has a series of gold plated, domed contacts 69 (FIG. 2) which interface with contact pads 41 , 42 and 43 on the fine pitch flex PCB 26 of each “Memjet” printhead module 11 .
[0071] Two copper busbar strips 19 and 20 , typically of 200 micron thickness, are jigged and soldered into place on the flex PCB 17 . The busbars 19 and 20 connect to a flex termination which also carries data.
[0072] The flex PCB 17 is approximately 340 mm in length and is formed from a 14 mm wide strip. It is bonded into the metal channel 16 during assembly and exits from one end of the printhead assembly only.
[0073] The metal U-channel 16 into which the main components are place is of a special alloy called “Invar 36”. It is a 36% nickel iron alloy possessing a coefficient of thermal expansion of {fraction (1/10)} th that of carbon steel at temperatures up to 400° F. The Invar is annealed for optimal dimensional stability.
[0074] Additionally, the Invar is nickel plated to a 0.056% thickness of the wall section. This helps to further match it to the coefficient of thermal expansion of silicon which is 2×10 −6 per ° C.
[0075] The Invar channel 16 functions to capture the “Memjet” printhead modules 11 in a precise alignment relative to each other and to impart enough force on the modules 11 so as to form a seal between the ink inlets 32 on each printhead module and the outlet holes 21 that are laser ablated into the elastomeric ink delivery extrusion 15 .
[0076] The similar coefficient of thermal expansion of the Invar channel to the silicon chips allows similar relative movement during temperature changes. The elastomeric pads 36 on one side of each printhead module 11 serve to “lubricate” them within the channel 16 to take up any further lateral coefficient of thermal expansion tolerances without losing alignment. The Invar channel is a cold rolled, annealed and nickel plated strip. Apart from two bends that are required in its formation, the channel has two square cutouts 80 at each end. These mate with snap fittings 81 on the printhead location moldings 14 (FIG. 17).
[0077] The elastomeric ink delivery extrusion 15 is a non-hydrophobic, precision component. Its function is to transport ink and air to the “Memjet” printhead modules 11 . The extrusion is bonded onto the top of the flex PCB 17 during assembly and it has two types of molded end caps. One of these end caps is shown at 70 in FIG. 18 a.
[0078] A series of patterned holes 21 are present on the upper surface of the extrusion 15 . These are laser ablated into the upper surface. To this end, a mask is made and placed on the surface of the extrusion, which then has focused laser light applied to it. The holes 21 are evaporated from the upper surface, but the laser does not cut into the lower surface of extrusion 15 due to the focal length of the laser light.
[0079] Eleven repeated patterns of the laser ablated holes 21 form the ink and air outlets 21 of the extrusion 15 . These interface with the annular ring inlets 32 on the underside of the “Memjet” printhead module lower micromolding 34 . A different pattern of larger holes (not shown but concealed beneath the upper plate 71 of end cap 70 in FIG. 18 a ) is ablated into one end of the extrusion 15 . These mate with apertures 75 having annular ribs formed in the same way as those on the underside of each lower micromolding 34 described earlier. Ink and air delivery hoses 78 are connected to respective connectors 76 that extend from the upper plate 71 . Due to the inherent flexibility of the extrusion 15 , it can contort into many ink connection mounting configurations without restricting ink and air flow. The molded end cap 70 has a spine 73 from which the upper and lower plates are integrally hinged. The spine 73 includes a row of plugs 74 that are received within the ends of the respective flow passages of the extrusion 15 .
[0080] The other end of the extrusion 15 is capped with simple plugs which block the channels in a similar way as the plugs 74 on spine 17 .
[0081] The end cap 70 clamps onto the ink extrusion 15 by way of snap engagement tabs 77 . Once assembled with the delivery hoses 78 , ink and air can be received from ink reservoirs and an air pump, possibly with filtration means. The end cap 70 can be connected to either end of the extrusion, ie. at either end of the printhead.
[0082] The plugs 74 are pushed into the channels of the extrusion 15 and the plates 71 and 72 are folded over. The snap engagement tabs 77 clamp the molding and prevent it from slipping off the extrusion. As the plates are snapped together, they form a sealed collar arrangement around the end of the extrusion. Instead of providing individual hoses 78 pushed onto the connectors 76 , the molding 70 might interface directly with an ink cartridge. A sealing pin arrangement can also be applied to this molding 70 . For example, a perforated, hollow metal pin with an elastomeric collar can be fitted to the top of the inlet connectors 76 . This would allow the inlets to automatically seal with an ink cartridge when the cartridge is inserted. The air inlet and hose might be smaller than the other inlets in order to avoid accidental charging of the airways with ink.
[0083] The capping device 12 for the “Memjet” printhead would typically be formed of stainless spring steel. An elastomeric seal or onsert molding 47 is attached to the capping device as shown in FIGS. 12 a and 12 b. The metal part from which the capping device is made is punched as a blank and then inserted into an injection molding tool ready for the elastomeric onsert to be shot onto its underside. Small holes 79 (FIG. 13 b ) are present on the upper surface of the metal capping device 12 and can be formed as burst holes. They serve to key the onsert molding 47 to the metal. After the molding 47 is applied, the blank is inserted into a press tool, where additional bending operations and forming of integral springs 48 takes place.
[0084] The elastomeric onsert molding 47 has a series of rectangular recesses or air chambers 56 . These create chambers when uncapped. The chambers 56 are positioned over the air inlet and exhaust holes 30 of the upper micromolding 28 in the “Memjet” printhead module 11 . These allow the air to flow from one inlet to the next outlet. When the capping device 12 is moved forward to the “home” capped position as depicted in FIG. 11, these airways 32 are sealed off with a blank section of the onsert molding 47 cutting off airflow to the “Memjet” chip 23 . This prevents the filtered air from drying out and therefore blocking the delicate “Memjet” nozzles.
[0085] Another function of the onsert molding 47 is to cover and clamp against the nozzle guard 24 on the “Memjet” chip 23 . This protects against drying out, but primarily keeps foreign particles such as paper dust from entering the chip and damaging the nozzles. The chip is only exposed during a printing operation, when filtered air is also exiting along with the ink drops through the nozzle guard 24 . This positive air pressure repels foreign particles during the printing process and the capping device protects the chip in times of inactivity.
[0086] The integral springs 48 bias the capping device 12 away from the side of the metal channel 16 . The capping device 12 applies a compressive force to the top of the printhead module 11 and the underside of the metal channel 16 . The lateral capping motion of the capping device 12 is governed by an eccentric camshaft 13 mounted against the side of the capping device. It pushes the device 12 against the metal channel 16 . During this movement, the bosses 57 beneath the upper surface of the capping device 12 ride over the respective ramps 40 formed in the upper micromolding 28 . This action flexes the capping device and raises its top surface to raise the onsert molding 47 as it is moved laterally into position onto the top of the nozzle guard 24 .
[0087] The camshaft 13 , which is reversible, is held in position by two printhead location moldings 14 . The camshaft 11 can have a flat surface built in one end or be otherwise provided with a spline or keyway to accept gear 22 or another type of motion controller.
[0088] The “Memjet” chip and printhead module are assembled as follows:
[0089] 1. The “Memjet” chip 23 is dry tested in flight by a pick and place robot, which also dices the wafer and transports individual chips to a fine pitch flex PCB bonding area.
[0090] 2. When accepted, the “Memjet” chip 23 is placed 530 microns apart from the fine pitch flex PCB 26 and has wire bonds 25 applied between the bond pads on the chip and the conductive pads on the fine pitch flex PCB. This constitutes the “Memjet” chip assembly.
[0091] 3. An alternative to step 2 is to apply adhesive to the internal walls of the chip cavity in the upper micromolding 28 of the printhead module and bond the chip into place first. The fine pitch flex PCB 26 can then be applied to the upper surface of the micromolding and wrapped over the side. Wire bonds 25 are then applied between the bond pads on the chip and the fine pitch flex PCB.
[0092] 4. The “Memjet” chip assembly is vacuum transported to a bonding area where the printhead modules are stored.
[0093] 5. Adhesive is applied to the lower internal walls of the chip cavity and to the area where the fine pitch flex PCB is going to be located in the upper micromolding of the printhead module.
[0094] 6. The chip assembly (and fine pitch flex PCB) are bonded into place. The fine pitch flex PCB is carefully wrapped around the side of the upper micromolding so as not to strain the wire bonds. This may be considered as a two step gluing operation if it is deemed that the fine pitch flex PCB might stress the wire bonds. A line of adhesive running parallel to the chip can be applied at the same time as the internal chip cavity walls are coated. This allows the chip assembly and fine pitch flex PCB to be seated into the chip cavity and the fine pitch flex PCB allowed to bond to the micromolding without additional stress. After curing, a secondary gluing operation could apply adhesive to the short side wall of the upper micromolding in the fine pitch flex PCB area. This allows the fine pitch flex PCB to be wrapped around the micromolding and secured, while still being firmly bonded in place along on the top edge under the wire bonds.
[0095] 7. In the final bonding operation, the upper part of the nozzle guard is adhered to the upper micromolding, forming a sealed air chamber. Adhesive is also applied to the opposite long edge of the “Memjet” chip, where the bond wires become ‘potted’ during the process.
[0096] 8. The modules are ‘wet’ tested with pure water to ensure reliable performance and then dried out.
[0097] 9. The modules are transported to a clean storage area, prior to inclusion into a printhead assembly, or packaged as individual units. The completes the assembly of the “Memjet” printhead module assembly.
[0098] 10. The metal Invar channel 16 is picked and placed in a jig.
[0099] 11. The flex PCB 17 is picked and primed with adhesive on the busbar side, positioned and bonded into place on the floor and one side of the metal channel.
[0100] 12. The flexible ink extrusion 15 is picked and has adhesive applied to the underside. It is then positioned and bonded into place on top of the flex PCB 17 . One of the printhead location end caps is also fitted to the extrusion exit end. This constitutes the channel assembly.
[0101] The laser ablation process is as follows:
[0102] 13. The channel assembly is transported to an eximir laser ablation area.
[0103] 14. The assembly is put into a jig, the extrusion positioned, masked and laser ablated. This forms the ink holes in the upper surface.
[0104] 15. The ink extrusion 15 has the ink and air connector molding 70 applied. Pressurized air or pure water is flushed through the extrusion to clear any debris.
[0105] 16. The end cap molding 70 is applied to the extrusion 15 . It is then dried with hot air.
[0106] 17. The channel assembly is transported to the printhead module area for immediate module assembly. Alternatively, a thin film can be applied over the ablated holes and the channel assembly can be stored until required.
[0107] The printhead module to channel is assembled as follows:
[0108] 18. The channel assembly is picked, placed and clamped into place in a transverse stage in the printhead assembly area.
[0109] 19. As shown in FIG. 14, a robot tool 58 grips the sides of the metal channel and pivots at pivot point against the underside face to effectively flex the channel apart by 200 to 300 microns. The forces applied are shown generally as force vectors F in FIG. 14. This allows the first “Memjet” printhead module to be robot picked and placed (relative to the first contact pads on the flex PCB 17 and ink extrusion holes) into the channel assembly.
[0110] 20. The tool 58 is relaxed, the printhead module captured by the resilience of the Invar channel and the transverse stage moves the assembly forward by 19.81 mm.
[0111] 21. The tool 58 grips the sides of the channel again and flexes it apart ready for the next printhead module.
[0112] 22. A second printhead module 11 is picked and placed into the channel 50 microns from the previous module.
[0113] 23. An adjustment actuator arm locates the end of the second printhead module. The arm is guided by the optical alignment of fiducials on each strip. As the adjustment arm pushes the printhead module over, the gap between the fiducials is closed until they reach an exact pitch of 19.812 mm.
[0114] 24. The tool 58 is relaxed and the adjustment arm is removed, securing the second printhead module in place.
[0115] 25. This process is repeated until the channel assembly has been fully loaded with printhead modules. The unit is removed from the transverse stage and transported to the capping assembly area. Alternatively, a thin film can be applied over the nozzle guards of the printhead modules to act as a cap and the unit can be stored as required.
[0116] The capping device is assembled as follows:
[0117] 26. The printhead assembly is transported to a capping area. The capping device 12 is picked, flexed apart slightly and pushed over the first module 11 and the metal channel 16 in the printhead assembly. It automatically seats itself into the assembly by virtue of the bosses 57 in the steel locating in the recesses 83 in the upper micromolding in which a respective ramp 40 is located.
[0118] 27. Subsequent capping devices are applied to all the printhead modules.
[0119] 28. When completed, the camshaft 13 is seated into the printhead location molding 14 of the assembly. It has the second printhead location molding seated onto the free end and this molding is snapped over the end of the metal channel, holding the camshaft and capping devices captive.
[0120] 29. A molded gear 22 or other motion control device can be added to either end of the camshaft 13 at this point.
[0121] 30. The capping assembly is mechanically tested.
[0122] Print charging is as follows:
[0123] 31. The printhead assembly 10 is moved to the testing area. Inks are applied through the “Memjet” modular printhead under pressure. Air is expelled through the “Memjet” nozzles during priming. When charged, the printhead can be electrically connected and tested.
[0124] 32. Electrical connections are made and tested as follows:
[0125] 33. Power and data connections are made to the PCB. Final testing can commence, and when passed, the “Memjet” modular printhead is capped and has a plastic sealing film applied over the underside that protects the printhead until product installation.
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A printhead assembly for a pagewidth drop on demand ink jet printer includes an array of printhead modules extending across the pagewidth. A flexible printed circuit board carries data and power to the modules and also extends across the pagewidth. A pair of busbars is electrically connected to the flexible printed circuit board to carry power to it. The busbars also extend across the pagewidth.
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BACKGROUND OF INVENTION
1. Field of Invention
This invention relates to a method of constructing concrete structures in which special apparatus is used to raise concrete plates cast one on top of the other at ground level, thus forming roof and floors and utilizing the lifting motion to form concrete walls.
2. Description of Prior Art
A method, generally known as "Liftslab" has been around in the building industry for many years. The method is well known. Equally well known in the building industry is a method called "Slipform." The Liftslab method has been employed in highrise apartments, office buildings, parking garages and other multi-floor structures. The Liftslab method is usually combined with posttensioning in the concrete slabs to enable the slabs to be thinner and more flexible.
The Slipform method has been employed extensively and practically exclusively in the construction of silo's, observation towers, elevator shafts and other structures where simple high vertical walls or columns form the main structural element. In the Slipform method walls or other vertical elements are formed by casting concrete in a bottomless form that rises while the concrete is being placed. Both the Liftslab and Slipform methods have been combined with conventional methods and have been generally restricted to highrise structures.
The advantages of the above described methods are: one; that practically no formwork is needed to form the concrete, and two; that placing of concrete is simple and fast. The Liftslab method and the Slipform method have not been used to any significant extent in residential and other one- and two- story structures for reason that equipment cost has thus far not justified such use.
SUMMARY OF INVENTION
This invention has for its object to take the lifting motion of one method (Liftslab) and use it for the other method (Slipform) thus bringing down cost. A further object is to simplify the method of lifting so that lifting can be done by unskilled labor further bringing down cost. The word slab is hereafter replaced by the word plate as plate is a more appropriate term to describe a thin, flat configuration. The objects of the invention will be made more apparent from the following more detailed description and accompanying drawings.
BRIEF DESCRIPTION OF INVENTION
FIG. 1 is a section showing yokes attached to a concrete plate in upward motion, and inside the yokes are horizontal members which support the sides of a bottomless form.
FIG. 2 shows the part of a slipform yoke that attaches to the upward moving slab.
FIGS. 3 4 and 5 show three stages in which a ground slab remains at ground level and suspended plates are lifted to higher levels. FIG. 4 shows walls being "extruded". FIG. 5 shows a completed Liftplate-Slipform structure, having a typical posttension type structure in which overhangs balance the midspan equalizing stresses in the plates.
FIG. 6 is a diagram showing wires and pulleys designed to prevent a lifted plate from tipping.
FIG. 7 shows a simple span concrete plate being lifted by a telescoping central post while the exterior walls are being "extruded".
FIG. 8 is a detail of the mechanism that activates the telescoping action.
FIGS. 9 10 11 and 12 show the progression of a two-plate structure being lifted, specifically drawing attention to suspender rods holding the first plate while the second plate travels further.
FIG. 13 shows the assembly of a lifting mechanism.
FIG. 14 is an exploded view of a split-nut-and-socket assembly belonging to the lifting mechanism shown in FIG. 13.
FIG. 15. shows a section through the split-nut-and-socket assembly of FIG. 14.
FIG. 16 shows an alternate to the split-nut-and-socket arrangement.
FIG. 17 is a diagram of wires and pulleys serving to ensure that a concrete plate is raised in a synchronous manner.
FIG. 18 shows details of a climbing mechanism that may be used to raise concrete plates as in FIGS. 3. 4. and 5.
FIG. 19 and 20 are longitudinal sections through the climbing mechanism of FIG. 18.
DESCRIPTION OF PREFERRED EMBODIMENTS
Referring now to the illustrations and describing the construction method in more detail, the building process is started by casting concrete plates one on top of the other using a bond breaking compound between them. When the plate to be lifted has hardened, yokes (1) spaced 5 to 10 feet apart, are placed along the edge of the top plate (2) and stringers (3) connecting a row of yokes and in turn supporting the bottomless form (4) are installed. A typical yoke (1) is attached to the concrete plate (2) by means of a bolt (5) which passes through a slotted hole (6) in the yoke into an insert cast in the concrete plate. The yoke has two adjusting screws (7) which, combined with the slotted hole (6) enable the yoke to be adjusted horizontally, vertically and angle-wise. Wood or steel wedges may be used in lieu of adjusting screws (7). The bottomless form is best placed above the plate as shown but may in particular circumstances be located wholy or partly under the plate after the plate is partly lifted. When all yokes (1) are aligned and the stringers (3) and the bottomless forms (4) are in place and the concrete plate (2) is ready for lifting, concrete (8) is poured in the bottomless form (4). After a period of time when the concrete (8) has taken its initial set the concrete plate (2) is slowly lifted. The lifting motion results in the concrete wall (8) to be exposed at the bottom and a cavity (9) to develop at the top. As the lifting continues the wall (8) continues to be exposed and the cavity (9) is filled with new concrete. Thus a wall (8) is formed as if extruded by the bottomless form (4).
The above described wall construction is flexible as to materials and composition. The wall can be made of lightweight concrete. The exterior can have a fluted texture or a cast-in skin of metal or other durable material. Similarly the interior can have prefinished sheet material cast in by placing that material against the interior face of the bottomless form and casting the concrete against it. The prefinished material should preferably have a vapor barrier and insulating material in its composition. Furthermore the wall can be made of sandwich type by placing blocks of insulation material in the middle of the wall during casting. The advantages of this invention become apparent when one considers that the floor and the roof can be insulated by spreading a thin layer of plaster on the bond breaking compound atop the slab below and bedding into this plaster a layer of insulation material. The plaster and the insulation material become an intregal part of the roof or floor construction when lifted. Thus a completely insulated and finished structural shell can be formed by unskilled labor in the shortest possible time.
Simplification of the lifting mechanism, so it can be operated by unskilled labor, is a further object of this invention.
Three methods have been developed to accomplish this goal, each serving specific structural conditions.
The telescoping post method shown in FIGS. 6, 7, and 8 is designed specifically for wall bearing structures. The crosshead method shown in FIGS. 13, 14, 15, 16 and 17 is designed for permanent post bearing structures and the climbing cone method shown in FIGS. 18, 19 and 10 is a universal system that can be used in low and high structures.
Now describing the telescoping-post method in more detail, this building process starts by casting concrete plate (11) on a ground slab or on soil. When that plate (11) is cured. One, two or more telescoping posts (12) are placed in openings reserved in the plate in strategic locations so as to permit rods or cables (10) pending from the top of the telescoping post (12) to attach to the edges of the plate (11). The bottomless form (4) is subsequently filled with concrete and after the concrete has its initial set the telescoping post is slowly extended while concrete is poured in the bottomless form (4). When the intended height is reached the wall (8) is poured solid with the concrete plate (11) and the telescoping post (12) removed. This action can be repeated for any number of stories.
The telescoping action is caused by two hydraulic rams (13) FIG. 8 which are placed on top of the fixed portions (14) of the telescoping post and which drives the crosshead (15) upward. Crosshead (15) attaches to the moving portion (16) of the telescoping post (12) through wedge (17) and cleats (18). When the rams (13) are activated, the moving portion (16) of the telescoping post (12) moves upward traveling the extent of the stroke of the ram. As the rams reach the end of the stroke, wedge (19) is inserted allowing crosshead (15) to return and start the next cycle. Ram actions are repeated until the desired height of the concrete plate (11) is reached.
Now referring to FIG. 6; in order to ensure that the concrete plate (11) is lifted evenly, cables (20) are attached to the top of the fixed portion of the telescoping post and, like the parallel ruler on a drawings board, the cables are laced through two pulleys (21) and (22) and attached at the other end to the ground or the structure on which the telescoping post (12) rests. Three or more cables (20) are required to ensure stability.
Now describing the crosshead method. Reference is made to Patent No. 2686420 obtained by Philip N. Youtz on Aug. 17, 1954. Youtz's patented method has suspended threaded rods pending from the top of supporting columns and attaching to a structural member or floor. Hydraulic rams in Youtz's method pull the threaded rods in a manner similar to the method described in here. My invention differs from Youtz's and other methods in the way in which the suspended rods engage the crossheads. This invention also differs in that it provides means for supporting a floor temporarily while a subsequent floor is being lifted. The action of this lifting method starts when hydraulic ram (23) FIG. 13, is activated and crosshead (24) rises in relation to column (25). Lifting rods (26) engaged to upper crosshead (24) by means of nuts (33t) also rise and lift floors (27) and (28). When ram (23) reaches the end of its stroke, nuts (33b) are lowered by lifting socket (33) off split nut (32), placing the split nut in the lower position, reinstalling the socket (33) and turning it until the split nut seats firmly on the crosshead. When both nuts (33b) are thus seated on the lower crosshead (29) the hydraulic ram (23) is retracted allowing upper crosshead (24) to return. Subsequently nuts (33t) are moved down in the manner nuts (33b) have been moved down. A new cycle can now be initiated.
The split plug (30) is designed to permit coupling (34) to pass-through the lifting assembly and can be eliminated if couplings are not used. Washer (31) serves to ensure even bearing of the nuts (33t and 33b) on the crossheads or on the split plugs (30).
A further simplification of the crosshead method is shown in FIG. 16 where lifting rods (26) are engaged to crossheads (24) and (29) by means of wedges instead of the split-nut-and-socket assembly.
Prior to this invention nuts were turned down by hand or by motor. The slightest damage in threads made hand turning most difficult and often caused motors to stop. The split-nut-and-socket method eliminates those problems and speeds up work.
Continuing discussion of the crosshead method, bottom crosshead (29) FIG. 13 shows four holes (35). These holes (35) are used to attach temporary suspension rods (36) FIGS. 10 and 11. Temporary suspension rods (36) serve to support a floor at an intermediate level while the next floor is being lifted as shown in FIGS. 10 and 11.
Now referring to FIG. 17; since simplification of the lifting mechanism so it can be operated by unskilled labor is a further object of this invention, it is necessary to have a simple and reliable method of synchronization. The method of synchronization is shown in FIG. 17. The method has wires or steel fish lines (37) attached to the tops of columns. The wires converge through a series of pulleys (38) and have weights (40) to keep them taut. As the plate (41) rises the wires move across the floor. Markers (39) attached to each wire must move at the same rate in order to ensure synchronous lifting. An operator manipulating the valves that feed the rams on each column watches the markers, moving them at the same rate of speed.
Now describing the climbing cone mechanism shown in FIGS. 18, 19, and 20 and also shown in FIGS. 3 and 4; this climbing method is for universal use and designed for lifting structures covered herein or any other lifting condition. The climbing cone assembly comprises two cone-shaped sleeves (42) and (43) that have wedges (44) gripping on a column or any other element. The two cone sleeves also have shelves (45) between which hydraulic rams (46) are placed. To put the climbing mechanism in operation rams (46) are extended. This action presses the lower cone (43) tight against the column while it raises upper cone (42). As the rams (46) reach the end of their stroke and are retracted, the upper cone grips around the column and asserts the location it has reached. As the rams (46) are retracted, internal or external springs (51) pull the lower cone (43) toward the upper cone until the rams (46) are completely retracted and ready to start a new cycle. This action of the climbing mechanism is powerful and capable of lifting concrete plates (2) in a secure and reliable fashion. Cones may be split and halves bolted or pinned together to facilitate installation and removal at midlevel.
In commonly known liftslab methods shearheads are attached to columns by welding or by pins or bolts. This invention has shearheads (47) which have tapered inside surfaces. The attachment of these shearheads (47) to the column is through wedges (50) which grip the column. This method of attachment is positive and eliminates the need for welding or any other mechanical method thus saving time and cost.
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A method for constructing concrete enclosures by means of casting two or three or more concrete plates one on top of the other, raising them o permanent or temporary structural posts and using the lifting motion of the plates to pour concrete in bottomless sideforms thus forming the walls.
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This application is a continuation of application Ser. No. 07/075,185, filed July 13, 1987 abandoned, which is a continuation of Ser. No. 06/811,778 filed Dec. 20, 1985 abandoned.
BACKGROUND OF THE INVENTION
Down-the-hole drills are generally known in the art. One such drill has been shown and described in U.S. Pat. No. 4,084,646 issued to Ewald H. Kurt and assigned to Ingersoll-Rand Company. The drawings and specifications of that patent are hereby incorporated by reference to describe the basic drill and similar drills to which the present invention applies.
OBJECT OF THE INVENTION
An object of the invention is to increase the effective volume in front of the impact piston without increasing the diameter of the drill.
A further object of this invention is to reduce the effective back pressure developed on the impact piston of a down-the-hole drill in order to improve its deep hole work output.
Yet a further object of this invention is to provide an impact piston with a reduced diameter section forming an accumulator of pressure fluid which travels with the piston without biasing the piston in directions of travel.
Another object of the present invention is to provide a down-the-hole drill with increased work output at higher back pressures experienced in deep holes without increasing the diameter of the drill.
These and other objects are obtained in a percussive drill apparatus of the valveless type comprising:
a casing; a backhead disposed at the back end of the casing adapted to connect the drill apparatus to a drill string and a source of pressure fluid; a distributor disposed within the casing towards the back end of the casing; a percussive member disposed at the front end of the casing to form a chamber having a back end disposed towards the distributor and a front end disposed towards the percussive member between the distributor and the percussive member within the casing; a cylinder sleeve disposed in the chamber toward the back end of the chamber; a first pressure fluid passage formed between the casing and the cylinder sleeve to connect the pressure fluid source to the chamber; a piston disposed in the chamber to reciprocate axially therein and impart a blow on the percussive member; the piston being in sliding contact with the cylinder sleeve adjacent the back end of the chamber and in sliding contact with the casing adjacent the front end of the chamber; a means for continuously applying pressure fluid to a selected portion of the back end of the piston to thereby provide a continued driving force on the piston towards the front end of the chamber; a means for alternately supplying and exhausting pressure fluid to a selected portion of one side of the piston disposed towards the back end of the chamber and to a selected portion of the other side of the piston disposed towards the front end of the chamber to thereby reciprocate the piston; the means for alternately supplying and exhausting pressure fluid to the back side of the piston includes a second pressure fluid passage extending from the first pressure fluid passage along the interior of the sleeve and the exterior of the piston;
The improvement comprising:
A means for accumulating additional pressure fluid in a portion of the piston dispersed towards the front end; and a means for communicating the means for accumulating additional pressure fluid with the first pressure fluid passage.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a longitudinal section of the center portion of a pneumatic down-the-hole rock drill according to the prior art.
FIG. 2 is a longitudinal section of the center portion of a pneumatic down-the-hole rock drill according to the present invention.
FIG. 3 is a cross sectional view of the prior art rock drill taken at section 3--3 shown on FIG. 1.
FIG. 4 is a cross sectional view of the rock drill according to the prior art taken at section 4--4.
FIG. 5 is a cross sectional view of the rock drill according to the present invention taken at section 5--5.
FIG. 6 is a cross sectional view of the rock drill according to the present invention taken at section 6--6.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The drawings are numbered to correspond with similar parts in U.S. Pat. No. 4,048,646 for easy identification and comparison. However, for purposes of understanding this invention it is necessary to know that, in a conventional down hole drill and similar reciprocating hammer devices driven by a pressurized gas, when the pressure fluid enters the area in front of the piston on its down stroke it restrains the piston. If this occurs prior to piston impact as it does in the referenced patent, it reduces the maximum obtainable impact.
In the referenced valveless design some overlap or early introduction of pressure fluid in the frontal area is required for the cycles to operate effectively and the present invention is directed at reducing the restraining effect prior to impact. I have determined that one way this may be accomplished is to effectively increase the volume associated with the frontal area of the impact piston. Since this volume must be pressurized a greater flow of pressure fluid is required to effect the same back pressure. Since the flow of pressure fluid is to some degree restricted by limitation of design in down-the-hole drills this results in an effective time delay in reaching full pressure below the piston. The delay results in increased piston impact while retaining the overlap required for the cycle to operate. The above is particularly effective where as in a deep hole, the exhaust back pressure is substantial and the frontal area pressure is therefore already relatively high.
Referring to FIG. 1 a rock drill longitudinal section is shown to illustrate the concerned parts of a down-the-hole pneumatic drill according to U.S. Pat. No. 4,048,646.
Briefly, in this pneumatic drill the air passes through the drilled ports 63 in the cylinder sleeve 50 into an annular passageway 52 between the outside diameter of the cylinder sleeve 50 and the inside of the casing 6.
From here the air moves forward into chamber 64 between the piston outside surface and the casing 6 inside diameter. This is an "air reservoir space" because there is always pressure fluid in this chamber and it is from here that the air passes either to the upper chamber 68 of the piston or the lower chamber 69 of the piston. With the piston in its lower position (shown in FIG. 1 which it would attain before the air is turned on, the air passes into the lower chamber 69, exerting a force on the lower impact imparting surface 40 of the piston 30, driving it upwards towards its one or inlet end. The air continues to feed into the lower chamber 69 or V1 and is trapped between the piston 30, the bit 8, the casing 6 and a spacer ring 13 until the lower sealing surface 37 of the casing, that is, until edge 86 contacts shoulder 87. When this occurs, air is shut off to the lower chamber 69. The piston continues to move upwards, however, by virtue of its velocity and expansion of the air in the lower chamber. As the piston rises, the lower sealing surface of the axial bore 42 of piston 30 pulls off the end of the exhaust tube 23. At this point, the air in the lower chamber 69 exhausts it to the drill bit 8 and out into the exhaust bore 67.
While this is going on at the lower end of the piston, other events are occurring at the upper end. The first is that the upper chamber 68 is sealed off as the sealing surface 43 of the piston axial bore engages the lower end of the enlarged head 66 of the exhaust rod 65 of the distributor. Shortly thereafter, pressure fluid is admitted, via axial porting slots 33, into the upper chamber 68 as edge 88 of the piston slots 36 uncover the shoulder 89 of the undercut 80 inside the cylinder sleeve 50. The air entering the upper chamber 68 first stops the piston on its upwards travel (about an inch from hitting the distributor) and then reverses the piston travel, pushing it forward at increasing velocity. The pressure fluid flow to the upper chamber 68 is shut off as edge 88 of the piston slots 36 cover the shoulder 89 of the undercut 80. From this point on, the piston is driven by expanding pressure fluid. When sealing surface 43 loses contact with enlarged head 66 of the distributor exhaust rod, air in the upper chamber 68 is exhausted through the piston 30, into the exhaust tube 23 and out the bit 8 as the piston continues to move towards its impact on other end, edge 86 of the lower sealing surface 39 of the piston 30 loses contact with the shoulder 87 of internal surface 39 of the casing again at which point air re-enters the lower chamber 69. Shortly thereafter, the piston 30 impacts against the bit 8. The piston rebounds somewhat. This, plus the air re-entering the lower chamber, starts the next cycle.
As can be appreciated by one skilled in the art once the edge of the lower sealing surface 39 loses contact with the shoulder 87 and air begins to enter the lower chamber, the piston 30 begins to loose velocity as a result of the force of such air action on the lower impact surface 40 of the piston. This results in energy loss and it is therefor desirable to minimize the pressure developed in chamber 69.
The pressure build up in chamber 69 has been substantially reduced by the present invention. As shown in FIG. 2 the piston 30 is provided with a substantial circumferential undercut 100 which forms a substantial volume V2 for the accumulation of pressure fluid. Shoulder 34 of the prior art device has been extended outward to form an upper circumferential sealing surface 101 of the same diameter as lower circumferential sealing surface 39.
The casing internal fluted longitudinal passages 102 have been extended to perform the same function, at shoulder 87' in cooperation with edge 86' of upper sealing surface 101, as edge 86 performed with shoulder 87 in the prior art and at the approximate same point in cycle timing.
FIGS. 3 and 6 compare the cross sections taken at sections 3--3 and 6--6 respectively in FIGS. 1 and 2.
FIGS. 4 and 5 compare the cross sections through the piston at sections 4--4 and 5--5 respectively in FIGS. 1 and 2. These clearly show the reduced piston diameter in FIG. 5 which forms volume V2.
It can now be appreciated by one skilled in the art that, once the upper sealing surface 101 loses contact with shoulder 87', in order for pressure to build up the pressure fluid or air must fill both volume V1 and V2. With a given available flow of air the total pressure build up is time delayed thereby substantially reducing the retarding force on the piston and dramatically increasing the impact of the piston on the bit.
The results have been most impressive particularly in deep holes where the back pressure or exhaust already reduces piston impact and where the slightly increased air flow resulting for the increased front end volume is of benefit air cleaning the hole.
Having described my invention numerous modifications will now occur to one skilled in the art and I do not wish to be limited in the scope of my invention except as claimed.
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A fluid impact tool is disclosed of the type commonly known as a down-the-hole drill for drilling of rock. The improvement herein described increases deep hole drill performance by providing a means for accumulating piston return air in a traveling air pocket found on the piston. This effectively increases the piston front end volume so as to decrease the effect of the front end air cushion and thereby increase impact. This is particularly effective during operation with increased back pressure such as found in deep holes.
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This is a division of application Ser. No. 07/234,382, filed Aug. 23, 1988 now U.S. Pat. No. 5,173,489.
BACKGROUND OF THE INVENTION
1. Field of Invention
This invention relates to α,α-disubstituted aromatic and heteroaromatic compounds, to pharmaceutical compositions containing them, processes for preparing them, and methods of using them in mammals to treat cognitive deficiencies and/or neurological dysfunction and/or mood disturbances such as found, for example, in degenerative nervous system diseases.
2. Background Including Prior Art
There is a steadily growing need for effective treatment for Nervous System Disorders causing cognitive and neurological deficiencies. Many of these diseases, of which the incidence generally rises with increasing age, are due to degenerative changes in the nervous system. Although in early stages of some diseases certain systems are rather specifically affected (e.g., cholinergic systems in Alzheimer's Disease, and Myasthenia Gravis, the dopaminergic system in Parkinson's Disease, etc.), multiple neurotransmitter system deficiencies (acetylcholine, dopamine, norepinephrine, serotonin) are generally found at later stages of diseases such as senile dementia, multi-infarct dementia, Huntington's disease, mental retardation, etc. This may explain the generally observed multiple symptomatology which includes cognitive, neurological and affective/psychotic components (see Gottfries, Psychopharmacol. 86, 245, 1985). Deficits in the synthesis and release of acetylcholine in the brain are generally thought to be related to cognitive impairment (see Francis et. al., New England J. Med., 313, 7, 1985) whereas neurological deficits (e.g., Parkinsonian symptoms) and mood/mental changes may be related to impairment of dopaminergic and serotonergic systems, respectively. Other neurological deficits (e.g., Myasthenia Gravis) are related to cholinergic deficiencies in the peripheral nervous system.
Treatment strategies employed hitherto encompass vasoactive drugs like vincamine and pentoxifylline; "metabolic enhancers" like ergoloid mesylates, piracetam and naftidrofuryl; neurotransmitter precursors like 1-DOPA, choline and 5-hydroxytryptamine; transmitter metabolizing enzyme inhibitors like physostigmine; and neuropeptides like adrenocorticotropic hormone and vasopressin-related peptides. Except for 1-DOPA treatment in Parkinson's disease and cholinesterase inhibitor treatment in Myasthenia Gravis, these treatment strategies have generally failed to produce clinically significant improvements (Hollister, Drugs, 29, 483, 1985). Another strategy to treat these multiple symptoms is to enhance the residual function of the affected systems by enhancing the stimulus-induced release of neurotransmitters. Theoretically, such an enhancement would improve the signal-to-noise ratio during chemical transmission of information, thereby reducing deficits in processes related to cognition, neurological function and mood regulation.
To date, there are not many patent or literature references which describe 3,3-heterocyclic disubstituted indolines. Most pertinent are Japanese Patent 55-129184, issued Oct. 6, 1980 and M. Ogata et. al., Eur. J. Med. Chem-Chim. Ther., 16(4), 373-378 (1981), which describe antifungal compounds having the formula: ##STR2## wherein R is H, halogen, alkyl, or alkoxy;
R 1 is H, alkyl, aryl or acyl; and
R 2 is thienyl, or imidazole, amongst non-heterocyclic groups.
R. W. Daisley, et. al.,, J. Heterocyclic Chem., 19, 1913-1916, (1982), report 1-methyl-3,3-dipiperidinoindol-2-(3H)-one as product from the reaction of the corresponding (Z) or (E) 1-arylmethylidene-indol-3 (2H) -one with ethyl cyanoacetate in the presence of excess piperidine. No utility for the compound is described.
Japanese Patent 59-98896 describes high sensitivity, high stability recording medium containing a 3,3-disubstituted-2-oxo-2,3-dihydroindole derivative of the formula shown below as a near infrared absorber. ##STR3## wherein R 1 , R 2 , same or different, are a saturated heterocyclic ring including morpholino, pyrrolidinyl, amongst others containing at least one nitrogen atom; and
R 3 is H or alkyl.
3,3-bis(morpholino)oxoindole is also disclosed in U.S. Pat. No. 4,273,860, to A. Adin, Jun. 16, 1981 and in A. Adin, et. al., Research Disclosures, 184, 446-454 (1979 ), as a destabilizer material in a photoinhibitor composition utilizing cobalt (111) complexes.
The above references, other than J55-129184, and M. Ogata et. al., Eur. J. Med. Chem-Chim, Ther., 16(4), 373-378 (1981) all describe 3,3-disubstituted indolines wherein the heterocyclic groups are both saturated rings. In all of the above references, the heterocyclic ring is attached to the indoline by a ring nitrogen. Furthermore, in the references other than J55-129284, there is no suggestion of pharmaceutical utility for these 3,3-disubstituted indolines.
SUMMARY OF THE INVENTION
It has now been found that certain aromatic and heteroarcmatic compounds having a broad ring core structure and pendant α,α-disubstituted heterocyclic groups enhance the stimulus-induced release of neurotransmitters, specifically acetylcholine and, in addition, dopamine and serotonin in nervous tissue and improve processes involved in learning and memorization of an active avoidance task.
More particularly, according to the present invention there is provided a pharmaceutical composition consisting essentially of a pharmaceutically suitable carrier and an effective amount of a compound of the formula ##STR4## or a salt thereof wherein X and Y are taken together to form a saturated or unsaturated carbocyclic or heterocyclic first ring and the shown carbon in said ring is a to at least one additional aromatic ring or heteroaromatic ring fused to the first ring;
one of Het 1 or Het 2 is 2, 3, or 4-pyridyl or 2, 4, or 5-pyrimidinyl and the other is selected from
(a) 2, 3, or 4-pyridyl,
(b) 2, 4, or 5-pyrimidinyl,
(c) 2-pyrazinyl,
(d) 3, or 4-pyridazinyl,
(e) 3, or 4-pyrazolyl,
(f) 2, or 3-tetrahydrofuranyl, and
(g) 3 -thienyl.
Additionally provided is a method for the treatment of a neurological disorder in a mammal which comprises: administering to the mammal a therapeutically effective amount of a compound of Formula (I).
Further provided are particular novel classes of compounds within Formula (I) which are active in treating a neurological disorder in a mammal. These compounds are as follows:
(1) A compound having the formula: ##STR5## wherein: p is 0 or 1;
Z is O or S;
R is C 1 -C 10 alkyl, C 3 -C 8 cycloalkyl 2-pyridyl, 3-pyridyl, 4-pyridyl, or ##STR6## V, W, X, and Y independently are H, halo, C 1 -C 3 alkyl, OR 1 , NO 2 , CF 3 , CN or NR 1 R 2 ;
R 1 and R 2 independently are H or C 1 -C 3 alkyl;
Het 1 and Het 2 independently are 6-membered heterocyclic aromatic rings containing one or two nitrogen atoms as part of the ring optionally substituted with one substituent selected from the group C 1 -C 3 alkyl, halo, OR 1 or NR 1 R 2 ; or
an N-oxide or pharmaceutically suitable acid addition salt thereof.
(2) A compound having the formula: ##STR7## or a salt thereof wherein each J, K, L and M independently are N, CR 1 , CR 5 or CR 2 with the proviso that when either M 4 , M 5 or both is N, then B, D or both cannot be R 1 or R 2 ; ##STR8## n is 0, 1, 2 or 3; R 1 and R 2 independently are H, halo, alkyl of 1-3 carbon atoms, acyl, OR 3 , NO 2 , CN, NR 3 R 4 , or fluoroalkyl of 1-3 carbon atoms;
R 3 and R 4 independently are H, alkyl of 1-3 carbon atoms, or acyl;
B and D independently are R 1 or R 2 or, when A is (CH 2 ) o can be taken together to form --CH═CH--, or --CH 2 --CH 2 --;
R 5 independently is H, or is taken together with R 1 to form a 2,3- or a 3,4-fused benzo ring;
one of Het 1 or Het 2 is 2, 3, or 4-pyridyl or 2, 4 or 5-pyrimidinyl and the other is selected from:
(a) 2, 3 or 4-pyridyl,
(b) 2, 4, or 5-pyrimidinyl,
(c) 2-pyrazinyl,
(d) 3, or 4-pyridazinyl,
(e) 3, or 4-pyrazolyl,
(f) 2, or 3-tetrahydrofuranyl, and
(g) 3-thienyl.
(3) having the formula: ##STR9## or a salt thereof wherein a is a single bond or double bond; X independently when a is a single bond is O, S, CR 1 R 2 , CQ, C(R 1 )OR 3 , or -(--C H 2 --)- n where n is 1, 2 or 3;
X independently when a is a double bond is CR 2 or COR 3 ;
X and Y taken together when a is a single bond is ##STR10## X and Y taken together when a is a double bond is ##STR11## where n is 1 or 2; Q when a is a single bond is ═O, ═S, H 2 , OR 3 , ═NOR 1 , ##STR12## --(H)F, F 2 , (R 1 )OR 3 , ═OR 1 R 2 ;
Q when a is a double bond is R 2 , OR 3 or halo.
p is 2 or 3;
R 1 is H, alkyl of 1-10 carbon atoms, cycloalkyl of 3-8 carbon atoms, or ##STR13## R 2 is R 1 , NO 2 , CN, CO 2 R 1 , ##STR14## or halo; R 3 is R 1 or ##STR15## W, Y, Z independently are H, halo, alkyl of 1-3 carbon atoms, OR 3 , NO 2 , CF 3 , fluoroalkyl, CN, or N(R 1 ) 2 ; and
Her 1 and Her 2 are as defined in (2) above.
(4) A compound having the formula: ##STR16## or a salt thereof wherein
a is a single bond or double bond;
b is a single bond or double bond, provided one of a or b is a single bond;
X independently when a and b are single bonds is O, S, CR 1 R 2 , CQ, C(R 1 )OR 3 , or --(--CH 2 --)-- n where n is 1, 2 or 3, N(CH 2 ) p R 3 where p is O or 1, or NCOR 1 ;
X independently when one of a or b is a double bond is CR 2 , COR 3 , or N;
V independently when b is a single bond is CQ;
V independently when b is a double bond is CR 2 or COR 3 ;
A is a single bond, --(--CR 2 1 --) n --, --X--, --(--CR 2 1 --) n --X, where n is 1, 2 or 3 and
X is as defined above when a is a single bond;
Y and V taken together when A and b are single bond is ##STR17## Y and V taken together when A is a single bond is --CH 2 --(--CH 2 --) m --CH 2 -- where m is 1 or 2;
provided that when Y and V are connected, then V and X are not connected;
V and X taken together when b is a double bond is C--CH═CH--CH═CH--C--, or --C--(--CH 2 --) p --C;
provided that when V and X are connected, then Y and V are not connected;
Q when a is a single bond is ═O, ═S, H 2 , OR 3 , ═NOR 1 ##STR18## --(H)F, F 2 , (R 1 )OR 3 , ═CR 1 R 2 ; Q when a is a double bond is R 2 , OR 3 or halo;
p is 2 or 3;
R 1 is H, alkyl of 1-10 carbon atoms, cycloalkyl of 3-8 carbon atoms, or ##STR19## R 2 is R 1 , NO 2 , CN, CO 2 R 1 , ##STR20## or halo; R 3 is R 1 or ##STR21## W, Y, Z each independently is H, halo, alkyl of 1-3 carbon atoms, OR 3 , NO 2 , CF 3 , CN, or N(R 1 ) 2 ; and
Het 1 and Het 2 are as defined in (2) above.
PREFERRED EMBODIMENTS
Preferred Het 1 and Het 2 in a compound of Formula (I) is where one is 2, 3 or 4-pyridyl or 2, 4, or 5-pyrimidinyl and the other is 2, 3, or 4-pyridinyl, 2, 4, or 5-pyrimidinyl, or 2, or 3-tetrahydrofuranyl.
Het 1 and Het 2 are most preferably selected from:
(a) 4-pyridinyl and 4-pyridinyl,
(b) 4-pyrimidinyl and 4-pyrimidinyl,
(c) 4-pyridinyl and 4-pyrimidinyl,
(d) 4-pyridinyl and 3-tetrahydrofuranyl.
Preferred compounds of Formula (4) are those where:
p is o; or
Z is O; or
X and Y are H; or
R is CH 3 , phenyl or m-chlorophenyl; or
Het 1 and Het 2 are each pyridyl attached by a ring carbon atom.
Specifically preferred compounds of Formula (4) are:
3,3-Bis(2-pyridylmethyl)-1-phenylindolin-2-one;
3,3-Bis(3-pyridylmethyl)-1-phenylindolin-2 -one;
3,3-Bis(4-pyridylmethyl)-1-phenylindolin-2-one;
3,3-Bis(4-pyridylmethyl)-1-methylindolin-2-one;
3,3-Bis(4-pyridylmethyl)-1-(3-chlorophenyl)-indolin-2-one;
and pharmaceutically suitable acid addition salts thereof.
Preferred compounds of Formula (II) are:
(a) those compounds of Formula (II) where:
A is a bond, i.e., is (CH 2 ) n where n is 0; B and D are R 1 and R 2 ; 0 to 2 of J, K 2 , L 3 and M 4 are N and the remainder are CR 1 or CR 5 ; and 0 to 2 of J 8 , K 7 , L 6 and M 5 are N and the remainder are CR 2 , with the proviso that when either M 4 , M 5 or both is N, then B, D or both cannot be R 1 or R 2 ; or
R 1 and R 5 are H; or
R 2 is H, halo, alkyl of 1-3 carbon atoms, OR 3 , NH 2 , or fluoroalkyl of 1-3 carbon atoms; or
Het 1 and Het 2 are as preferred for compounds of Formula (I).
Specifically preferred compounds of Formula (II) (a) are:
5,5-Bis(4-pyridinylmethyl)cyclopenta[2, 1-b:3,4-b']dipyridine;
9,9-Bis(4-pyridinylmethyl)indeno-[1,2-b]pyridine;
5,5-Bis (4-pyridinylmethyl)cyclopenta[2,1-c:3,4-c']dipyridine;
9,9-Bis(4-pyridinylmethyl)cyclopenta[1,2-c:4,3-c']dipyridine;
9,9-Bis(4-pyridinylmethyl)cyclopenta[1,2-b:3,4-b']dipyridine.
(b) those of Formula (II) where:
B and D are both H; and J, K, L and M are carbon atoms; or
A is (CH 2 ) n where n is 0-3, ##STR22## CHOH, C═NOH, O, S, NR 3 , ##STR23## or SO 2 ; or R 1 and R 5 are H; or
R 2 is H, halo, alkyl of 1-3 carbon atoms, OR 3 NH 2 , or fluoroalkyl of 1-3 carbon atoms; or
Het 1 and Het 2 are as preferred for compounds of Formula (I).
Specifically preferred compounds of Formula (II) (b) are:
9,9-bis(4-pyridylmethyl)anthrone dihyctrochloride;
9,9-bis(4-pyridylmethyl) fluorene dihydrochloride;
9,9-bis(4-pyridylmethyl)xanthene;
9,9-bis(4-pyridylmethyl)anthrone dihydrochloride;
(c) those of Formula (II) where:
A is a bond, i.e., is (CH 2 ) n where n is O; and J, K, L and M are carbon atoms; or
B and D are taken together to form --CH═CH-- or --CH 2 --CH 2 --
R 1 and R 5 are H; or
R 2 is H, halo, alkyl of 1-3 carbon atoms, OR 3 , NH 2 , or fluoroalkyl of 1-3 carbon atoms; or
Het 1 and Het 2 are as preferred for compounds of Formula (I).
Specifically preferred compounds of Formula (II)(c) are:
9,9-bis(4-pyridinylmethyl)cyclopenta[def]phenanthrene;
9,9-bis(4-pyridinylmethyl)-4,5-dihydrocyclopenta[def]phenanthrene.
Preferred compounds of Formula (III) are:
(a) those of Formula (III) where:
a is a single bond; and
X independently is O, CR 1 R 2 , or C(R 1 )OR 3 ;
W, Y and Z independently are H or OCH 3 ; or
Q is ═O, ═S, H 2 , OR 3 , ═CR 1 R 2 , or C(R 1 )OR 3 ; or Het 1 and Het 2 are as preferred for compounds of Formula (I).
Specifically preferred compounds of Formula (III)(a) where a is a single bond are:
4-((2,3-dihydro-3-phenyl-l-(4-pyridinylmethyl)-1-inden-1-ylmetyyl))-pyridine dihydrochloride;
1,1-bis(4-pyridinylmethyl)-1,3-dihydro-2H-inden-2-one;
3,3-bis(4-pyridinylmethyl)-2,3-dihydro-1-phenyl-1H-indene-1,2-diodiacetate dihydrochloride;
3,3-bis(4-pyridinylmethyl)-2(3H)-benzofuranone dihydrochloride.
(b) those of Formula (III) where:
a is a double bond; and
X independently is CR 2 ; or
W, Y and Z independently are H or CH 3 ; or
Q is R 2 ; or
Het 1 and Het 2 are as preferred for compounds of Formula (I).
A specifically preferred compound of Formula (III)(b) where a is a double bond is: 1,1-bis(4-pyridinyl-methyl)-3-phenyl-1H-indene-bis-methanesulfonate.
(c) those of Formula (III) where:
a is a single bond; and
X and Y are taken together; and
Q is ═O, ═S, H 2 , ═CR 1 R 2 , or C(R 1 )OR 3 ; or
W and Z are each H or OCH 3 ; or
Het 1 and Het 2 are as preferred for compounds of Formula (I).
Specifically preferred compounds of Formula (III)(c) are:
2,2-bis(4-pyridinylmethyl)-1(2H) acenaphthylenone dihydrochloride;
4-((1,2-dihydro-2-methylene-l-(4-pyridinylmethyl)-1-acenaphthylene-1-ylmethyl)) pyridine dihydrochloride.
Preferred compounds of Formula (IV) are:
(a) those of Formula (IV) where:
A is a single bond, and X and Y are taken independently; and
a and b are single bonds; or
Q is ═O, ═S, ═CR 1 R 2 , H 2 or C(R 1 )OR 3 ; or
X is CR 1 R 2 , O, or NR 3 ; or
V is --CH 2 --, CQ, or CR 1 ; or
W, Y and Z each is H or OCH 3 ; or
Het 1 and Het 2 are as preferred for compounds of Formula (I); or
R 1 is H, CH 3 or phenyl; or
R 2 is H; or
R 3 is H or ##STR24##
Specifically preferred compounds of Formula (IV) (a) where a and b are single bonds are:
1,1-bis(4-pyridinylmethyl)-2-(1H)-naphthalenone;
4,4-bis(4-pyridinylmethyl)-2-phenyl-1,3(2H, 4H)-isoquinolinedione.
(b) those of Formula (IV) where:
A is a single bond, and X and Y are taken independently; and
a is a single bond and b is a double bond; or
Q is H 2 or ═O; or
X is N or CR 2 ; or
V is CR 2 ; or
W, Y and Z each is H or OCH 3 ; or
Het 1 and Het 2 are as preferred for compounds of Formula (I); or
R 2 is H or phenyl.
A specifically preferred compound of Formula (IV) (b) where a is a single bond and b is a double bond is: 4,4-bis(4-pyridinylmethyl)-3,4-dihydro-6,7-dimethoxy-1-phenyl isoquinoline.
(c) those of Formula (IV) where:
A is a single bond, and Y and V are taken together, and b is a single bond; and
a is a single bond; or
Q is ═O, ═S, ═CR 1 R 2 , or C(R 1 )OR 3 ; or
X is CR 1 R 2 , O, or NR 3 ;
W and Z each is H or OCH 3 ; or
Het 1 and Het 2 are as preferred for compounds of Formula (I); or
R 1 is H, CH 3 or phenyl; or
R 2 is H; or
R 3 is H, ##STR25## or phenyl.
A specifically preferred compound of Formula (IV) (c) where a is a single bond is: 3,3-bis(4-pyridinylmethyl)-naphtho[1,8-b,c]pyran-2-one.
(d) those of Formula (IV) where:
V and X are taken together, and a is a single bond, and b is a double bond; and
A is (CH 2 ) n , (CH 2 ) n --X where X is O, S, SO 2 , ##STR26## or NH 3 where R 3 is H, alkyl of 1-3 carbon atoms or acyl, and n is 0, 1 or 2; or
Q is ═O, ═S, ═CR 1 R 2 , or C(R 1 )OR 3 ; or
W, Y and Z each is H or OCH 3 ; or
Het 1 and Het 2 are as preferred for compounds of Formula (I); or
R 1 is H, CH 3 or phenyl; or
R 2 is H; or
R 3 is H or ##STR27##
A specifically preferred compound of Formula (IV) (d) is: 11,11-bis(4-pyridinylmethyl)-5H-dibenzo[a,d]cyclohepten-10(11H)-one dihydrochloride.
DETAILED DESCRIPTION OF THE INVENTION
Synthesis
Most of the oxindole compounds of this invention are prepared by the synthetic sequence represented by Scheme 1. ##STR28## X, Y, p, R, --Het 1 , and --Het 2 are as defined above, D represents a displaceable group such as halogen (I, Br, Cl, or F) or methanesulfonate or p-toluenesulfonate. The reactions result from formation of an anion at the 3-position of the oxindole of Formula (2) by reaction of the oxindole with a suitable base followed by displacement of D by the anion and formation of the 3-mono-substituted compound (3). This mono-substituted product (3) can then either be isolated prior to the next step or, preferably, especially when --Het 1 and --Het 2 are the same, treated again with another equivalent of base without prior isolation, to give the 3,3-disubstituted oxindole (4).
Suitable bases for forming the anion include sodamide, lithium diisopropylamide, sodium hydride, potassium tert-butoxide, sodium alkoxide, potassium alkoxide, lithium alkoxide, potassium hydride, lithium 2,2,6,6-tetramethylpiperidide, butyl lithium, sec-butyl lithium, tert-butyl lithium, and lithium, sodium or potassium hexamethyldisilazide. The reaction is run in an aprotic solvent, generally in an ether such as diethylether, glyme, tetrahydrofuran or dioxane. However, if the oxoindole is soluble in a nonpolar solvent, the reaction may be run in a hydrocarbon such as hexane, heptane, cyclohexane, methylcyclohexane, benzene or toluene.
In running the reaction, the oxindole is dissolved in an appropriate solvent, and, depending upon the strength of the .base, the solution is cooled to a temperature between -40° C. and room temperature. When a more reactive base such as lithium diisopropylamide (LDA) is used, the solution is cooled to a temperature of -30° C. and a solution of the LDA in an appropriate solvent, such as tetrahydrofuran, is added dropwise over a period of 15 minutes to one hour, while maintaining the temperature at approximately -30° C.
If one chooses to use sodamide instead of LDA, benzene is the preferred solvent. The sodamide is added to a solution of the indolinone in benzene at room temperature. In order to drive the reaction to completion, the solution is refluxed until ammonia can no longer be detected evolving from the reaction.
A solution of the electrophile D--CH 2 -Het 1 is then added to the indolinone anion. Again, if a very reactive base such as LDA is used to generate the anion, the reaction is cooled to -30° C. and the electrophile is added dropwise. If a less active base is used to generate the anion, the electrophile is added at a temperature between 0° C. and room temperature and then the reaction mixture is refluxed.
The bisubstituted product (4) can be prepared by generation of a second anion at the three position of the indolinone. The anion formation followed by alkylation can be done in the same manner as described above for the preparation of a mono-substituted compound of Formula (3).
Instead of running the reaction sequentially, one may at tines, add two equivalents of base to the indolinone, followed by two to three equivalents of the alkylating agent. In some cases, especially those where --Het 1 is the same as --Het 2 , it may be convenient to accomplish alkylation of the oxindole under phase transfer conditions, e.g., using a base such as sodium hydroxide dissolved in water, a water immiscible solvent such as benzene or toluene, a phase transfer catalyst such as benzyltriethylammonium chloride and two molar equivalents of the alkylating agent D--CH 2 --Het 1 . Under such conditions, vigorous stirring and elevated reaction temperatures, e.g., 60°-80° C., may facilitate conversion to the 3,3-dialkylated oxindole.
When the reaction is complete as evidenced by thin layer chromatography, excess anion is decomposed with saturated ammonium chloride solution, and the reaction is taken through an acid-base cycle to remove neutral starting materials. Purification of the basic product generally involves conventional purification techniques such as flash chromatography followed by recrystallization if necessary. The pure base (one spot on thin layer chromatography and analytical HPLC) is converted to the dihydrochloride by adding a slight excess of 25% hydrochloric acid in a solvent such as ethanol. Generally, adding an equal volume of acetone to the boiling solution affords a crop of pure colorless crystals upon cooling. Other methods that will be. obvious to one skilled in the art can be used to obtain a crystalline product. The hydrochloride salt can be recrystallized from isopropanol, 1-propanol, ethanol, 95% ethanol, methanol, or mixtures of an alcohol with acetone, ethyl acetate, isopropyl acetate, or acetonitrile.
The hydrochloride salt can be converted to the corresponding free base by treatment with an inorganic base, e.g., sodium hydroxide, potassium hydroxide, sodium phosphate, ammonium hydroxide, or potassium carbonate, and then can be taken up in an organic solvent such as methylene chloride, ether, or ethyl acetate, and reprecipitated as a salt with some other pharmacologically acceptable acid such as maleic acid, methanesulfonic acid, napthalene-2-sulfonic acid, tartaric acid, hydrogen bromide, etc.
Alternatively, thallium (I) ethoxide can be used as the base as illustrated by Scheme 2. The indolinone is dissolved in a suitable solvent, preferably warm benzene, and an equimolar quantity of thallium (I) ethoxide is added rapidly to it. The organothallium compound (5) which precipitates out as a poisonous, yellowish, crystalline stable solid, is filtered affording the thallium compound in yields of 85-95%. Care must be exercised in handling thallium compounds because of their toxicity. ##STR29##
Organothallium compounds generally react with electrophiles to form the monoalkylated products. However, with very reactive electrophiles such as picolyl chlorides, benzyl bromide or the like, the 3,3-bis-alkylated products are obtained, as shown in Scheme 2, and as is exemplified by Example 1.
The thallium indoline (5) is heated with an electrophile such as picolyl chloride in an inert solvent, such as benzene or toluene, at 30° C. to the boiling point of the solvent, for several hours to 24 hours. Preferred is a temperature of 80° C. for 24 hours. When the reaction is complete as indicated by thin layer chromatography and the precipitated thallium chloride is filtered off, the remaining organic solution is taken through an acid-base cycle and purification, and optional salt formation is carried out as described above.
Preparation of the starting oxindole (2) represented in Scheme 1 and Scheme 2 can be carried out by one or more of a large number of general synthetic methods described in the chemical literature. For instance the reaction of an N-substituted aniline (6) with chloroacetyl chloride to form an amide (7) is a well known reaction. This is illustrated in Scheme 3. ##STR30##
Requisite diarylamine syntheses (6; where p=0, R=substituted phenyl) are widely known in the chemical literature. Many involve conversion of N-arylphenyl-enediamine by diazotization and for example Sandmeyer reaction with the appropriate substituted diarylamine. Again, one skilled in the art of organic synthesis can select a suitable synthesis for preparation of the appropriate diarylamine required to extend the Examples to the related compound of this invention. Recent useful syntheses include those described by Katritzsky et al., J. Chem Soc., Perkin. Trans. I, 2611 (1983), Gorwin et al., Chem. Commun., 4, 238 (1985), and Malz et al. in U.S. Pat. No. 4,431,841A (1984).
Other N-substituted anilines (6; where p=1) can be made by conventional synthetic methods commonly used in organic chemistry, e.g., by reaction of a suitable carboxylic acid chloride with an aniline to afford an amide which is then reduced by lithium aluminum hydride or diborane in tetrahydrofuran at about 67° C. to afford the N-substituted aniline (6), as depicted in Scheme 4 below. ##STR31##
The starting oxindole (2) can then be prepared by Friedel-Crafts ring closure of an amide of Formula (7) in the presence of a Lewis acid such as aluminum chloride (AlCl 3 ). Other Lewis acids such as tin tetrachloride (SnCl 4 ) or boron trifluoride (BF 3 ) can be used depending on the chemical structure of the amide (7). Choice of solvent if any is dependent on the actual compound of Formula (7) to be cyclized and on the Lewis acid used. Nitrobenzene, tetrachloroethane, ethylene dichloride and methylene chloride are often used as solvents. Generally, the use of AlCl 3 without a solvent is preferred.
If substituents X and Y are electron withdrawing and deactivate the aronmatic ring to which they are attached towards electrophilic substitution and if V and W are electron donating or activate the ring (where R is substituted phenyl) other methods may be more convenient for synthesis of oxindoles (2). These methods will be known to one skilled in the art of organic synthesis who is familiar with the literature of oxindole synthesis.
For example, in addition to the Friedel-Crafts cycloalkylation illustrated by Scheme 2, X and Y substituted oxindoles can be made by the general "azasulfonium ion" rearrangement methods of Gassman [U.S. Pat. Nos. 3,897,451 (1975), 3,996,264 (1976), and 3,972,894 (1976); see also J. Am. Chem. Soc., 96, 5512 (1974) etc.] or in some instances from o-nitrophenyl acetic acid [see Walker, J. Am. Chem. Soc., 77, 3544 (1955) and Hardigger et al., Helv. Chim. Acta., 39, 514 (1956)].
Compounds of the Formula (4) are preferably prepared as shown in (Scheme 5 ) by reaction of a substituted isatin (8) with an alkyl pyridine, such as 4-picoline, in acetic acid at 120°-130° C. to yield the aldol addition product (9). The reaction can also be performed in 4-picoline and the product isolated via dilution with methylene chloride followed by filtration and recrystallization of the product. Other high boiling solvents such as xylene or toluene containing an excess of 4-picoline may also be used for this reaction. Substituted isatins (8) are well described in the literature. 1-Phenyl isatin is prepared from diphenylamine and oxalyl chloride as described in Ber. 46, 3915 (1914). Condensation of alkyl pyridines with carbonyl compounds is described in E. Klingsberg, et.al., Pyridines and Its Derivatives, Pt. II, 191-197 (1961). ##STR32##
Dehydration of (9) to produce (10) preferably is executed with acetic anhydride between 100°-130° C. This reaction can also be performed in the presence of acetic acid. Other aprotic solvents such as toluene or xylene at elevated temperatures may also be used for the above transformation. Other methods of dehydration familiar to one skilled in the art include zinc chloride, other acid anhydrides, phosphorus pentoxide, potassium bisulfate, and sulfuric acid as described in J. March, Advanced Organic Chemistry, 901-903, (1985). Dehydration of carbinols (9) resulting from the condensation of alkyl pyridines with carbonyl compounds is described in E. Klingsberg, et al., Pyridine and Its Derivatives, Pt. II, 203 (1961).
Compounds of the Formula (3) are obtained via reduction of (10). Treatment of (10) with sodium borohydride in methanol is the preferred method for conversion of (10) to (3). This method is illustrated in J. Org. Chem., 31, 620 (1966). (3) may also be obtained via transfer hydrogenation as described in Chem. Rev., 85, 129-170 (1985) or via catalytic hydrogenation in acetic acid or ethyl acetate under standard conditions known to one skilled in the art.
The conversion of (3) to (4) is preferably performed in a methanol-water mixture using sodium hydroxide as the preferred base, followed by the reaction of the resultant anionic species with a compound of the formula D--CH 2 --Het 2 where D is preferably halogen, methanesulfonate or p-toluenesulfonate. Other alcohols such as ethanol, isopropanol, n-propanol can be substituted for methanol as described above. Other bases such as potassium hydroxide, lithium hydroxide, and quaternary amines such as N-benzyltrimethyl ammonium hydroxide are also acceptable. Preparation of (4) from (3) can also be accomplished under phase-transfer catalysis using toluene-50% sodium hydroxide as the solvents and hexadecyltributyl phosphonium bromide as the catalyst.
Other more direct synthesis of 3,3-disubstituted 2-oxindoles can be carried out by use of the Brunner reaction of N-arylhydrazides [Org. Synthesis, 37, 60 (1957); Rohrscheidt et al., Liebigs Ann. Chem., 680 (1978)] and by processes involving direct oxidation of substituted indoles [Lawson et al., J. Org. Chem., 26, 263 (1961); R. L. Hinman et al., ibid, 29, 1206 (1964); Lawson et al., J. Am. Chem. Soc., 82, 5918 (1960); Szabo-Pusztag et al., Synthesis, 276 (1979). Other methods for making oxindoles are described by A. P. Kozikowski, et al., J. Am. Chem. Soc., 43 (10), 2083 (1978); T. Nakashima, et al., Chem. Pharm. Bull., 17 (11), 2293 (1969); Y. Tamura, et al., Synthesis, 534 (1981); J. F. Bunnett, J. Org. Chem., 28 (1), 1 (1963); R. R. Goehring, J. Am. Chem. Soc., 107 (z), 435 (1985); T. Hamada, et. al., Chen. Pharm. Bull., 29 (1), 128 (1981); D. Ben-Ishai, et al., Tet. Lett., 21 (6), 569-72 (1980); J. F. Wolfe, J. Am. Chem. Soc., 112 (10), 3646 (1980); J. G. Atkinson, Tet. Lett., (31), 3857 (1979); M. Mori, et al., Tet. Lett., (21) 1807 (1976); P. Parimoo, Indian J. Chem., 10 (17), 764 (1972); D. Klamann, et al., Chem Bet., 100 (6), 1870 (1967).
This bibliographic list is intended to be illustrative of the great variety of methods available to make the 2-oxindole intermediates useful in this invention.
The 2-thiooxindoles (11) of this invention can be made by reaction of the oxindoles with Lawesson's reagent or with phosphorus. pentasulfide (P 4 S 10 ) as is illustrated in Scheme 6. ##STR33##
Lawesson reagent is 2,4-bis (4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide. Its use in the thiation of carboxamides and lactams is well known, as is the use of phosphorus pentasulfide for similar reactions. The reactions are customarily carried out in methylene chloride, benzene, toluene, acetonitrile, or piperidine depending on the solvent power and reaction temperature required for the particular oxindole involved. Usually the P 4 S 10 works better if it is first purified by extraction into methylene chloride by Soxhlet extraction. Ordinarily thiation reactions can be carried out at mild temperatures (25°-80° C.) and the products can be isolated by chromatography or crystallization.
The nitrogen-containing heterocyclic compounds D--CH 2 --Het 1 used as intermediates in Schemes 1 and 2 are available by methods described in standard works on heterocyclic chemistry such as Katritzsky and Rees, Comprehensive Heterocyclic Chemistry, Vols. 2-5, Pergamon Press, N.Y., 1984. In some instances the preparation of the corresponding hydroxy compounds (D=OH) is described in the literature; these can be converted to the corresponding halo compounds (e.g. D=Br) for the alkylation reaction indicated in Schemes 1 and 2 by mild reagent (such as Ph 3 P,CBr 4 ). Alternatively the hydroxy compounds can be converted to the corresponding sulfonate esters (e.g. D=CH 3 SO 2 O) by reaction with the corresponding sulfonylchloride in the presence of pyridine or triethylamine at cold temperatures. Generally, temperatures of about 0° C. to -20° C. are preferred for formation of these sulfonates.
Compounds of the Formula (14) (Scheme 7), particularly where Het 1 is the same as Het 2 , can be prepared by treatment of indene (12) with a suitable base followed by displacement of D by the resultant anion forming the 3-substituted indene (13). Indene (13) can then either be isolated prior to the next step or treated again with another equivalent of base and alkylating reagent without prior isolation to give the 3,3-substituted indene (14). D in DCH 2 Het 1 represents a displaceable group as described in Scheme 1.
Suitable bases for forming the anion include those described for Scheme 1. The reaction is run in an aprotic solvent such as diethylether, glyme, tetrahydrofuran, or dioxane.
In addition to the bases listed previously, other suitable bases are n-butyllithium, tert-butyllithium, sec-butyllithium, methyllithium, and phenyllithium. Starting material (12), where W, Z=H, Q=H, and R 2 =Ph, can be prepared via addition of phenylmagnesium bromide to 1-indanone, followed by dehydration, Parham and Wright J. Org. Chem., 22, 1473 (1957).
Other general methods for the preparation of indenes are described in the chemical literature, Parham and Sayed, Synthesis, 116-7 (1976); Greifenstein, et. al., J. Org. Chem., 46, 5125-32 (1981). ##STR34##
Compounds of the formula (16) (Scheme 8), where Q and R 2 are described above, can be prepared via catalytic reduction of the multiple bend in olefin (14) with hydrogen in the presence of a catalyst such as palladium on carbon (15) or platinum on carbon. This method is limited to compounds in which R 2 , W or Z is not NO 2 . Other methods of reduction my be found in House, H. O., Modern Synthetic Reactions, second edition, W. A. Benjamin, Inc., Menlo Park, Calif., 1972. ##STR35##
Compounds of the formula (18) and (19) can be prepared using the methods outlined in Scheme 9. Hydroxylation of the double bond in indene (17) is conveniently achieved with osmium tetroxide, either stoichiometrically or catalytically in the presence of an oxidant such as hydrogen peroxide or N-methyl morpholine-N-oxide, Schroder, Chem. Rev. 80, 187 (1980). The diol (18) can be further elaborated into the esters or ethers (19) via methods described in the chemical literature. ##STR36##
Compounds of the formula (24) can be prepared using the sequence outlined in Scheme 10. The 2-methoxy-phenyl acetonitrile (20) can be dialkylated with D--CH 2 -Het 1 and D--CH 2 --Het 2 via the general methods described for Scheme 1. Het 1 and Het 2 may be different or the same. If they are the same, the phase-transfer technique described for Scheme 5 is the most convenient method to prepare compounds of the formula (22). The nitrile group in (22) is subsequently hydrolyzed to the acid (23) using basic conditions available in the chemical literature. Lactonisation to compound (24) is achieved by demethylation of (23), followed by dehydration. Demethylation reagents include boron tribromide, Benton and Dillon, J. Am. Chem. Soc., 64, 1128 (1942), McOmie and Watts, Chem. Ind., 1658 (1963); mercaptide ions, Vowinkel, Synthesis, 430 (1974); or acids such as hydrogen chloride, hydrogen bromide, and hydrogen iodide, Fieser and Fieser, Reagents for Organic Synthesis, Vol. 1-12, Wiley, 1967-1986. This method is limited to compounds in which W or Z is not CN or OR 3 . ##STR37##
Compounds of the formula (27), where n is 1 or 2, may be prepared as outlined in Scheme 11, using the reagents and conditions previously described for Scheme 1. ##STR38##
The ketone group in compound (27) can be elaborated to the derivatives as shown in Scheme 12. Compounds of the formula (28) can be prepared via treatment of the ketone (27) with a reagent such as an alkylidene triarylphosphorane (32) (the Wittig reaction) yielding the olefin (28). Olefin (28) can be reduced via catalytic hydrogenation in the presence of a catalyst such as palladium on carbon, or platinum on carbon to yield (29). Compounds of the formula (30) can be prepared via reduction of the ketone with a hydride reagent such as sodium borohydride. Subsequent treatment of alcohol (30) with an acid chloride, or formation of the alkoxide followed by treatment with an alkylating reagent, produces the ester or the ether (31), respectively.
Other ketone derivatives such as oximes, ketals, acetals, thioketals, thioacetals, thioketones, etc., can be prepared via methods described in the chemical literature. The ketone function in (27) can also be reduced to the methylene compound with hydrazine by methods described by Hudlicky, Reductions in Organic Chemistry; Halsted Press, NY, 1984, or converted into the geminal difluoride with diethylaminosulfur trifluoride as described by W. J. Middleton, J. Org. Chem., 40, 574 (1975). Other Ketone derivatives are available to anyone skilled in the art. ##STR39##
Compounds of formula (36), particularly where Het 1 is the same as Het 2 , can be prepared by the synthetic sequence represented by Scheme 13. D represents a displaceable group as described for Scheme 1. Ketone (34) can be prepared via the oxidation of the alcohol (33) with a chromium salt. An example of this technique is reported by E. J. Corey et al., Tetrahedron Letters, 2467 (1975). The alkylations result from formation of an anion at the 2-position of the ketone (34) by treatment of the ketone with a suitable base followed by displacement of D by the anion and formation of the 2-mono-substituted ketone (35).
Suitable bases and solvents used for forming the anion include those described for Scheme 1. This mono-substituted ketone (35) can then either be isolated prior to the next step or treated again with another equivalent of base and alkylating reagent without prior isolation, to give the 2,2-disubstituted acenaphthenone (36).
In some cases, especially those where Het 1 and Het 2 are the same, it may be convenient to accomplish alkylation of the acenaphthenone under phase-transfer conditions, e.g., using a base such as sodium hydroxide dissolved in water, a water immiscible solvent such as benzene or toluene, a phase transfer catalyst such as benzyltriethylammonium chloride and two molar equivalents of the alkylating agent D-CH 2 -Het. Suitable procedures are described by Stark and Liotta; Phase Transfer Catalysis. Principles and Techniques; Academic Press: N.Y., 1978. Under such conditions, vigorous stirring and elevated reaction temperatures, e.g., 50°-80° C., may facilitate conversion to the 2,2-dialkylated acenaphthenone.
Purification of the product generally involves column chromatography followed by recrystallization if necessary. The pure material can be converted to the hydrochloride salt if desired. ##STR40##
An alternative method of synthesis is illustrated by Scheme 14. Aldol condensation of ketone (34) with the appropriately substituted aldehyde (39) under basic conditions yields the unsaturated ketone (37). An example of this conversion is described by O. Tsuge et al., Bulletin of the Chemical Society of Japan, 42, 181-185 (1969). Catalytic reduction of the multiple bond in ketone (37) is performed with hydrogen in the presence of a catalyst such as palladium on carbon. Alkylation of the intermediate ketone with an equivalent of D--CH 2 --Het 2 under the conditions described above or other standard methods described in the chemical literature yield the ketones (38). The required heterocyclic aldehydes (39) are either available commercially, or may be prepared using techniques and methods reported in the chemical literature. ##STR41##
Compounds of the formula (40), where R 1 and R 2 are as described above, can conveniently be prepared via the method shown in Scheme 15. Treatment of ketones (36) with a reagent such an as alkylidene triarylphosphorane (32) (the Wittig reaction) provides the olefins (40). This method is limited to compounds where W or Z is not COR 1 . When R 1 and R 2 are not H, the Z or the E isomer, or a mixture of the two, may be obtained from these reactions. ##STR42##
Compounds of the formula (41), where R l and R 2 are described above, can be prepared via catalytic reduction of the multiple bond in olefin (40) with hydrogen in the presence of a catalyst such as palladium on carbon, or platinum on carbon (Scheme 16). This method is limited to compounds in which W or Z is not NO 2 . Other methods of reduction can be found in House, H. O., Modern Synthetic Reactions, second edition, W. A. Benjamin, Inc., Menlo Park, Calif., 1972. ##STR43##
Compounds of the formula (43), where R 3 is as described above, may be obtained via the methods shown in Scheme 17. Reduction of the ketone (36) with a hydride reagent such as lithium aluminum hydride provides the alcohol (42). Treatment of (42) with an acid chloride, or formation of the alkoxide followed by treatment with an alkylating reagent, produces the ester or the ether, respectively. ##STR44##
Compounds of the formula (49) are prepared using the sequence outlined in Scheme 18. The substituted phenylacetonitrile (44 ) can be dialkylated with D--CH 2 --Het 1 and D--CH 2 --Het 2 via the general methods described for Scheme 1. Het 1 and Het 2 may be different or the same. If they are the same, the phase-transfer technique described for Scheme 5 is the most convenient method to prepare compounds of the formula (45). The nitrile group in (45) is subsequently reduced to the amine (46) as described by C. Kaiser and P. A. Dandridge, et. al., J. Med. Chem. 28, 1803 (1985), or by similar methods outlined in the chemical literature. The amine (46) is converted into the amide (47) using an acid chloride or acid anhydride. Conversion to the dihydroisoquinoline (48) is accomplished using phosphorus oxychloride or other reagents known to affect Bischler-Napieralski cyclization; W. M. Whaley and T. R. Govindachari, Org. Reactions 6, 74 (1951). Catalytic reduction over palladium or platinum provides compounds of the formula (49). ##STR45##
Compounds of the formula (49) can also be prepared as outlined in Scheme 19. Condensation of amine (46) with an aldehyde under Pictet-Spengler reaction conditions; W. M. Whaley and T. R. Govindachari, Org. Reactions 6, 151 (1951), Abramovich, Adv. Heterocyclic Chen. 3, 79 (1964), Stuart, et. al., Meterocycles 3, 223 (1975) will produce compound (49). ##STR46##
Compounds of the formula (50) are prepared by treating (49) with an acid anhydride or an acid chloride (Scheme 20) as previously described for Scheme 17. ##STR47##
Compounds of the formula (55) can be prepared using the sequence outlined in Scheme 21. The benzyl amine starting material (51) can be prepared from the corresponding benzaldehyde, through reduction to the benzyl alcohol followed by conversion to the benzyl halide and amination with dimethylamine. Alternatively, (51) can be prepared via a Mannich reaction directly on the aromatic substrate with formaldehyde and dimethylamine; F. F. Blicke, Org. Reactions 1, 303 (1942). Amine (51) can be converted into protected benzyl alcohol (52) through treatment with a strong base, such as butyllithium or lithium diisopropylamine, addition of formaldehyde, and introduction of a protecting group such as trimethylsilyl or 2-tetrahydropyranyl. Compound (52) can then be converted into the phenylacetonitrile (53) via treatment with ethyl chloroformate followed by potassium cyanide; R. S. Mali, et al., Indian J. Chem. 25B, 256 (1986). Compound (53) is then dialkylated with D--CH 2 --Het 1 and D--CH 2 --Het 2 via the general methods described for Scheme 1. Hydrolysis of the resulting product (54), followed by deprotection of the alcohol group provides compounds of the formula (55). ##STR48##
Compounds of the formula (56) can be prepared by treating (55) with a primary amine. Heat is usually required for this transformation (Scheme 22). ##STR49##
Compounds of the formula (60) can be prepared according to the sequence outlined in Scheme 23. Treatment of (51) with a strong base such as butyllithium or lithium diisopropylamine, followed by ethyl chloroformate provides (57). This compound is then carried through the same series of reactions described in Scheme 22 to produce anhydrides (60). ##STR50##
Compounds of the formula (61) can be prepared by heating anhydrides (60) with a primary amine (Scheme 24). ##STR51##
Compounds of the formula (60) can also be prepared according to Scheme 25. Hydrolysis of the nitrile (58) provides arthydride (62), which is then dialkylated with D--CH 2 --Het 1 and D--CH 2 --Het 2 via the general methods described for Scheme 1. ##STR52##
Compounds of the formula (61) are also prepared according to Scheme 26. Treatment of arthydride (62) with a primary amine produces imide (63); Ueda, et. al, J. Polym. Sci., Polym. Chem. Ed. 17, 2459 (1979). This compound is dialkylated with D--CH 2 --Het 1 and D--CH 2 --Het 2 Via the general methods described for Scheme 1. ##STR53##
Compounds of the formula (64) can be prepared via reduction of the nitrile portion of compound (59), followed by hydrolysis of the ester and ring closure (Scheme 27). ##STR54##
Compounds of the formula (65) can be prepared according to Scheme 28. Treatment of tetralone (27, n=2) with bromine, followed by dehydrohalogenation with collidine produces naphthalenones (65).; Marvell and Stephenson, J. Am. Chem. Soc. 77, 5177 (1955). The compounds may also be prepared via the sequence described in Scheme 23. 2-Naphthols (66) can be treated with a strong base such as lithium tert-butoxide in the presence of alkylating agent: D--CH 2 --Het 1 produce (65); Bram, et. al., J. Chem. Soc. Chem. Commun., 325 (1980), Bram, et. al., Tetrahedron Lett. 25, 5035 (1984). This method seems to be limited to those cases where Het 1 and Het 2 are the same. ##STR55##
Derivatives of (65) can be prepared via the general reactions described in Scheme 30. Treatment of (65) with Lawesson's reagent provides thioketone (67); Rao and Ramamurthy, J. Org. Chem. 50, 5009 (1985 ). Treatment of (65) with a phosphonium ylid or similar compound produces olefin (68). Reactions of this type are well known in the chemical literature. Alternatively, (68) can be prepared from (65) via an aldol-type reaction with, e.g. a nitroalkane, alkylcyanide, or alkyl ester. Compounds of the formula (69) can be prepared via reduction of the ketone with diisobutylaluminum hydride; Mathur, et. al., Tetrahedron 41, 1509 (1985). The alcohol may be converted into the ester (70) via methods described previously for Scheme 17. ##STR56##
Compounds of the formula (72) are prepared according to Scheme 31. Lactone (71) is prepared from the acenaphthenone according to O'Brien and Smith, J. Chem. Soc. 2907-17 (1963). This compound is dialkylated with D--CH 2 --Het 1 and D--CH 2 --Het 2 via the general methods described for Scheme 1. A phase transfer method described by Chan and Huang, Synthesis, 452 (1982) proved to be particularly useful in cases where Het 1 and Het 2 are the same.
Compounds of the formula (75) can be prepared. according to Scheme 32. Amide (73) can be prepared from the acenaphthenone according to O'Brien and Smith, J. Chem. Soc. 2907-17 (1963). Alkylation or arylation on nitrogen provides (74); Renger, Synthesis, 856 (1985). This compound is then dialkylated with D--CH 2 --Het 1 and D--CH 2 --Het 2 via the general methods described for Scheme 1. ##STR57##
Compound of the formula (77) can be prepared according to Scheme 33. Phenalenes (76) are prepared according to the literature; Bauld, et. al., Tetrahedron Lett., 2865 (1979), Jorgensen and Thomsen, Acta Chem. Scand. B 38, 113 (1984). This compound is then dialkylated with D--CH 2 --Het 1 and D--CH 2 --Het 2 via the general methods described for Scheme 1. The ketone group in (77) can be converted into the thioketone, olefin, alcohol, or ester according to Scheme 30 or by other methods described in the chemical literature. Other ketone derivatives are available to anyone skilled in the art.
Compounds of the formula (78) and (79) can be prepared according to Scheme 34. Treatment of (77) with base, followed by addition of an alkylating agent such as methyl iodide, ethyl iodide, etc. produces enol ether (78). Addition of an organometallic species such as phenylmagnesium bromide to (77), followed by dehydration, provides olefin (79).
Compounds of the formula (81) can be prepared according to Scheme 35. The ketones (80) can be dialkylated with D--CH 2 --Het 1 and D--CH 2 --Het 2 via the general methods described for Scheme 1. The starting materials are prepared via literature methods: --A-- is --CH 2 -- or --CH 2 CH 2 --, Leonard, et al., J. Am. Chem. Soc. 77, 5078 (1955);--A-- is --O--, Ikuo, et al., Chem. Pharm. Bull. Japan 23, 2223 (1975), Protiva, et al., Coll. Czech. Chem. Commun. 34, 2122 (1969); --A-- is --S--, Protiva, et al., Monatsh. Chem. 96, 182 (1965), Kimoto, et. al., Yakugaku Zasshi 88, 1323 (1968), Protiva, et. al., Coll. Czech. Chem. Commun. 34, 1015 (1969); --A -- is --NR 3 --, Allais, et al., Eur. J. Med. Chem.--Chem. Ther. 17, 371 (1982), Schindler and Blattner, U.S. Pat. Nos. 3,144,400 and 3,130,191. The ketone group in (81) can be converted into the thioketone, olefin, alcohol, or ester according to Scheme 30 or by other methods described in the chemical literature. Other ketone derivatives are available to anyone skilled in the art. ##STR58##
Compounds of the Formula (83)(Scheme 36) can be prepared from anthra-9,10-quinones (82) by catalytic reduction with nickel or chemical reduction with tin, tin chloride, iron, aluminum or copper in sulfuric, hydrochloric, and acetic acid as described in Chem. Berichte 20, 1854 (1887); Ann. 379, 55 (1911); Chem. Berichte, 58, 2675 (1925), and Bull, Soc. Chem. France [4], 33, 1094 (1923).
The following Schemes 36-63 show the preparation of core ring structures with active methylene sites (compounds 83, 86, 87, 89, 91, 97, 100, 102, 116, 121, 124, 127, 128, 130, 131, 133). These compounds are then alkylated via the methods described for Scheme 1. ##STR59##
Compounds of the formula (83) can also be prepared via ring closure of benzyl benzoic acids (84) under Friedel-Crafts conditions (Scheme 37) as described by the following: Ann., 234, 235 (1886); U.S. Pat. No. 2,053,430; J. Org. Chem., 23, 1786 (1958); U.S. Pat. No. 2,174,118. ##STR60##
Alkyl and halogen substituted arthrones can be prepared via reduction of the corresponding anthraquione. 1-Chloro-9,10-anthraquinone (85) is reduced to 1-chloroanthrone (87) via reduction with iron and iron chloride (Scheme 38) as described in German Pat. 249,124. 4-Chloroanthrone (86) is produced via reduction of (85) with aluminum in sulfuric acid as described in FLAT Final Report Nr, 1313 II, 105(1948). ##STR61## Other halo- and alkyl anthrones are described by the following: German Pat. 598,476; Ber., 66, 1876 (1933); J. Chem. Soc., 123, 2549 (1923).
Hydroxy-anthrones (89) are prepared from hydroxy-9,10-anthraquinones (88) by reduction with tin in acetic and hydrochloric acids (Scheme 39) as described in J. Am. Chem. Soc., 52, 4887 (1930) or by reduction with zinc (German Pat. 296,091; 301,452). Further hydroxy-anthrones are described by the following: Ann., 212, 28 (1882); Brit. Pat. 353,479. Scheme 39 ##STR62## Methoxy-anthrones are prepared as above via reduction of the corresponding anthraquinone described in J. Chem. Soc., 2726, (1949). Amino- and acetamido-anthrones are prepared via reduction of the corresponding anthraquinone (German Pat. 201,542).
Compounds of the Formula (91), can be prepared by the addition of ten parts methylene chloride to a mixture of fifteen parts biphenyl (90) and one part aluminum chloride as described by Adam, Annales de Chimie, [6], 15 235 Scheme 40). ##STR63##
Also, conversion of 2-aminodeiphenylmethane (92) to the corresponding diazonium salt and subsequent cyclization at elevated temperatures yields (91) (Scheme 41) (Ber, 27, 2787). ##STR64##
Halogenated derivatives of (91) are readily available. 2-chlorofluorene is prepared by heating the corresponding diazonium salt with cuprous chloride in concentrated mineral acid (Bull. Soc. Chem. France, [4], 41, 1626). Bromination of (91) in chloroform yields 2-bromfluorene (J. Chem. Soc. 43, 165, (1883). Iodination of (91) occurs by heating fluorene-2-diazonium iodide with cuprous iodide in hydroiodic acid (Bull. Soc. Chem. France, [4], 41, 1626). Nitration of (91) with nitric acid in acetic acid yields 2-nitrofluorene as described by Kuhn, Org. Syn., 13, 74, (1933).
Further nitration or halogenation of the above species may occur as described in Ann., [10], 14; J. Chem. Soc., 43, 170, (1883). Ann., [10], 14, 104 (1930). Reduction of nitrofluorenes with zinc in boiling alcohol-water mixtures yields the corresponding amino-fluorene as described by Diels, Ber., 34, 1759 (1901).
Carboxylated derivatives of (91) are known. Fluorene-2-carboxaldehyde is produced via treatment of (91) with hydrogem cyanide and aluminum chloride in chlorobenzene as described by Hinkel, J. Chem. Soc., 339, (1936). Treatment of (91) with acetic arthydride and aluminum chloride yields 2-acetylfluorene as described by Bochmann, J. Amer. Chem. Soc., 62, 2687(1940).
Compounds of the formula (91) may also be also be prepared by the reduction of fluorenone (93) (Scheme 42) with hydroiodic acid in the presence of phosphorus (Ber., 36, 213) or under standard Wolff-Kischner conditions using hydrazine in the presence of potassium hydroxide. ##STR65##
Treatment of fluorene with acetic arthydride and AlCl 3 in CS 2 yields 2-acetylfluorene, (Ray, J. Amer. Chem. Soc., 65 836 [1943]; Org. Synth., Coll. Vol. III, 23 [1955]; Bachmann, J. Am. Chen. Soc. 62, 2687-2688 [1940]Treating 2-nitrofluorene with acetylchloride and AlCl 3 in nitrobenzene at 40°-55° yields 7-nitro-2-acetylfluorene (Oehlschlaeger, J. Am. Chem. Soc. 71, 3223 [1949].
Fluorenone (93) is prepared in quantitative yield by treating diphenyl-2-carboxylic acid chloride (94) with AlCl 3 in benzene (Scheme 43) ##STR66## (Ann., 464, 33) or by treating it with phosphorus pentachloride (Bachmann, J. Am. Chem. Soc., 49, 2093) or thionylchloride (Bell, J. Chen. Soc., 3247 (1928).
Substituted fluorenones are prepared as follows: 1-bromofluorenone is prepared from 2,6-dibromobenzophenone (Rec. Trav. Chem., 32, 167). 2,4-Dibromobenzophenone yields 1,3-dibromofluorenone (Rec. Trav. Chem., 32, 173). Treating 9,9-Dichloro-2,7-dibromofluorene with PCl 5 at 210°-220° C. yields 2,7-dibromofluorenone (Annalen der Chemie, 387, 156). Treating 2,9,9-trichlorofluorene with water yields 2-chlorofluorenone (Ber., 54, 2073). Preparation of 2-nitrofluorenone is described in (Rec. Trav. Chem., 48, 897); (Annalen der Chemie, 43, 65). 4-Nitrofluorenone is described by Morgan, J. Chem. Soc., 2696, 1926. 1,8-Dinitrofluorenone is described by Huntress, J. Am. Chem. Soc., 54, 827, (1932 ). Preparation of 2,5-dinitrofluorenone by nitration is described by Morgan, J. Chem. Soc., 1926, 2696. 1,4-dimethylfluorenone is prepared from 2,5-dimethylbenzophenone-2-diazonium sulfate and copper powder (Ber., 53, 1395). 2-Fluorofluorenone is prepared by treating the 2-diazonium salt of fluorenone with HBF 4 and heating the tetrafluoroborate salt to 180° C. (Ber. 66, 46, S2 [1933]. 2-Chlorofluorenone is prepared from 4-chlorobiphenyl-2-carboxylic acid or from 4-chlorobiphenyl-2-carboxylic acid in conc. H 2 SO 4 at 50° C. (J. Chem. Soc., 113, (1950). Heating 4-Bromobiphenyl carboxylic acid with conc. sulfuric acid produces 2-bromofluorenone (J. Chem. Soc., 113, (1938). Treatment of 1-aminofluorenone with nitrous acid and potassium iodide yields 1-iodofluorenone J. Am. Chem. Soc., 64, 2845, (1942). The treatment of 4-nitrobiphenyl carboxylic acid with H 2 SO 4 yields 2-nitrofluorenone (J. Chem. Soc., 113, (1938), and 5-nitrobiphenyl carboxylic acid yields 3-nitrofluorenone (J. Chen. Soc., 70, 1492 [1948]). 7-Bromo-2-nitrofluorenone is produced from 9-bromofluorene and nitric acid (J. Chem. Soc., 1607, (1935). 2,5-dinitrofluorenone and 2,7-dinitrofluorenone are produced by nitric acid on fluorenone (J. Chem. Soc., 68 2489, [1946]). Treatment of 2-amino-3,4-dimethylbenzophenone with sodium nitrite in hydrochloric acid and warming the reaction yields 2,3-dimethylfluorenone (J. Chem. Soc., 63, 2564-2566 [1941]). Reacting 2-bromofluorenone with ammonium hydroxide in the presence of Cu(I)Cl yields 2-aminofluorenone (Bull. Soc. Chem. France, [4]41 61). Dimethylsulfate reacts with 2- aminofluorenone to produce 2,2-dimethylamino fluorenone (Monats., b 41, 209 ), and treatment with acetic arthydride produces 2-acetamido fluorenone (Monats., 41, 207). Treating 3-hydroxydiphenyl-2-carboxylic acid with H 2 SO.sub. 4 produces 1-hydroxy-fluorenone (Ber., 28, 113), and further reaction with methyliodide yields 1-methoxy fluorenone (J. fur prakt. Chem., 59 453). Prep of 4 cyanofluorenone is described (Ber., 47, 2825) and vacuum distillation of 2-cyanodiphenyl carboxylic acid chloride produce 4-cyanofluorenone (J. Chem. Soc., 3248, (1928). All other positional isomers may be prepared in a similar manner to those transformations described above.
Other fluorenone preparations are described by J. Fur. Prakt. Chem., [27]331; Comptes Rendue 184, 608; Ber., 53 2243; Bull. Soc. Chim. France, [43], 41 71; Annalen 436 5; (J. Chem. Soc., 1696, (1926); (J. Chen. Soc., 54, 827 (1932); (J. Chem. Soc., 2694, (1926); (J. Chem. Soc., 20, 3958, (1948); (J. Chem. Soc., 65, 836 (1943); (J. Chem. Soc., 62, 2687, (1940).
Azafluorenes (97) can be prepared via reduction of azafluorenones (96) by hydrogen iodide in the presence of phosphorus. Azafluorenones (96) are prepared by cyclization of 2-(2-phenylcarboxylic acid)-pyridine-3-carboxylic acid (95) (Scheme 44) as described in Monatsh., 4, 472; Ber., 23, 1237; J. Chem. Soc., 125, 2369. ##STR67##
Compounds of the Formula (100) are prepared by reacting substituted phenols (98) with formaldehyde (99) followed by cyclization with sulfuric acid (J. Fur Prakt. Chem., 54, 217 [1896]) (Scheme 45). ##STR68##
Alkylxanthenes are prepared by distillation of cresols (Ber. 49 169 [1916]). Treating 2'-chloro-2-hydroxy-5-methylbenzophenone (101) with hydrazine hydrate produces 2-methyl xanthene (102), (Scheme 46) (J. Am. Chem. Soc., 73, 2483 [1951]). ##STR69##
Xanthene (100) may also be prepared by reducing xanthen-9-ones with sodium or hydrogen iodide in the presence of red phosphorus (J. Chem. Sec., 812, (1956) or by Wolff-Kischner conditions as described in U.S. Pat. No. 2,776,299.
Xanthones (104) can be prepared by acid catalyzed cyclization of substituted-diphenylether-2-carboxylic acids (103) (Scheme 47). ##STR70## For example, 2-chloroxanthone is formed from heating 4 chlorodiphenylether-2carboxylic acid in sulfuric acid at 100° C. (Annalen. 355 366, 371 388). The haloisomers may be prepared in a similar manner (Annalen. 370 183, 371 389). Haloxanthones can be prepared by direct halogenation of xanthone as described in J. Chen. Soc., 109, 745 (1916).
Substituted xanthones can be prepared from substituted salicylic acids (105) and acetic anhydride (Scheme 48) and from treating substituted 2-hydroxybenzophenones (106) with a base such as sodium hydroxide (Scheme 49) (Ber., 38 1488, 1494, 39 2361; Ann., 254 284). ##STR71## Fluoroxanthones are prepared from 2-[fluorophenoxy]benzoic acids, (Tetrahedron, 6 315 [1959]). Haloxanthones may also be prepared from the xanthondiazonium salts (J. Chem. Soc., 1958 4234, 4238). Halo-substituted-xanthones can then be reduced to halo-xanthenes by lithium aluminum hydride, sodium in alcohol, and hydrogen iodide in the presence of red phosphorus, (J. Am. Chem. Soc., 77 5121, 5122 [1955]). Further preparations of haloxanthones are described J. Org. Chen., 28 3188, 3193 [1963]; J. Am. Chem. Soc., 77 543, 546 [1955]. Nitroxanthones can be prepared by direct nitration of xanthone or by cyclization of 2-(nitro-phenoxy)benzoic acid with sulfuric acid and acetic anhydride or phosphoryl chloride, J. Am. Chem. Soc., 56 120 [1934].
Aminoxanthenes can be prepared by reduction of nitroxanthenes or nitroxanthones with tin (II) chloride in hydrochloric/acetic acids, or metallic tin in acid, (J. Chen. Soc., 109 747). Acylation of the amino-xanthene or xanthones produces acylaminoxanthene or xanthones, J. Pharm. Soc. Japan, 74 610 [1954]. Hydroxy and alkoxyxanthenes (109) and xanthones are prepared by reacting salicyclic acid (107 ) with resorcinol (108) and zinc chloride 180° C. (Scheme 50). ##STR72## (J. Scient. Ind. Res. India, 13B 396, 398 [1954]) or by cyclizing alkoxyphenoxy benzoic acids (110) with tin (IV) chloride (Scheme 51) (Ber. 91 1801, 1803 [1958]). ##STR73## Ber. 81 19, 24 [1948]). Hydroxyxanthenes can be reacted with dimethylsulfate or alkyliodide to yield alkoxy-xanthenes (J. Am. Chen. Sec., 79 2225, 2229 [1957]. Cyanoxanthones (113) are prepared by ring closure of cyanophenoxybenzoic acid (112) (Scheme 52) (J. Chem. Soc., 4227, (1958). ##STR74##
Compounds of the Formula (116) can be prepared by reduction of thioxanthones (115) by sodium in alcohol, hydrogen iodide in the presence of phosphorus, and Wolff-Kishner conditions using hydrazine hydrate and ethylene glycol. Thioxanthones are prepared by cyclizing phenylmercaptobenzaldehydes (114) (Scheme 53). ##STR75## (J. Chem. Soc., 747, 1941). Haloxanthones can be prepared by cyclizing phenylmercaptobenzoic acids (117) with sulfuric acid (Scheme 54), to yield (118), (J. Org. Chen. Sec., 24 1914 [1959]). ##STR76##
Nitrothioxanthones are prepared in the same manner (J. Am. Chen. Soc., 69 1925, 1928 [1947]).
Similarly, amino-thioxanthones (120) can be reduced to aminoxanthenes (121). Aminothioxanthones (120) are prepared by cyclization of aminodiphenylsulfide-2-carboxylic acids (119) (Scheme 55) (Ber. 42, 3065). They are converted acetamido derivatives by well-known methods (Ber., 42, 3057). ##STR77##
Hydroxythioxanthones (123) are likewise prepared from S-hydroxy-substituted-phenylthiosalicyclic acids (122) with sulfuric acid (Scheme 56). ##STR78## Alkoxy substituted thioxanthones are prepared in the same manner from S-alkoxy substituted phenylthiosalicylic acids (J. Chem. Soc., 869 (1929). Thioxanthenes (124) are prepared by reducing thioxanthones with hydrogen iodide in the presence of red phosphorus.
Thioxanthon-S.S-dioxides (126) are prepared as above by cyclization of diphenylsulfoncarboxylic acids (125) (Scheme 57) or by oxidation (Scheme 58) of the thioxanthone with hydrogen peroxide, or metachloroperbenzoic acid. ##STR79## The carbonyl in (126) is then reduced by hydriodic acid in the presence of red phosphorus as described above to the thioxanthen-S,S-dioxide. Also, the thioxanthene (116) may be oxidized to the thioxanthen-S-oxide (128) (Scheme 59). ##STR80##
Dibenzosuberenes (130) are prepared by oxidative cyclization of the bis-Wittig reagent (129) prepared from the corresponding dibromide (Scheme 60) (Angew. Chem., 76 226 [1964]; Ber., 99 2848 [1966]). Catalytic hydrogenation of (130) yields dibenzosuberane (131). ##STR81##
9,10-Dihydroacridines (133) are prepared by reduction of acridines (132) with sodium amalgam in alcohol, or zinc in hydrochloric acid (Scheme 61). ##STR82## (Annalen, 158 278; Ber., 16 1818, 1972). 9,10-Dihydroacridines are also prepared by the reduction of 9,10-dihydro-9-acridones with sodium in alcohol, (Ber. 40 2521), or by reduction of the quaternary acridinjure halide (Ber., 35 2536).
Substituted acridines (132) can be prepared by reacting a 2-halo-benzaldehyde (134) with substituted anilines (135) (Scheme 62) (Ber. 50 1312, 52 1648). Substituted 9,10-dihydroacridines are described: (Ber., 62, 4161 Annalen, 463 301; J. Chem. Soc 125 1775; Chem. Soc 49 1051, 1052). ##STR83##
Acridones (137) can be prepared by cyclizing substituted-diphenylamine-2-carboxylic acids (136) with sulfuric acid or phosphorus pentachloride (Scheme 63) (Annalen, 355 345, 346, 344, 371). ##STR84##
Heteroderivatives of fluorene, such as azafluorenes and diazafluorenes are alkylated under similar conditions as fluorene and substituted-fluorenes, (Schemes 64 and 65) ##STR85##
Monoazafluorenes are generally prepared from the commercially available 4-azaphenanthrene (138) or 1-azaphenanthrene (143). These are oxidized with iodine pentoxide in acetic acid (glacial) to yield the corresponding 4- and 1-azaphenanthren-5,6-dione (139,144). Bask rearrangement of these 5,6-diones with sodium hydroxide solutions in water yield the corresponding 1-azafluorenone (140) and 4-azafluorenone (145). Reduction with hydrazine in diethyleneglycol at 180°-225° occurs rapidly to produce the desired 1-azafluorene (141) and 4-azafluorene (146). Alkylation produces the target compound (147).
Syntheses of monoazafluorenes are described by: K. Kloc, et al., J. Fur. Prakt. Chem., 319, 959-967 (1977); L. J. Henderson, Jr., et al., J. Amer. Chem. Soc., 106, 5876-5879 (1984); K. Kloc, et. al., Heterocycles, 9, 849-852 (1978); J. Mtochonski and Z. Szule, Polish J. Chem., 57, 33-39 (1983).
Diazafluorenes are generally prepared from phenanthrolines, which are most often prepared by a double Skraup synthesis or by an oxidative photocyclization of a diazastilbene.
In a Skraup synthesis, a phenylene diamine (148) or a nitroaniline is reacted with glycerine (149) and sulfuric acid or arsenic acid and an oxidizing agent, such as m-nitrobenzene sulfonic acid (Scheme 66). ##STR86## An intermediate amino- or nitro-guinoline or isoguinoline is produced. In the case of the amino-quinoline, it is not isolated, as it reacts immediately with excess reagents to yield the phenanthroline. If a nitro-aniline has been used to produce a nitroguinoline, it is isolated and purified if necessary. This often removes large amounts of tars produced by the Skraup synthesis. The nitro group is then reduced by standard conditions to yield an aminoquinoline. The aminoquinoline is then subjected to another Skraup reaction (sulfuric or arsenic acid, or both, glycerins and m-nitrobenzenesulfonic acid) to yield the phenanthroline.
Some phenanthrolines are very reluctant to undergo the usual basic oxidative rearrangement to the corresponding diazafluorenone. This is true of 4,7-phenanthroline, for instance. In this case, one uses 2-methoxyparaphenylenediamine in a double Skraup synthesis to produce the enolether, 5-methoxy-4,7-phenanthroline (150). Reaction of it with concentrated sulfuric acid and fuming nitric acid yields 4,7-phenanthrolin-5,6-quinone (151). The quinone undergoes oxidative rearrangerent to produce 1,8-diazafluoren-9-one (152). Hydrazine reduction produces 1,8-diazafluorene (153) which is alkylated to the target compound, 9,9-bis(4-pyridinylmethyl)-1,8-diazafluorene (154). Other diazafluorenes produced by this method include 1,5-diazafluorene, (Scheme 67, 157), 1,6-diazafluorene, 2,5-diazafluorene, 3,5-diazafluorene, and 4,5-diazafluorene. See references for Scheme 64 and: French patent 382 542; French patent 1,369,626, U.S. Pat. No. 2,640,830, Swiss patent 275,433. ##STR87##
Phenanthrolines may also be prepared by an oxidative photocyclization of diazastilbenes (Scheme 68). ##STR88## Commercially available trans-1,2-di(4-pyridinyl)ethene (159) in the presence of medium pressure ultraviolet light (200 watts to 1200 watts) isomerizes to the cis-isomer which, in the same reactor absorbs another photon producing dihydro-2,9-phenanthroline (161). In the presence of air, the material is quickly oxidized to 2,9-phenanthroline. Oxidative rearrangement in the presence of base yields 3,6-diazafluoren-9-one (162). Hydrazine reduces it to 3,6-diazafluorene (163). Alkylation by the usual methods described above yield the target 5,5-Bis(4-pyridinylmethyl)cyclopenta[2,1-c:3,4-c']dipyridine (164). Pertinent references are the following: J. Org. Chem., 52 3975-79 (1987); Ann., 696 1-14 (1966) for the preparation of phenanthrolines, which when rearranged to diazafluorenes yield the following: 1,8-diazafluorene; 1,5-; 1,7-; 1,6-; 2,7-; 2,5-; 4,5-; 2,6-; 3,5-; and 3,6-diazafluorenes.
The preparation of 2-azafluorene begins with the photocyclization of 3-styrylpyridine (165) to the 3 -azaphenanthrene (166) described by G. Galiazzu, et al., Tet. Letters, 3717 (1966) and also Organic Reactions, 30, Chapter 1, Photocyclization of stilbenes and related molecules, by Mallory and Mallory, pp. 1-456 (1984), John Wiley & Sons, and references cited therein for preparation of azastilebenes. The 3-azaphenanthrene (165) is then oxidized as described above with iodine pentoxide in acetic acid to yield the 5,6-quinone. This is rearranged with sodium hydroxide solution to 2-azafluorenone. Hydrazine in diethyleneglycol yields the desired 2-azafluorene (167), which is alkylated with picolylchloride to produce the target compound, 9,9-bis (4-pyridinylmethyl)-2-azafluorene (168) (69). ##STR89##
Following the photocyclization conditions described above, 4-styrylpyridine (169) may be converted to 3-azafluorene (170) and alkylated to yield the target 9,9-bis (4-pyridinylmethyl)-3-azafluorene (171) (Scheme 70). ##STR90##
The nitrogen in the above diazastilbenes and monoazastilbenes may be replaced with other heteroatoms and heterocycles to yield targets as shown in Scheme 71. ##STR91## For instance, 3-styrylthiophene (172) yields a photocyclization product (J. Chem. Soc. C, 2504 (1970) which may be converted by the methods described above to 4H-indeno[1,2-b]thiophene (173). Likewise, 2-styrylthiophene (175) is converted by photocyclization [J. Chem. Soc., 6221 (1965)] to an intermediate that will yield 8H-indeno[2,1-b]thiophene (176). These may then be alkylated by picolyl chloride to yield 4,4-bis (4-pyridinylmethyl)indeno[1,2,-b]thiophene (174) and 8,8-bis(4-pyridinylmethyl)indeno[2,1-b ]thiophene (177). Also, the furan derivatives are available via this route (Z. Naturfursch., Teil B, 24 (1969).
In the same manner, Scheme 72 shows the conversion of 1,2-di(3-thienyl)ethylene (178) to 4,4-bis(4-pyridinylmethyl)cyclopenta[2,1-b:3,4-b']-dithiophene (179) and the 2-isomer (180) to 7,7-bis(4-pyridinylmethyl)cyclopenta[1,2-b:4,3-b']-dithiophene (181). The corresponding furans produce 4,4-bis(4-pyridinylmethyl)cyclopenta[2, 1-b:3,4-b']difuran and 7,7-bis(4-pyridinylmethyl)-cyclopenta[1,2-b:4,3-b']-difuran. ##STR92##
The heterocyclic compounds D--CH 2 --Het used as intermediates in the processes described above are available commercially or by methods described in standard works on heterocyclic chemistry such as Katritzky and Rees, Comprehensive Heterocyclic Chemistry, Vols. 2-5, Pergamon Press, N.Y., 1984. In some instances the preparation of the corresponding hydroxy compounds (D═OH ) is described in the literature; these can be converted to the corresponding halo compounds (e.g. D═Br) by mild reagents such as triphenylphosphine with carbon tetrabranide. Alternatively, the hydroxy compounds can be converted to the corresponding sulfonate esters (e.g. D═CH 3 SO 2 O) by reaction with the corresponding sulfonylchloride in the presence of a base such as pyridine or triethylamine. In sane cases, the methyl substituted heterocycles CH 3 ---Het can be converted directly into the halo compounds (D═Cl or Br) with a halogenating reagent such as N-bromosuccinimide or N-chlorosuccinimide. Specifically, the following heterocyclic compounds were prepared by the methods described in the literature references given: 2-chloromethylpyrazine, Newkate, et.al., Synthesis, 676 (1984); 4-bromomethylpyrimidine, Lombardino, et. al., U.S. Pat. Nos. 4,426,263 and Brown, et. al., Aust. J. Chem., 27, 2251 (1974); 4-chloranethylpyridazine, Heinisch, Monatsh. Chem., 104, 1354 (1973); 1-benzyl-4-hydroxymethylpyrazole, Stein, U.S. Pat. No. 4,151,293.
The compounds useful in the present invention can be used as their free base or their pharmaceutically suitable salts. Salt formation is well known to those skilled in the art.
The invention can be further understood by the following examples in which parts and percentages are by weight unless otherwise indicated; all temperatures are in degrees centigrade.
EXAMPLE 1
3,3-Bis(2-pyridylmethyl)-1-phenylindolin-2-one
To a solution of 0.1 mole of N-phenylindolin-2-one in 200 ml of benzene under N 2 was rapidly added 0.1 mole of thallium ethoxide. The solution was heated briefly to boiling. At about 50°, a heavy precipitate started to form. After refluxing for 5 minutes, the mixture was cooled and 200-300 ml of hexane was added to complete precipitation. The solid was filtered off and dried to yield 85% of the thallium salt of N-phenylindolin-2-one as a yellow solid.
0.22 Mole of picolylchloride hydrochloride was carefully converted to the free base by dissolving in 30 ml cold water, cooling to 0-5° and basifying extracted out (3×100 ml benzene), dried with Na 2 SO 4 and filtered, while maintaining the temperature no higher than 10°.
To this solution was added the thallium salt of the N-phenylindolin-2-one, followed by 200 ml benzene. This mixture was refluxed overnight and after cooling, the precipitated thallium chloride was filtered off. The basic product was extracted out of the filtrate with 0.5N hydrochloric acid and was then reconverted to the base with ammonium hydroxide and extracted into methylene chloride, dried with anhydous potassium carbonate, filtered and evaporated. The remaining thick dark red oil was dissolved in 50 ml ether and trituration with a glass rod started crystallization, which was complete in a short while. The solid was filtered off, washed with ether and dried to yield 11.2 g of product; m.p. 107°-111°. The product was purified by flash chromatography using 40-60 micron silica gel 60 (E. Merck) on a column 10" long×2" in diameter. Elution with 95:5 methylene chloride-methanol (detection with a 256 m m Gow-Mac detector) afforded 8.2 g of pure free base in fractions 5 through 10 (100 ml each), Rf 0.33 (silica gel; 95:5 methylene chloride/methanol ); m.p. 129°-130°.
Anal. Calcd. for C 26 H 21 N 3 O: C, 79.77; H, 5.41; N, 10.73. Found C, 80.05; H, 5.65; N, 10.67.
EXAMPLE 2
3,3-Bis(2-pyridylmethyl)-1-phenylindolin-2-one dihydrochloride
8.2 g of 3,3-Bis(2-pyridylmethyl)-1-phenylindolin-2-one was converted to the dihydrochloride salt by dissolving it in 25 ml methylene chloride and adding 25 ml of 25% hydrochloric acid in ethanol. The solution was evaporated and the glassy residue was dissolved in 75 ml boiling acetone. Cooling to room temperature and trituration started crystallization. After sitting at room temperature for 6 hours, the mixture was kept at 0° overnight. The product was then filtered, washed with cold acetone and dried in a vacuum oven for 1 hour at over Granusic to yield 8.55 g; m.p. 250°-251°. The product was recrystallized from isopropanol affording 8.29 g; m.p. 250°-251°.
EXAMPLE 3
3,3-Bis(3-pyridylmethyl)-1-phenylindolin-2-one dihydrochloride
To 0.3 mole of N-phenylindolinone in 300 ml of benzene was added 0.36 mole of sodamide in one batch. The mixture was refluxed for 3 hours (until anmonia evolution ceases), and the reaction was then cooled to room temperature. 0.5 Mole of 3-picolylchloride was carefully prepared from the hydrochloride salt in the same manner previously described for 2-picolylchloride and was then extracted into benzene, dried with sodium sulfate and filtered. This benzene solution of 3-picolylchloride was added dropwise with vigorous mechanical stirring to the N-phenylindolinone anion solution under nitrogen over a period of 30 minutes at 20°. After completion of addition, the reaction was refluxed for an additional 3 hours.
The reaction mixture was cooled to room temperature and a second portion of 0.36 mole of sodamide was added in one batch. As above, the mixture was refluxed until ammonia evolution from the reaction ceased (3 hours).
The reaction mixture was cooled to room temperate and an additional 0.5 mole of 3-picolylchloride base in benzene was added dropwise with vigorous stirring to the indolinone anion solution over a period of 30 minutes at 20°. After completion of addition of the 3-picolylchloride, the reaction mixture w-as refluxed 3 hours. The reaction was added (300 ml) in conjunction with vigorous mechanical stirring. The HCl phase was separated and the organic phase was extracted twice more with 100 ml of 1N HCl. The combined acid extracts were made basic, extracted with methylene chloride, washed with water, dried with sodium sulfate, filtered and evaporated. The dark oil was triturated with ether to yield a crop of dense crystals, which were filtered, washed with ether until the washings were colorless, to afford 3.1 g of solid; m.p. 136.5°-138°. A portion (2.8 g) was dissolved in 10 ml of 25% hydrochloric acid in ethanol. Scratching started crystallization (dense crystals). After one hour at 0°, the white crystals were filtered off and dried to yield 3.2 g of the title compound; m.p. 156°. The product was dissolved in 115 ml boiling ethanol, to which 10 ml of boiling acetone was carefully added. The solution was allowed to cool undisturbed for 8 hours, then overnight at 0°. The pure white crystals were filtered, washed with cold 1:1 ethanol-acetone and dried under infrared lamps, to afford 2.6 g of pure product; m.p. 156°-156.5°.
EXAMPLE 4--Method A
3,3-Bis(4-pyridylmethyl)-1-phenylindolin-2 -one dihydrochloride
N-phenylindolinone (0.05 mole) was dissolved in the minimum amount of dry tetrahydrofuran in a multi-neck flask under N 2 . Lithium diisopropylamide (0.05 mole) was weighed out in a dry box into a dropping funnel and then dry tetrahydrofuran was added to the lithium diisopropylamide to dissolve it. The dropping funnel containing the lithium diisopropylamide-tetrahydrofuran solution was sealed and removed from the dry box. The indolinone solution was cooled to -30° and the lithium diisopropylamide solution was added to it dropwise at -30° over a period of 15 minutes. After the addition, the reaction was allowed to warm to room temperature. The reaction mixture was again cooled to -30° and 4-picolylchloride (0.06 mole), which had described and then dissolved in 25 ml tetrahydrofuran, was added dropwise during 30 minutes at -30°.
After completion of addition, the reaction was allowed to warm to room temperature for 30 minutes. It was then cooled to -30° and the second portion of lithium diisopropylamide (0.05 mole ) in tetrahydrofuran was added dropwise over a period of 15 minutes at -30°. After completion of addition, the reaction mixture was allowed to warm to room temperature as a second batch of 4-picolylchloride hydrochloride (0.06 mole) was converted to the free base.
The room temperature anion reaction mixture was again cooled to -30° and the second portion of 4-picolylchloride in 25 ml tetrahydrofuran was added dropwise over a period of 30 minutes at -30°. The reaction mixture was brought to room temperature and maintained at room temperature for 1-7 hours depending on convenience. Any remaining anion was destroyed by carefully adding 50 ml saturated ammonium chloride solution. The tetrahydrofuran was then evaporated and the residue was dissolved in methylene chloride and extracted out of the methylene chloride with 3×100 ml portions of 0.5N hydrochloric acid. The combined HCl portions were made basic (pH=12) and product extracted with (3×100 ml) methylene chloride. The methylene chloride was dried with sodium sulfate, filtered and evaporated to yield 20 g of product. Purification by chromatography in 10 g batches (40-3 mm silica gel on a column 8" long×2" diameter; eluting with: EtOAc 69.46%, Hexane 29.75%, and Et 3 N 0.79%) gave 19.2 g of the base (93%); m.p. 186.0°-186.5°.
3,3-Bis (4-pyridylmethyl)-1-phenylindolin-2-one (19 g) was converted to the dihydrochloride by treatment with 40 ml 25% hydrochloric acid in ethanol. To the mixture was added 50 ml isopropanol and the solution was heated to boiling. Boiling acetone was added until thick needles just started to form (total volume of solvents: 200-250 ml). The solution was allowed to cool to room temperature, then allowed to stand overnight at 0°. The solid was filtered and washed with cold isopropanol to yield 19.5 g (84%) of the title compound; m.p. 257°-8°. (Note: degree of drying has an effect on m.p. of the dihydrochloride; very slowly increasing the temperate of the melting point apparatus gives a melting point of 275°-276°). A second crop was obtained by evaporating the filtrate, dissolving the residue in isopropanol and adding approximately an equal volume of acetone; the mixture was allowed to sit overnight at temperature, and then 6 hours at 0° to yield an additional 2.8 g, m.p. 252°-253°. Recrystallization yielded 2.4 g, of the second crop: m.p. 257°-258°. The total dihydrochloride yield was 21.9 g (94%).
EXAMPLE 4--Method S (Preferred)
Part A: 3-(4-Pyridinylmethylidene)-1-phenylindolin-2-one
A solution of oxalyl chloride (175 mL, 254.6 g, 2.01M) was cooled to 5°, and a solution of diphenylamine (320 g, 1.89M) and toluene (580 mL) added over 8 minutes. The mixture was heated to 50° -65° for 74 minutes. The mixture was then heated to 125° to distill toluene and excess oxalyl chloride; total distillate collected was 630 mL. The solution was then refluxed at 125°±2° for 20 hours. The mixture was cooled to 104°, and a solution of 4-picoline (215 mL, 205.7 g, 2.21M) in acetic acid (750 mL) was added over 17 minutes. The mixture was heated to 130° to remove excess toluene via acetic acid/toluene azeotrope. Additional acetic acid (750 mL) was added during the distillation. A total of 875 mL distillate containing 260 mL toluene was collected. The mixture was cooled to 115°, and acetic anhydride (360 mL, 389.5 g, 3.81M) added over 10 minutes while heating to 120°-130°. The mixture stirred at 120°±2° for 1.75 hours, and then cooled to 76°. Water (530 mL) was added over 7 minutes followed by isopropanol (430 mL) while maintaining the temperature between 82° and 63°. The mixture was cooled to ambient temperature overnight, then to 0-5°. The crude product was collected by filtration, washed with isopropanol (2.16 1) and water 1.64 1). Drying in a vacuum oven at 80°-90° yielded the title compound (422.6 g, 75%) as an orange crystalline solid. m.p.: 160.1°-161.9°.
Part B: 3,3-bis(4-pyridinylmethyl)-1-phenylindolin-2-one
A slurry of 3-(4-pyridinylmethylidene phenylindolin-2-one (80 g, 0.268M) and methanol (600 mL) was cooled to 6°. Sodium borohydride pellets (0.2 g each, 3.19 g total 0.084M) were added over 20 minutes with gentle cooling. The mixture was stirred for 50 minutes, cooled to 7°, and 10N sodium hydroxide (64 mL, 0.64M) added over 11 minutes. A solution of 4-picolychloride hydrochloride (4.85 g, 0.296M) and water (160 mL) was then added over 28 minutes while maintaining a temperature of 10-15°. Cooling was then removed, and 10N sodium hydroxide (80 mL, 0.8M) added over 10 minutes. The mixture was stirred for 2 hours and then water (580 mL) added over 45 minutes. The slurry was cooled to 10°-15°, stirred for 10 minutes, and the solids collected by filtration. The solids were then reslurried in water (450 mL), filtered, and washed with water. Drying in a vacuum oven at 85°-95° yielded 89.4 g (85%) crude title compound. Eighty-five grams of this crude product was recrystallized in isopropanol and water to yield 77.3 g of the title compound (90% recovery), m.p. 186°-188°.
EXAMPLE 5
3,3-Bis(4-pyridylmethyl)-1-methylindolin-2-one dihydrochloride
To a solution of 0.05 mole of 1-methylindolin-2-one in 50 ml of tetrahydrofuran cooled to -30° was added 0.1 mole of lithium diisopropylamide in 100 ml of tetrahydrofuran in a dropwise fashion over 30 minutes. The reaction mixture was allowed to warm to room temperature after completion of addition, and was then cooled back down to -30°. Following the careful conditions described previously for the conversion of picolylchloride hydrochloride to picolylchloride base, 0.21 mole of 4-picolylchloride hydrochloride was converted to the anhydrous free base and was then dissolved in tetrahydrofuran (150 ml). This solution was added dropwise during 60 minutes at -30° to the reaction mixture.
After completion of addition, the reaction mixture was allowed to warm to room temperature for one hour, then was cooled and carefully decomposed by the dropwise addition of saturated ammonium chloride.
When the addition was complete, the tetrahydrofuran was evaporated and the residue was partitioned between benzene and 0.5N HCl. This residue was transferred to a separatory funnel and the organic phase was extracted twice more with 0.5N HCl. The combined acid extracts were basified, extracted with benzene, dried with Na 2 SO 4 , filtered and evaporated. The residue was triturated with ether, filtered and washed with a small amount of ether to yield 2.9 g; m.p. 149.9°-150.9°. This product was converted to the dihydrochloride salt with 25% hydrochloric acid and ethanol and crystallized from ethanol-acetone to yield 1.9 g of the title compound, m.p. 274.5°.
EXAMPLE 6
3,3-Bis(4-pyridylmethyl)-1-(3-chlorophenyl)indolin-2 -one dihydrochloride
Using the procedure of Example 3, the title compound was prepared from N-(3-chlorophenyl)-indolin-2-one in a yield of 24%, m.p. 275°-276°.
EXAMPLES 7 AND 8
3,3-Bis(4-pyridylmethyl-1-oxido)-1-phenylindolin-2one and 3-(4-pyridylmethyl)-3-(4-pyridylmethyloxido)-1-phenylindolin-2-one
A solution of 4.14 g (0.024 mole) of 80-5% ml) chloroperbenzoic acid in 50 ml methylene chloride was added dropwise with magnetic stirring to 3,3-bis(4-pyridylmethyl)-1-phenylindolin-2-one in 100 ml methylene chloride, and solution was stirred overnight. Checking for peroxide with moist starch iodide paper was negative, so the methylene chloride solution was washed with 3×75 ml 5% sodium bicarbonate, dried with sodium sulfate, filtered and evaporated.
The residue was triturated with 5:1 ether/ethyl acetate to yield 2.14 g of a solid containing the bis-N-oxide, the mono-N-oxide, and a small amount of starting material. The reaction mixture was purified by flash chromatography (silica gel, 40-63 mm, eluting with 90:10 chloroform/methanol) affording 1.18 g, of the major product, R f =0.34; m.p. 265.3°-65.7° (after recrystallization from 10 ml water). The high resolution mass spectrum confirmed the major product as the bis N-oxide; m/e 423. 1595 (M+, calcd. for C 26 H 21 N 3 O 3 423.1582).
A second fraction (200 mg) obtained from the flash chromatography was identified as the mono-N-oxide; 3-(4-pyridylmethyl)-3-(4-pyridylmethyloxido)-1-phenylindolin-2-one, Rf=0.41; m.p. 217.7°-218.5°.
Mass spectrum m/e 407.1631 (M+, calcd. for C 26 H 21 N 3 O 2 407.1634).
The compounds of Examples 1-8, and other compounds which can be prepared by such procedures and procedures described in the synthesis disclosure are illustrated by the structures represented in Table 1. This Table is intended to illustrate the invention, but not to limit its breadth.
TABLE 1 ##STR93## Ex. No. X Y R V W p Het.sup.1 Het.sup.2 Z m.p. °C. 1 H H ##STR94## H H 0 ##STR95## ##STR96## O 129-130 2 H H ##STR97## H H 0 ##STR98## ##STR99## O 250-251 (2 HCl) 3 H H ##STR100## H H 0 ##STR101## ##STR102## O 156-156.5 (2 HCl)136.5-138 (free base) 4 H H ##STR103## H H 0 ##STR104## ##STR105## O 257-258 (2 HCl)186-186.5 (free base) 5 H H CH.sub.3 -- -- 0 ##STR106## ##STR107## O 274-275 (2 HCl)149.5-150.9 (free base) 6 H H ##STR108## 3-Cl H 0 ##STR109## ##STR110## ) 275-276 (2 HCl) 7 H H ##STR111## H H 0 ##STR112## ##STR113## 265.3-265.7 8 H H ##STR114## H H 0 ##STR115## ##STR116## O 217.7-218.5 9 H H ##STR117## -- -- 1 ##STR118## ##STR119## O 173-174 (3 HCl) 10 H H ##STR120## H H 0 ##STR121## ##STR122## O 196.1-196.7 11 H H ##STR123## H H 0 ##STR124## ##STR125## O 201.7-202.0 12 H H ##STR126## H H 0 ##STR127## ##STR128## O Amorphous 13 H H ##STR129## H H 0 ##STR130## ##STR131## O Amorphous 14 H H ##STR132## H H 0 ##STR133## ##STR134## S 15 H H ##STR135## H H 0 ##STR136## ##STR137## O 230.8-231.4 16 H H CH.sub.3 CH.sub.2 CH.sub.2 -- -- 0 ##STR138## ##STR139## O 227-228 (2 HCl) 17 H H ##STR140## H H 0 ##STR141## ##STR142## O 18 H H ##STR143## H H 0 ##STR144## ##STR145## O 19 6-CH.sub.3 H ##STR146## H H 0 ##STR147## ##STR148## O 217-219 20 6-OCH.sub.3 H ##STR149## H H 0 ##STR150## ##STR151## O 21 5-Cl H ##STR152## H H 0 ##STR153## ##STR154## O 22 H H S -- -- 0 ##STR155## ##STR156## O 23 H H ##STR157## H H 1 ##STR158## ##STR159## O 24 H 0 C.sub.2 H.sub.5 -- -- 0 ##STR160## ##STR161## O 25 H 7-NHC.sub.3 H.sub.7 ##STR162## H H 0 ##STR163## ##STR164## O 26 H H ##STR165## H H O ##STR166## ##STR167## S 27 H H ##STR168## 4-OCH.sub.3 3-OCH.sub.3 0 ##STR169## ##STR170## O 28 5-OCH 3 6-OCH.sub.3 ##STR171## H H 0 ##STR172## ##STR173## O 29 H H ##STR174## 3-Cl 4-Cl 1 ##STR175## ##STR176## O 30 H H ##STR177## -- -- 1 ##STR178## ##STR179## O 31 H H ##STR180## 2-NO.sub.2 H 0 ##STR181## ##STR182## O 32 H H -n-C.sub.10 H.sub.21 -- -- 1 ##STR183## ##STR184## O 33 5-CH.sub.3 4-CH.sub.3 ##STR185## H H 0 ##STR186## ##STR187## S 34 4-NO.sub.2 H ##STR188## -- -- 1 ##STR189## ##STR190## O 35 4-N(CH.sub.3).sub.2 H ##STR191## H 4-CF.sub.3 0 ##STR192## ##STR193## O 36 H H ##STR194## H 4-CN 0 ##STR195## ##STR196## O 37 H H ##STR197## H 4-CF.sub.3 1 ##STR198## ##STR199## O 38 H H ##STR200## H 3-N(C.sub.2 H.sub.5).sub.1 0 ##STR201## ##STR202## O 39 H H ##STR203## H H 0 ##STR204## ##STR205## S 40 H H ##STR206## 3-Cl 4-Cl 0 ##STR207## ##STR208## O 41 H 4-CF.sub.3 ##STR209## H H 0 ##STR210## ##STR211## O 42 ##STR212## H ##STR213## -- -- 1 ##STR214## ##STR215## O 43 H H ##STR216## H H 0 ##STR217## ##STR218## O 167.5-169 44 H H ##STR219## 3-NO.sub.2 H 0 ##STR220## ##STR221## S 45 H H ##STR222## H H 0 ##STR223## ##STR224## O 123-124 46 H H ##STR225## H H 0 ##STR226## ##STR227## O 152 47 H H ##STR228## 4-CN H 0 ##STR229## ##STR230## O 48 5-OC.sub.2 H.sub.5 H ##STR231## H H 0 ##STR232## ##STR233## O 49 H H ##STR234## H H 0 ##STR235## ##STR236## O 233-235 50 H H ##STR237## H H 0 ##STR238## ##STR239## O 51 H H ##STR240## H H 0 ##STR241## ##STR242## O 52 H H ##STR243## H H 0 ##STR244## ##STR245## O 53 H H ##STR246## H H 0 ##STR247## ##STR248## O 54 H H ##STR249## H H 0 ##STR250## ##STR251## O 131-133 55 H H ##STR252## H H 0 ##STR253## ##STR254## O 56 H H ##STR255## H H 0 ##STR256## ##STR257## O 57 H H ##STR258## H H 0 ##STR259## ##STR260## O 58 H H ##STR261## H H 0 ##STR262## ##STR263## O 59 H H ##STR264## H H 0 ##STR265## ##STR266## O 60 H H ##STR267## -- -- 1 ##STR268## ##STR269## O
EXAMPLE 61
1,1-Bis(4-pyridinylmethyl)-3-phenyl-1H-indene bismethanesulfonate
To a cooled (-20°) solution of 3-phenyl-1H-indene (5.0 g, 26 mmol) in tetrahydrofuran (THF) (70 ml) was added n-butyllithium (1.1 equivalents, 1.17M, 28.6 mmol, 24.5 ml) dropwise. After stirring for 30 min., a solution of 4-picolyl chloride (1.5 equivalents, 39 mmol, 5.0 g) in THF (70 ml) was added. The solution was warmed to 0°, and maintained at this temperature for 1 h. The mixture was again cooled to -20°, and additional n-butyllithium and 4-picolyl chloride were added as described above. The solution was then warmed to 0° for about 2 h. The reaction mixture was quenched with saturated ammonium chloride solution, and diluted with ether. The organic phase was washed with water, brine, and dried over magnesium sulfate. Removal of solvent by rotary evaporation provided an oil which was purified by column chromatography (silica gel, dichloromethane/methanol, 60:1 to 20:1) to give 1,1-Bis(4-pyridinyLmethyl)-3-phenyl-1H-indene as a solid, 5.8 g, 15.5 mmol, 60% yield. NMR (200MHz, CDCl 3 ) δ 3.18 (dd, 4H); 6.23 (s, 1H); 6.79 (d, 4H, J=6 Hz); 7.12 (m, 4H); 7.29 (m, 4H); 7.51 (d, 1H, J=7 Hz); 8.28 (d, 4H, J=6 Hz). Mass spec. 374.
To a solution of 1,1-bis (4-pyridinylmethyl)-3-phenyl-1H-indene (1.0 g, 2.7 mmol) in dichlorcmethane was added methanesulfonic acid (5.4 mmol, 0.52 g, 0.35 ml ). The solvent was evaporated and the residue was recrystallized from ethyl acetate/ispropanol to give white crystals, 0.8 g, m.p.>250°.
EXAMPLE 62
4-((2,3-Dihydro-3-phenyl-1-(4-pyridinylmethyl)-1H-inden-1-ylmethyl))-pyridine dihydrochloride
To a solution of 1,1-bis(4-pyridinylmethyl)-3-phenyl-1H-indene (5.8 g, 15.5 nmol ) in 95% ethanol (100 ml), was added 5% palladium on carbon catalyst (1.45 g) and the mixture was shaken under hydrogen (50 psig) at room temperature for 2 h. The catalyst was removed by filtration, and the solvent removed by rotary evaporation. The oil was purified via column chromatography (silica gel, 10% methanol/dichloromethane) to give pure 4-((2,3-dihydro-3-phenyl-1-(4-pyridinylmethyl)-1H-inden-l-ylmethyl))-pyridine. NMR (200 MHz, CDCl 3 ) δ 2.05 (dd, 1H); 2.38 (dd, 1H); 2.93 (dd, 2H); 3.15 (dd, 2H); 3.42 (m, 1H); 6.67 (dd, 4H); 7.00 (d, 2H); 7.10-7.34 (m, 7H); 8.36 (d, 2H, J=5 Hz); 8.42 (d, 2H, J=5 Hz). Mass Calcd. for C 27 H 24 N 2 : 376.1937. Found: 376.1951.
The oil was dissolved in methanol, and HCl in ether was added to precipitate the salt. Recrystallization from isopropanol/ethyl acetate gave a white solid, 6.2 g, m.p. 210°-225°.
EXAMPLE 63
3,3-Bis(4-pyridinylmethyl)-2,3-dihydro-1-phenyl-1H-indene-1,2-dioldiacetate dihydrochloride
To a solution of 1,1-Bis(4-pyridinylmethyl)-3-phenyl-1H-indene (1.0 g, 2.7 mmol) in dry pyridine (10 ml) was added osmium tetroxide (1.0 g, 3.9 mmol, dissoleved in ether). The mixture was stirred at room temperature and monitored by TLC. After completion of the reaction, sodium bisulfite (2.0 g), water (20 ml), and pyridine (5 ml) was added. The mixture was stirred for 1 h, and extractd three times with chloroform: isopropanol (4:1). The combined extracts were washed with brine, dried over magnesium sulfater, and evaporated to give 3,3-bis(4-pyridinylmethyl)-2,3-dihydro-1-phenyl-1H-indene-1,2-diol as a yellow solid, 1.15 g.
The crude 3,3-bis(4-pyridinylmethyl)2,3-dihydro-1-phenyl-1H-indene-1,2-diol was redissolved in pyridine (20 ml) and acetic anhydride (4 ml) was added. The mixture was heated to 50° for 2 days. After cooling, the volatile materials were removed by vacuum transfer, and the residue was redissolved in dichloromethane and water. The aqueous layer was made slightly basic with potassium carbonate, and extracted several times with dichloromethane. The combined extracts were dried over sodium sulfate, and the solvent was evaporated to afford an oil. This material was purified via column chromatography (silica gel, 10% methanol/dichloromethane) to give 3,3-bis(4-pyridinylmethyl)2,3-dihydro-1-phenyl-1H-indene-1,2-dioldiacetate as an oil NMR (200 MHz, CDCl 3 ) δ 2.06 (s, 3H); 2.11 (s, 3H); 3.05-3.49 (2dd, 4H); 5.28 (s, 1H); 6.64 (dd, 1H); 6.89 (m, 6H); 7.26 (m, 5H); 7.60 (dd, 1H); 8.27 (d, 2H, J=6 Hz); 8.,51 (d, 2H, J=6 Hz). Mass Calcd. for C 31 H 28 N 2 O 4 : 492.2049. Found 492.2041.
To a solution of 3,3-bis(4-pyridinylmethyl)2,3-dihydro-1-phenyl-1H-indene-1,2-dioldiacetate in dichloromethane was added excess HCl in dichloromethane. The solvent was removed, and the residue was recrytallized from ethanol/ethyl acetate to give a white solid, 0.42 g, m.p.>300°.
EXAMPLE 64
Part A: α,α-Bis(4-pyridinylmethyl)-2-methoxybenzeneacetonitrile
To a mechanically stirred slurry of (2-methoxyphenyl)acetonitrile (10.0 g, 68 nmol ), 4-picolyl chloride hydrochloride (25.0 g, 152 nmol), and 1.2 g benzyltriethylammonium chloride in toluene (200 ml) at room temperature was added 50% NaOH (50 ml) over a period of 15 min. After addition was complete, the reaction mixture was slowly heated to 50° and maintained at that temperature for approx. 3 h. Completion of the reaction was determined by TLC. While still stirring the reaction mixture at 50°, 70 ml of water was added, and stirring was continued for 15 min. The mixture was cooled to room temperature, and the layers were separated. To the toluene layer was added 14.0 g Magnesol (an intimate mixture of silica gel and magnesium sulfate), and the solution was stirred at 50° for 30 min. The solution was filtered, and the solvent was removed under reduced pressure. The subsequent oil was purified via column chromatography (silica gel, 10% methanol/methylene chloride) to give α,α-Bis(4-pyridinylmethyl)2-methoxybenzeneacetonitrile as a solid, 16.4 g, 73% yield. NMR (200 MHz, CDCl 3 ) δ 3.26 (d, 2H, J=13 Hz); 3.88 (d, 2H, J=13 Hz); 4.07 (s, 3H); 6.70 (m, 6H); 7.00 (m, 6H); 7.30 (m, 1H); 8.38 (m, 4H). Mass Calcd. for C 21 H 19 N 3 O: 329.1528. Found: 329.1505.
The solid was treated with HCl in methanol, and ether was added to precipitate a white solid. Recrystallization from methanol/acetone produced white needles, m.p. 228°-233° (dec).
Part B: 3,3-Bis(4-pyridinylmethyl)-2(3H)-benzofuranonedihydrochloride
To a solution of α,α-Bis(4-pyridinylmethyl)- 2-methoxybenzeneacetonitrile (14.36 g, 43.6 nmol) in ethylene glycol (100 ml), was added KOH (40 ml of a saturated solution) and the mixture was heated at 120°-130° under nitrogen for 20 h. The solution was cooled to room temperature, diluted with 200 ml water, and neutralized with aqueous anmonium chloride to about pH 7. The mixture was extracted with chloroform: isopropanol (4:1) until complete by TLC. The ccrbined extraRs were washed with brine, dried over sodium sulfate, and evaporated (rotary evaporator). The solid was dried in a vacuum oven at 50° and 5 torr to give 7.7 g, 22 mmol, 50% yield of α,α-bis(4-pyridinylmethyl)-2-methoxybenzeneacetic acid as a white powder.
To a suspension of α,α-bis(4-pyridinylmethyl)-2-methoxybenzene-acetic acid (7.7 g) in dichloroethane (150 ml) at 0° was added boron tribromide-methyl sulfide complex (1M in dichlorcrethane, 5 equivalents, 110 mmol, 110 ml). The mixture was wamred to room temperature, then heated at reflux for 20 h. After cooling to room temperature, 6N HCl (100 ml) was added, and the mixture was refluxed for 18 h. The mixture was cooled, diluted with water, and the layers were separated. The organic layer was extracted twice with 1N HCl (50 ml each). The combined aqueous layer was basified to pH 9 with concentrated ammonium hydroxide, and extracted with dichloromethane. The organic solution was dried over magnesium sulfate, filtered, and evaporated to give an oil. Purification by column chromatography (silica gel/3% methanol in dichloromethane afforded 3,3-bis(pyridinylmsthyl)-2(3H)benzofuranone [(4.7 g, 14.9 nmol, 68%) NMR (200 MHz, CDCl 3 ) δ 3.31 (dd, 4H); 6.75 (m, 1H); 6.82 (dd, 4H); 7.14-7.30 (m, 3H); 8.35 (dd, 4H). Mass Calcd. for C 20 H 16 N 2 O 2 : 316.1211. Found: 316.1202] and unreacted α,α-bis(4-pyridinylmethyl)- 2-methoxybenzene-acetic acid (2.5 g, 7.2 nmol).
This compound was converted into the hydrochloride salt as described above to give a white powder, m.p. 269°-270°. Analysis. Calcd. for C 20 H 18 Cl 2 N 2 O 2 : C, 61.70; H, 4.66; N, 7.19. Found: C, 61.65; H, 4.83; N, 7.06.
EXAMPLE 65
1,1-Bis(4-pyridinylmethyl)-1,3-dihydro-2H-inden-2-one
To stirred mixture of 2-indanone (2.64 g, 0.02 mol), 4-picolyl chloride hydrochloride (7.22 g, 0.044 mol ), and benzyltriethylanmonium chloride (0.45 g, 0,002 mol) in 100 ml of benzene was added 1N sodium hydroxide (84 ml, 0.084 mol ) dropwise over a period of 30 min. The mixture was stirred for an additional 2.5 h. at room temperature, then heated to 60° and maintained at this temperature for 1 h. Thin layer chromatographic analysis indicated that the reaction was complete. The reaction mixture was cooled, the organic layer was separated, and diluted with an additional 80 ml of benzene. The benzene solution was extracted with 100 ml of 1N HCl. The acidic layer was basified with 10% sodium hydroxide, wherein the crude product separated as a gum. The crude material was crystallized frcn cyclohexane, and further purifed by recrystallization from cyclohexane to give 1,1-bis(4-pyridinylmethyl)-1,3-dihydro-2H-indene-2-one as a white solid, 0.300 g, m.p. 95°-96°. NMR (200 MHz, CDCl 3 ) δ 2.66 (s, 2H); 3.07-3.34 (d, 4H); 6.73 (d, 4H); 6.82-7.47 (m, 4H). IR (nujol) 1714 cm -1 . Analysis. Calcd. for C 21 H 18 N 2 O: C, 80.23; H, 5.77; N, 8.91. Found: C, 80.47; H, 5.76; N, 8.89.
EXAMPLE 124
1,1-Bis(4-pyridinylmethyl)-2(1 H)-naphthalenone
To a stirred mixture of 2-tetralone (4.4 g, 0.03 mol), 4-picolylchloride hydrochloride (10.82 g, 0.066 mol), and benzyltriethylanmonium chloride (1.4 g, 0.006 mol) in 80 ml of benzene was added 1N sodium hydroxide (178 ml, 0.178 mol) dropwise during a period of 1 h. at room temperature. Stirring was continued for another hour. Additional benzene (80 ml ) was added, the organic layer was separated, and dried over sodium sulfate. The inorganic salts were filtered off, and to the filtrate was added 5 g of Florisil (a magnesium silicate adsorbent). The mixture was stirred for 30 min., the solids were filtered off, and the benzene was removed by rotary evaporation. The oily residue was dissolved in the minimum amount of ethanolic HCl (5 ml), and a small amount of acetone was added, whereupon the dihydrochloride salt crystallized out of solution. This salt was collected (1.57 g), redissolved in water, and made basic with potassium carbonate. The solids obtained were air dried (900 mg), and recrystallized from cyclohexane to give 1,1-bis(4-pyridinylmethyl)-2(1H)-naphthalenone as a white solid, 460 mg, m.p. 111°-112° NMR (200 MHz, CDCl 3 ) δ 1.9 (m, 4H); 3.30 (d, 4H); 6.55 (d, 4H); 6.95 (d, 1H); 7.15 (t, 7.45 (t, 1H); 7.66 (d, 1H); 8.30 (d, 4H). IR (nujol) 1709 cm -1 . Analysis. Calcd. for C 22 H 20 N 2 O: C, 80.46; H, 6.14; N, 8.53. Found: C, 80.12; H, 6.25; N, 8.61.
EXAMPLE 125
1,1-Bis(4-pyridinylmethyl)-3,4 -dihydro-7-methoxy-2(1H) -naphthalenone
To a suspension of sodium hydride (60% oil dispersion, 1.6 g, 0.04 mol) in 30 ml of dry 1,2-dimethoxyethane was added a solution of 7-methoxy-2-tetralone (3.6 g, 0.02 mol) in 30 ml of dry 1,2-dimethoxyethane dropwise. The reaction mixture turned yellow, and after all the tetralone was added, the mixture was heated gently at reflux for fifteen minutes. A solution of 4-picolyl chloride was prepared by dissolving 4-picolyl chloride hydrochloride (6.56 g, 0.04 mol) in 100 ml of water, basifying the solution with sodium bicarbonate, and extracting the free base into ether (200 ml). After drying over sodium sulfate, the mixture was filtered, and the ether was renoved by rotary evaporation. The residue was immediately redissolved in 1,2-dimethoxyethane (30 ml). This solution was added dropwise to the hot reaction mixture, and the mixture was heated at reflux for 6 h. The reaction mixture was cooled, and methanol (10 ml) was added to decompose excess sodium hydride. The solvents were evaporated, and the brown oily residue was dissolved in 200 ml of dichloromethane. The organic phase was washed with water and dried over sodium sulfate. After filtration and rotary evaporation, the crude product was purified by column chromatography (silica gel, 10% methanol in ethyl acetate). The product thus obtained was recrystallized frum ethyl acetate to give 1,1-bis(4-pyridinylmethyl)- 3,4-dihydro-7-methoxy-2(1H)-naphthaleneone as a white solid, 1.5 g, m.p. 125-127°. NMR (200 MHz, CDCl 3 ) δ 3.13-3.19 (d, 4H); 3.46-3.52 (d, 4H); 3.92 (s, 3H); 6.66-6.67 (d, 4H); 8.27-8.30 (d, 4H). IR 1707, 1599 cm -1 . Analysis. Calcd. for C 23 H 22 N 2 O 2 : C, 77.06; H, 6.18; N, 7.81. Found: C, 77.21; H, 6.13; N, 7.76.
The compounds of Examples 61-65, 124, 125 and other compounds which can be prepared by the methods described above, are illustrated by the structures represented in Tables II and III. The tables are intended to illustrate the invention, but not to iimit its breadth.
In the Tables, D=double bond, S=single bond and Ph=phenyl.
TABLE II__________________________________________________________________________ ##STR270##Ex. Q a X W Z Het.sup.1 Het.sup.2 mp °C.__________________________________________________________________________61 H D CPh H H ##STR271## ##STR272## >250 CH.sub.3 SO.sub.3 H Salt62 H.sub.2 S CHPh H H ##STR273## ##STR274## 210-225 HCl Salt63 ##STR275## S ##STR276## H H ##STR277## ##STR278## >300° HCl Salt64 O S O H H ##STR279## ##STR280## 269-270 HCl Salt65 O S CH.sub.2 H H ##STR281## ##STR282## 95-9666 O S CH.sub.2 H 5-OMe ##STR283## ##STR284##67 O S CH.sub.2 5-Cl 4-Cl ##STR285## ##STR286##68 O S CH.sub.2 H 4-Ph ##STR287## ##STR288##69 O S C(CH.sub.3).sub. 2 H H ##STR289## ##STR290##70 CH.sub.3 D CCH.sub.3 H H ##STR291## ##STR292##71 CH.sub.3 D CC.sub.2 H.sub.5 H H ##STR293## ##STR294##72 CH.sub.3 D CCH.sub.3 5-OMe 4-OMe ##STR295## ##STR296##73 H D CCH.sub.3 7-Ph H ##STR297## ##STR298##74 H.sub.2 S CH(CH.sub.3) 7-Ph H ##STR299## ##STR300##75 H D CPh 5-Cl 4-Cl ##STR301## ##STR302##76 H.sub.2 S CHPh 5-Cl 4-Cl ##STR303## ##STR304##77 H(OAc) S C(OAc)Ph 5-Cl 4-Cl ##STR305## ##STR306##78 H(OAc) S C(OAc)CH.sub.3 H H ##STR307## ##STR308##79 H D CPh 5-OCH.sub.3 4-OCH.sub.3 ##STR309## ##STR310##80 H.sub.2 S CHPh 5-OCH.sub.3 4-OCH.sub.3 ##STR311## ##STR312##81 H.sub.2 S CHPh H 5-OCH.sub.3 ##STR313## ##STR314##82 H(OAc) S C(OAc)Ph 6-OCH.sub.3 H ##STR315## ##STR316##83 CH.sub.3 D CC.sub.2 H.sub.5 4-Ph H ##STR317## ##STR318##84 (H)CH.sub.3 S CHC.sub.2 H.sub.5 4-Ph H ##STR319## ##STR320##85 O S O H 4-OCH.sub.3 ##STR321## ##STR322##86 O S O 6-Br H ##STR323## ##STR324##87 O S O 6-OCH.sub.3 H ##STR325## ##STR326##88 O S O 6-OCH.sub.3 5-OCH.sub.3 ##STR327## ##STR328##89 CH.sub.2 S CH.sub.2 H H ##STR329## ##STR330##90 CH.sub.2 S CH.sub.2 H 5-OCH.sub.3 ##STR331## ##STR332##91 CHCH.sub.3 S CH.sub.2 5-Cl 4-Cl ##STR333## ##STR334##92 CHPh S CH.sub.2 H 4-Ph ##STR335## ##STR336##93 CHPh S C(CH.sub.3).sub.2 H H ##STR337## ##STR338##94 H D CPh H H ##STR339## ##STR340##95 H.sub.2 S CHPh H H ##STR341## ##STR342##96 O S O 6-Br H ##STR343## ##STR344##97 O S O H H ##STR345## ##STR346##98 H D C(CH.sub.3) 7-Ph H ##STR347## ##STR348##99 O S CH.sub.2 H H ##STR349## ##STR350##100 O S CH.sub.2 5-Cl 4-Cl ##STR351## ##STR352##101 H D CPh H H ##STR353## ##STR354##102 H(OAc) S C(OAc)Ph H H ##STR355## ##STR356##103 H.sub.2 S CHCH.sub.3 5-OCH.sub.3 4-OCH.sub.3 ##STR357## ##STR358##104 O S CH.sub.2 H H ##STR359## ##STR360##105 O S O 6-OCH.sub.3 H ##STR361## ##STR362##106 O S CH.sub.2 H H ##STR363## ##STR364##107 O S O H H ##STR365## ##STR366##108 O S O H H ##STR367## ##STR368##109 O S CH.sub.2 H H ##STR369## ##STR370##110 H D CPh H H ##STR371## ##STR372##111 H.sub.2 S CHPh H 4-Ph ##STR373## ##STR374##112 CHPh S CH.sub.2 H H ##STR375## ##STR376##113 CHCH.sub.3 S CH.sub.2 5-OCH.sub.3 H ##STR377## ##STR378##114 (H)CH.sub.2 Ph S CH.sub.2 5-OCH.sub.3 H ##STR379## ##STR380##115 (H)CH.sub.2 CH.sub.3 S CH.sub.2 H H ##STR381## ##STR382##116 CH.sub.3 D C(CH.sub.3) H 4-Ph ##STR383## ##STR384##117 CH.sub.3 D C(CH.sub.3) H H ##STR385## ##STR386##118 H.sub.2 S CHCH.sub.3 H H ##STR387## ##STR388##119 H(OAc) S C(OAc)Ph H H ##STR389## ##STR390##120 H D CPh H H ##STR391## ##STR392##121 (H)OH S CH.sub.2 H H ##STR393## ##STR394##122 (H)(OAc) S CH.sub.2 5-OCH.sub.3 H ##STR395## ##STR396##123 NOCH.sub.3 S CH.sub.2 H H ##STR397## ##STR398##__________________________________________________________________________
TABLE III__________________________________________________________________________ ##STR399##Ex. Q W Z Het.sup.1 Het.sup.2 mp °C.__________________________________________________________________________124 O H H ##STR400## ##STR401## 111-112°125 O 7-OCH.sub.3 H ##STR402## ##STR403## 125-127126 OH H H ##STR404## ##STR405##127 OCOCH.sub.3 H H ##STR406## ##STR407##128 CH.sub.2 H H ##STR408## ##STR409##129 CHPh H H ##STR410## ##STR411##130 CH.sub.3 H H ##STR412## ##STR413##131 NOCH.sub.3 H H ##STR414## ##STR415##132 NOH 7-OCH.sub.3 H ##STR416## ##STR417##133##STR418## H H ##STR419## ##STR420##134##STR421## H H ##STR422## ##STR423##135 H.sub.2 H H ##STR424## ##STR425##136##STR426## H H ##STR427## ##STR428##137 (H)F H H ##STR429## ##STR430##138 F.sub.2 H H ##STR431## ##STR432##139 O 8-CH.sub.3 5-CH.sub.3 ##STR433## ##STR434##140 O H 6-OCH.sub.3 ##STR435## ##STR436##141 O H 5-Cl ##STR437## ##STR438##142 O H 5-NH.sub.2 ##STR439## ##STR440##143 O 7-OAc H ##STR441## ##STR442##144 O H 5-NO.sub.2 ##STR443## ##STR444##145 O 8-OCH.sub.3 7-OCH.sub.3 ##STR445## ##STR446##146 CH.sub.2 7-OCH.sub.3 H ##STR447## ##STR448##147 CH.sub.2 H 5-NH.sub.2 ##STR449## ##STR450##148 CH.sub.2 H 5-Cl ##STR451## ##STR452##149 O H H ##STR453## ##STR454##150 O 7-OCH.sub.3 H ##STR455## ##STR456##151 CH.sub.2 H 6-OCH.sub.3 ##STR457## ##STR458##152 CHPh H 5-NO.sub.2 ##STR459## ##STR460##153 OCOCH.sub.3 8-CH.sub.3 H ##STR461## ##STR462##154 NOCH.sub.3 H H ##STR463## ##STR464##155 CH.sub.2 H 5-Cl ##STR465## ##STR466##156 CHPh H 5-NO.sub.2 ##STR467## ##STR468##157 (H)CH.sub.2 Ph H H ##STR469## ##STR470##158##STR471## 7-OCH.sub.3 H ##STR472## ##STR473##159 O 8-OCH.sub.3 H ##STR474## ##STR475##160 CH.sub.2 H 6-OCH.sub.3 ##STR476## ##STR477##161 O 8-CH.sub.3 H ##STR478## ##STR479##162 CHPh H 6-CH.sub.3 ##STR480## ##STR481##163 OH H H ##STR482## ##STR483##164 NOCH.sub.3 H 6-CF.sub.3 ##STR484## ##STR485##165 CH.sub.2 H 5-NO.sub.2 ##STR486## ##STR487##166 CHPh H H ##STR488## ##STR489##167##STR490## 7-OAc H ##STR491## ##STR492##168##STR493## 7-CH.sub.3 H ##STR494## ##STR495##169 OCOCH.sub.3 H 5-Cl ##STR496## ##STR497##170 CHCH.sub.3 7-OCH.sub.3 H ##STR498## ##STR499##171 (CH.sub.3)(OH) H H ##STR500## ##STR501##172 O H H ##STR502## ##STR503##173 O 7-OCH.sub.3 H ##STR504## ##STR505##174 O H H ##STR506## ##STR507##175 O H H ##STR508## ##STR509##176 CH.sub.2 H 6-OEt ##STR510## ##STR511##177 CHCH.sub.3 H H ##STR512## ##STR513##178 CHPh H 5-NH.sub.2 ##STR514## ##STR515##179 O H H ##STR516## ##STR517##180 OH 8-OMe 7-OMe ##STR518## ##STR519##181 OCOCH.sub.3 H H ##STR520## ##STR521##__________________________________________________________________________
EXAMPLE 182
2,2-Bis(4-pyridinylmethyl)-1(2H)-acenaphthylenone dihydrochloride
To a mechanically stirred slurry of acenaphthylenone (1.682 g, 10 mmol ), 4-picolyl chloride hydrochloride (3.3 g, 22 mmol ), and 0.2 g benzyltriethylanronium chloride in toluene (50 ml) at room temperature was added 50% NaOH (5 ml) over a period of 15 min. After addition was complete, the reaction mixture was slowly heated to 50° and maintained at that temperature for approx. 3 h. Completion of the reaction was determined by TLC. While still stirring the reaction mixture at 50°, 10 ml of water was added, and stirring was continued for 15 min. The mixture was cooled to room temperature, and the layers were separated. To the toluene layer was added 2.0 g Magnesol (an intimate mixture of silica gel and magnesium sulfate), and the solution was stirred at 50° for 30 min. The solution was filtered, and the solvent was removed under reduced pressure. The subsequent oil was purified via column chromatography (silica gel, ethyl acetate) to give a solid, which was recrystallized from ethyl acetate/hexane to give 2.51 g, 71% yield, of 2,2-bis(4-pyridinylmethyl)-1(2H)-acenaphthylenone as white crystals, m.p. 165°.
The solid was treated with HCl in methanol, and ether was added to precipitate a white solid. Recrystallization from methanol/acetone produced white needles, m.p. 255° (dec). NMR (200 MHz, EMSO-d 6 ) δ 3.16 (s, 2H), 3.68 (d, 2H, J=12 Hz), 3.83 (d, 2H, J=12 Hz), 7.47 (d, 4H, J=6 Hz), 7.60-8.15 (m, 6H), 8.53 (d, 4, J=6 Hz). Analysis. Calcd. for C 24 H 20 Cl 2 N 2 O.1/2 H 2 O: C, 66.65; H, 4.90; N, 6.48. Found: C, 66.32; H, 5.26; N, 6.08.
EXAMPLE 183
4-((1,2-Dihydro-2-methylene-1-(4-pyridinylmethyl)-1-acenaphthylen-1-ylmethyl))pyridine dihydrochloride
To a mechanically stirred slurry of methyltrimethylphosphonium methylphosphonium bromide (6.25 g, 17.5 nmol) in THF (150 ml) at 0° was added n-butyllithium (1.6M, 11 ml, 17.5 nmol) dropwise. The solution was warmed to room temperature for 1 hr., then cooled back down to 0°. A solution of the ketone 2,2-bis(4-pyridinylmethyl)-1(2H)-acenaphthylenon (2.25 g, 7 mmol ) in THF (50 ml ) was added dropwise. After addition was complete, the mixture was warmed to room temperature, and stirred for about 18 hr. Saturated armonium chloride solution was added, the mixture was diluted with ether, and the layers were separated. The organic layer was washed with water, then saturated sodium chloride solution. After drying over magnesium sulfate, the solution was filtered and concentrated by rotary evaporation to give pyridine a brcsm oil. This material was purified by column chrcnmtography (silica gel, 10% methanol/ethyl acetate) to give 4-((1,2-dihydro-2-methylene-1-(4-pyridinylmethyl-1-acenaphthylen-1-ylmethyl))pyridine as a white solid, 2.27 g, 6.5 mmol, 93% yield.
The aforerentioned solid was treated with HCl in methanol, and ether was added to produced a white solid. Recrystallization from methanol/acetone/ether provided white needles, m.p.>250° (dec). NMR (200 MHz, EMSO-d 6 )δ 3.81 (q, 4H, J=13 Hz), 5.97 (s, 1H), 6.25 (s, 1H), 7.43 (m, 6H), 7.61 (m, 3H), 7.75 (m, 1H), 8.47 (d, 4H, J=6 Hz).
The ccmlDounds of Examples 182 and 183, and other orepounds which can be prepared by the methods described above, are illustrated by the structures represented in Table IV. The table is intended to illustrate the invention, but not to limit its breadth.
TABLE IV__________________________________________________________________________ ##STR522##Ex. Q W Z Het.sup.1 Het.sup.2 mp °C.__________________________________________________________________________182 O H H ##STR523## ##STR524## 255 (dec) HCl Salt183 CH.sub.2 H H ##STR525## ##STR526## 248-264 (dec) HCl Salt184 S H H ##STR527## ##STR528##185 OCOCH.sub.3 H H ##STR529## ##STR530##186 O H H ##STR531## ##STR532##187 CH.sub.2 H H ##STR533## ##STR534##188 O H H ##STR535## ##STR536##189 CH.sub.2 H H ##STR537## ##STR538##190 S H H ##STR539## ##STR540##191 O H H ##STR541## ##STR542##192 O H H ##STR543## ##STR544##193 O H H ##STR545## ##STR546##194 O H H ##STR547## ##STR548##195 O H H ##STR549## ##STR550##196 O H H ##STR551## ##STR552##197 O H H ##STR553## ##STR554##198 O H H ##STR555## ##STR556##199 O H H ##STR557## ##STR558##200 O H H ##STR559## ##STR560##201 O H H ##STR561## ##STR562##202 O H H ##STR563## ##STR564##203 CH.sub.2 H H ##STR565## ##STR566##204 CH.sub.2 H H ##STR567## ##STR568##205 CH.sub.2 H H ##STR569## ##STR570##206 CH.sub.2 H H ##STR571## ##STR572##207 CH.sub.2 H H ##STR573## ##STR574##208 S H H ##STR575## ##STR576##209 S H H ##STR577## ##STR578##210 S H H ##STR579## ##STR580##211 S H H ##STR581## ##STR582##212 S H H ##STR583## ##STR584##213 CHPh 5-Br H ##STR585## ##STR586##214 CHCH.sub.3 5-Br H ##STR587## ##STR588##215 OH H H ##STR589## ##STR590##216 S H 6-NO.sub.2 ##STR591## ##STR592##217 CH.sub.2 5-NO.sub.2 H ##STR593## ##STR594##218 CHPh H 8-CH.sub.3 ##STR595## ##STR596##219 O H 8-CH.sub.3 ##STR597## ##STR598##220 CH.sub.2 H 8-CH.sub.3 ##STR599## ##STR600##221 O 5-NH.sub.2 H ##STR601## ##STR602##222 CH.sub.2 5-NH.sub.2 H ##STR603## ##STR604##223 S 5-NH.sub.2 H ##STR605## ##STR606##224 NOCH.sub.3 H 6-NH.sub.2 ##STR607## ##STR608##225 CH.sub.3 H 6-NH.sub.2 ##STR609## ##STR610##226 OCOCH.sub.3 H 6-NH.sub.2 ##STR611## ##STR612##227 OCOCH.sub.3 H 6-NO.sub.2 ##STR613## ##STR614##228 OCOCH.sub.3 H 6-NO.sub.2 ##STR615## ##STR616##229 CH.sub.2 5-Cl 6-Cl ##STR617## ##STR618##230 O 5-Cl 6-Cl ##STR619## ##STR620##231 CHPh 5-Cl 6-Cl ##STR621## ##STR622##232 S 5-Cl 6-Cl ##STR623## ##STR624##233 OCOCH.sub.3 5-Cl 6-Cl ##STR625## ##STR626##234 O 5-CN H ##STR627## ##STR628##235 CH.sub.2 5-OH H ##STR629## ##STR630##236 S 5-OCH.sub.3 H ##STR631## ##STR632##237 CHPh H 6-COCH.sub.3 ##STR633## ##STR634##238 O H 6-COCH.sub.3 ##STR635## ##STR636##239 OCOCH.sub.3 3-CH.sub.3 8-CH.sub.3 ##STR637## ##STR638##__________________________________________________________________________
EXAMPLE 240
4,4-Bis(4-pyridinylmethyl)-3,4-dihydro-6,7-dimethoxy-1-phenyl-isoquinoline
To a suspension of amide N-((2-3,4-dimethoxyphenyl)-3-(4-pyridinyl)-2-(4-pyridinylmethyl)-propyl))-benzamide (2.306 g, 4.93 mmol) in acetonitrile (20 ml), was added phosphorus oxychloride (6 ml) and the mixture was heated to reflux for 6 hrs. After cooling to room temperature, the solvents renored by vacuum transfer. The residue was dissolved in water, basified with sodium hydroxide, and extracted with dichlorcmethane. After drying over magnesium sulfate, the solvent was removed by rotary evaporation to give a yellow oil. Purification by column chrcmatography (silica gel, 10% methanol/dichloromethane) gave a solid, which was recrystallized from ether/ethyl acetate to give white crystals of the title compound, 1.898 g, 4.22 mmol, 86% yield, m.p. 168.5°-169°. NMR (200 MHz, CDCl 3 ) 2.96 (d, 2H, J=13 Hz); 3.10 (d, 2H, J=13 Hz); 3.74 (s, 5H); 3.84 (s, 3H); 6.72 (s, 1H); 6.81 (s, 1 H); 6.95 (d, 4H, J=5 Hz); 7.43 (s, 5H); 8.44 (d, 4H, J=5). IR (KBr) 2930, 1599, 1559, 1515, 1283 cm -1 . Mass spec. 449. Analysis. Calcd. for C 29 H 27 N 3 O 2 : C, 77.48; H, 6.05; N, 9.35. Found: C, 77.29; H, 6.36; N,9.06.
EXAMPLE 288
4,4-Bis(4-pyridinylmethyl)-2-phenyl-1,3(2H,4H)-isoquinolinedione
The procedure used was essentially the same as described by Chan and Huang, Synthesis, 452 (1982). To a solution of 2-phenyl-1,3(2H,4H)-isoquinolinedione [Ueda, et. al, J. Polym. Sci., Polym. Chem. Ed. 17, 2459 (1979)], (2.14 g, 9.02 mmol ) and picolyl chloride (30.5 nmol, freshly prepared from 5.0 g of the hydrochloride) in chlorofom (50 ml) was added benzyltriethylammonium chloride (6.17 g, 27 mmol ) and potassium carbonate (3.75 g, 27 mmol). The mixture was heated at 50° for 2 hr., then held at room temperature overnight. Water (15 ml ) was added, and the mixture was extracted several times with chloroform. After drying over magnesium sulfate, the solvent was removed by rotary evaporation to give a green-black oil. The crude product was pttrified via column chromatography (silica gel, 5% methanol/dichlorcmethane) and recrystallized from hexane/dichlorcmethane to give 4,4-bis (4-pyridinylmethyl)-2-phenyl-1,3 (2H, 4H) -isoquinolinedione as a pale yellow solid, 3.034 g, 7.2 mmol, 80% yield. Further recrystallization from ethyl acetate/hexane provided off-white crystals of the title ccrpound, m.p.>270°. NMR (200 MHz, CDCl 3 ) δ 3.45 (d, 2H, J=13 Hz); 3.81 (d, 2H, J=13 Hz ); 6.56 (m, 2H); 6.68 (d, 4H, J=6 Hz); 7.41 (m, 3H); 7.53 (m, 1H); 7.91 (d, 2H, J=4 Hz); 8.02 (d, 2H, J=8 Hz,); 8.35 (d, 4H, J=6 Hz). IR (KBr) 1716, 1674, 1600, 1375 cm -1 . Mass spec. 419. Analysis. Calcd. for C 27 H 21 N 3 O 2 : C, 77.31; H, 5.05; N, 10.02. Found: C, 77.12; H, 5.27; N, 9.93.
The compounds of Exanples 240 and 288, and other compounds which can be prepared by the methods described above, are illustrated by the structures represented in Tables V and VI. The tables are intended to illustrate the invention, but not to limit its breadth.
TABLE V__________________________________________________________________________ ##STR639##Ex. Q X V W Z Het.sup.1 Het.sup.2 mp__________________________________________________________________________ °C.240 H.sub.2 N CPh 6-OCH.sub.3 7-OCH.sub.3 ##STR640## ##STR641## 169241 H.sub.2 N C(CH.sub.3) 6-OCH.sub.3 ##STR642## ##STR643##241 H.sub.2 N CH H 7-OCH.sub.3 ##STR644## ##STR645##243 H.sub.2 N OC.sub.2 H.sub.5 5-OCH.sub.3 H ##STR646## ##STR647##244 H.sub.2 N CPh H H ##STR648## ##STR649##245 H.sub.2 N OCH.sub.3 7-OCH.sub.3 6-Br ##STR650## ##STR651##246 H.sub.2 N CPh 5-CF.sub.3 H ##STR652## ##STR653##247 H.sub.2 N C(CH.sub.3) H 7-CH.sub.3 ##STR654## ##STR655##248 H.sub.2 N C( .sub.--m-OCH.sub.3 Ph) H 7-NO.sub.2 ##STR656## ##STR657##249 H.sub.2 N CPh 6-OCH.sub.3 7-OCH.sub.3 ##STR658## ##STR659##250 H.sub.2 N OCH.sub.3 6-OCH.sub.3 H ##STR660## ##STR661##251 H.sub.2 N C( -p-OCH.sub.3 Ph) H 7-OCH.sub.3 ##STR662## ##STR663##252 H.sub.2 N CH H 6-Cl ##STR664## ##STR665##253 H.sub.2 N CPh 5-OCH;.sub.3 8-OCH.sub.3 ##STR666## ##STR667##254 H.sub.2 N C(CH.sub.3) 6-OCH.sub.3 7-OCH.sub.3 ##STR668## ##STR669##255 H.sub.2 N CPh H 7-Br ##STR670## ##STR671##256 H.sub.2 N CPh H 7-CN ##STR672## ##STR673##257 H.sub.2 N C(m-ClPh) H 7-OCH.sub.3 ##STR674## ##STR675##258 H.sub.2 N C(CH.sub.3) 5-CF.sub.3 H ##STR676## ##STR677##259 H.sub.2 N CPh 5-CH.sub.3 7-CH.sub.3 ##STR678## ##STR679##260 H.sub. 2 N OC.sub.2 H.sub.5 5-OCH.sub.3 H ##STR680## ##STR681##261 H.sub.2 N CPh H 7-Ph ##STR682## ##STR683##262 H.sub.2 N CPh 6-OCH.sub.3 7-OCH.sub.3 ##STR684## ##STR685##263 H.sub.2 N CH 6-OCH.sub.3 H ##STR686## ##STR687##264 O CH CH H H ##STR688## ##STR689##265 O CH CH H 7-Br ##STR690## ##STR691##266 O CH CH H 7-OCH.sub.3 ##STR692## ##STR693##267 O CH CH H 7-OH ##STR694## ##STR695##268 O CH CH H 8-NH.sub.2 ##STR696## ##STR697##269 O CH CH 5-NH.sub.2 H ##STR698## ##STR699##270 CH.sub.2 CH CH H H ##STR700## ##STR701##271 CH.sub.2 CH CH H 7-OCH.sub.3 ##STR702## ##STR703##272 OH CH CH 5-NH.sub.2 H ##STR704## ##STR705##273 OH CH CH H 7-Br ##STR706## ##STR707##274 S CH CH H H ##STR708## ##STR709##275 S CH CH H 7-OH ##STR710## ##STR711##276 OCOCH.sub.3 CH CH H H ##STR712## ##STR713##277 OCOPh CH CH H 7-OCH.sub. 3 ##STR714## ##STR715##278 O CH CH H H ##STR716## ##STR717##279 O CH CH H 7-Br ##STR718## ##STR719##280 OH CH CH H 7-OCH.sub.3 ##STR720## ##STR721##281 OH CH CH H H ##STR722## ##STR723##282 OCOCH.sub.3 CH CH 5-NH.sub.2 H ##STR724## ##STR725##283 CHPh CH CH H H ##STR726## ##STR727##284 (Ph)(OH) CH CH H 8-NH.sub.2 ##STR728## ##STR729##285 OCOPh CH CH H H ##STR730## ##STR731##286 S CH CH H 7-Br ##STR732## ##STR733##287 S CH CH H 7-OH ##STR734## ##STR735##__________________________________________________________________________
TABLE VI__________________________________________________________________________ ##STR736##Ex. Q X V W Z Het.sup.1 Het.sup.2 mp °C.__________________________________________________________________________288 O NPh CO H H ##STR737## ##STR738## >270289 H.sub.2 NCOCH.sub.3 CPh 6-OCH.sub.3 7-OCH.sub.3 ##STR739## ##STR740## 278-280 (dec)290 O O CO H H ##STR741## ##STR742##291 O O CO 6-OAc H ##STR743## ##STR744##292 O O CO H 8-OH ##STR745## ##STR746##293 O O CO 5-OCH.sub.3 6-OCH.sub.3 ##STR747## ##STR748##294 O O CH.sub.2 H 7-CH.sub.3 ##STR749## ##STR750##295 O O CH.sub.2 7-OCH.sub.3 8-OCH.sub.3 ##STR751## ##STR752##296 O NCH.sub.3 CO H H ##STR753## ##STR754##297 O NCH.sub.3 CH.sub.2 H H ##STR755## ##STR756##298 H.sub.2 NCOPh CH.sub.2 6-OCH.sub.3 7-OCH.sub.3 ##STR757## ##STR758##299 H.sub.2 NCOCH.sub.3 CHCH.sub.3 6-OCH.sub.3 H ##STR759## ##STR760##300 H.sub.2 NCOCH.sub.3 CH.sub.2 H H ##STR761## ##STR762##301 O O CH.sub.2 5-OCH.sub.3 H ##STR763## ##STR764##302 O O CO 5-OCH.sub.3 8-OCH.sub.3 ##STR765## ##STR766##303 O NPh CO 5-CH.sub.3 H ##STR767## ##STR768##304 O NCH.sub.3 CO H 7-F ##STR769## ##STR770##305 H.sub.2 NCOPh CHPh H 7-OCH.sub.3 ##STR771## ##STR772##306 H.sub.2 NH CO H 7-NO.sub.2 ##STR773## ##STR774##307 H.sub.2 NPh CO 6-CH.sub.3 7-CH.sub.3 ##STR775## ##STR776##308 O NPh CO H 7-CF.sub.3 ##STR777## ##STR778##309 O O CO H 8-NH.sub.2 ##STR779## ##STR780##310 O O CO 5-F 8-F ##STR781## ##STR782##311 O O CH.sub.2 H 7-OCH.sub.3 ##STR783## ##STR784##312 O O CH.sub.2 6-CH.sub.3 8-CH.sub.3 ##STR785## ##STR786##313 O NPh CH.sub.2 H 7-NO.sub.2 ##STR787## ##STR788##314 H.sub.2 NH C O H 7-Br ##STR789## ##STR790##315 H.sub.2 NCOCH.sub.3 CH.sub.2 H 7-OCH.sub.3 ##STR791## ##STR792##316 H.sub.2 NCOPh CHPh 5-OCH.sub.3 8-OCH.sub.3 ##STR793## ##STR794##317 O NPh CO H 8-OEt ##STR795## ##STR796##318 H.sub.2 NCOCH.sub.3 CHCH.sub.3 H 7-OCH.sub.3319 H.sub.2 NCOPh CHPh 6-OCH.sub.3 H320 O O CO H H321 O O CH.sub.2 H H322 H.sub.2 NCOCH.sub.3 CHPh H 7-Ph323 H.sub.2 NCOPh CHPh 5-CH.sub.3 8-CH.sub.3__________________________________________________________________________
EXAMPLE 324
3,3-Bis(4-pyridinylmethyl)-naphtho[1,8-b,c]pyran-2-one
To a solution of naphtho[1,8-b,c]pyran-2(3H)-one [prepared according to O'Brien and Smith, J. Chem. Soc., 2907-17 (1963)], (1.842 g, 10 nmol ) and picolyl chloride (30.5 mmol, freshly prepared by basifying 5.0 g of the hydrochloride) in chloroform (50 ml) was added benzyltriethylanmonium chloride (6.83 g, 30 mmol ) and potassium carbonate (4.15 g, 30 mmol). The mixture was heated at 50° for 5 hr., then cooled to room temperature. Water (15 ml ) was added, and the mixture was extracted several times with chloroform. After drying over magnesium sulfate, the solvent was removed by rotary evaporation to give a green-black oil. The crude product was purified via column chrcmatography (silica gel, 5% methanol/ethyl acetate) and recrystallized from hexmne/dichlorcmethane to give a pale yellow solid, 1,459 g, 3.98 nmol, 40% yield. Further recrystallization from ethyl acetate/hexane provided off-white crystals of the title compound, m.p. 166°-7° . NMR (200 MHz, CDCl 3 ) 6 3.40 (d, 2H, J=13 Hz); 3.84 (d, 2H, J=13 Hz); 6.70 (d, 4H, J=6 Hz); 6.73 (m, 1H); 7.23 (m, 1H); 7.47 (d, 1H, J=8 Hz); 7.65 (d, 2H, J=5 Hz); 7.77 (dd, 1H, J=5,8 Hz); 8.18 (d, 4H, J=6 Hz). IR (KBr) 3033, 1746, 1636, 1601 cm -1 . Mass spec. 366. Analysis. Calcd. for C 24 H 18 N 2 O 2 : C, 78.67; H, 4.95; N, 7.65. Found: C, 78.46; H, 5.08; N, 7.64.
The compound of Example 324, and the other compounds which may be prepared by the methods described above, are illustrated in Table VII. The table is intended to illustrate, but not to limit its breadth.
TABLE VII__________________________________________________________________________ ##STR797##Ex. Q a X W Z Het.sup.1 Het.sup.2 mp °C.__________________________________________________________________________324 O S O H H ##STR798## ##STR799## 166-167325 O S NH H H ##STR800## ##STR801##326 O S NPh H H ##STR802## ##STR803##327 O S CH.sub.2 H H ##STR804## ##STR805##328 Ph D CH H H ##STR806## ##STR807##329 (H)Ph S CH.sub.2 H H ##STR808## ##STR809##330 (H)OH S CH.sub.2 H H ##STR810## ##STR811##331 (H)OCOCH.sub.3 S CH.sub.2 H H ##STR812## ##STR813##332 NOCH.sub.3 S CH.sub.2 H H ##STR814## ##STR815##333 NOH S CH.sub.2 H H ##STR816## ##STR817##334 S S CH.sub.2 H H ##STR818## ##STR819##335 S S O H H ##STR820## ##STR821##336 S CH.sub.2 H H ##STR822## ##STR823##337 S CH.sub.2 H H ##STR824## ##STR825##338 S CH.sub.2 H H ##STR826## ##STR827##339 S CH.sub.2 H H ##STR828## ##STR829##340 H.sub.2 S CH.sub.2 H H ##STR830## ##STR831##341 (H)CHF S CH.sub.2 H H ##STR832## ##STR833##342 F.sub.2 S CH.sub.2 H H ##STR834## ##STR835##343 CH.sub.2 S CH.sub.2 H H ##STR836## ##STR837##344 CHCH.sub.3 S CH.sub.2 H H ##STR838## ##STR839##345 CHPh S CH.sub.2 H H ##STR840## ##STR841##346 (H)C(H)Ph(OH) S CH.sub. 2 H H ##STR842## ##STR843##347 OCH.sub.3 D CH H H ##STR844## ##STR845##348 OC.sub.2 H.sub.5 D CH H H ##STR846## ##STR847##349 O S O H H ##STR848## ##STR849##350 O S NPh H H ##STR850## ##STR851##351 O S CH.sub.2 H H ##STR852## ##STR853##352 (H)OH S CH.sub.2 H H ##STR854## ##STR855##353 CH.sub.2 S CH.sub.2 H H ##STR856## ##STR857##354 O S O 6-OH H ##STR858## ##STR859##355 O S O 5-OAc 4-OAc ##STR860## ##STR861##356 O S CH.sub.2 H H ##STR862## ##STR863##357 O S CH.sub.2 H H ##STR864## ##STR865##358 O S NPh 5-Br H ##STR866## ##STR867##359 O S O H 2-CH.sub.3 ##STR868## ##STR869##360 O S O 7-NO.sub.2 H ##STR870## ##STR871##361 O S NH 5-OH H ##STR872## ##STR873##362 O S NPh 5-Cl 4-Cl ##STR874## ##STR875##363 O S NCH.sub.3 7-CH.sub.3 2-CH.sub.3 ##STR876## ##STR877##364 O S NPh H H ##STR878## ##STR879##365 O S O 5-Cl 4-Cl ##STR880## ##STR881##366 O S NH 7-CH.sub.3 H ##STR882## ##STR883##367 O S O 5-NH.sub.2 H ##STR884## ##STR885##368 CH.sub.2 S CH.sub.2 H H ##STR886## ##STR887##369 CHPh S CH.sub.2 H H ##STR888## ##STR889##370 CHCH.sub.3 S CH.sub.2 H H ##STR890## ##STR891##371 OCH.sub.3 D CH H H ##STR892## ##STR893##372 NOCH.sub.3 S CH.sub.2 H H ##STR894## ##STR895##373 H.sub.2 S CH.sub.2 H H ##STR896## ##STR897##374 H D CH H H ##STR898## ##STR899##375 (H)OH S CH.sub.2 H H ##STR900## ##STR901##376 (H)OAc S CH.sub.2 H H ##STR902## ##STR903##377 S S CH.sub.2 H H ##STR904## ##STR905##378 S S NPh 5-NO.sub.2 H ##STR906## ##STR907##379 NOH S CH.sub.2 H H ##STR908## ##STR909##380 S CH.sub.2 H H ##STR910## ##STR911##381 S CH.sub.2 5-Br H ##STR912## ##STR913##382 S CH.sub.2 5-Cl 4-Cl ##STR914## ##STR915##383 F.sub.2 S CH.sub.2 5-OAc 4-OAc ##STR916## ##STR917##384 Ph D CH H H ##STR918## ##STR919##385 (H)Ph S CH.sub.2 H H ##STR920## ##STR921##__________________________________________________________________________
EXAMPLE 386
11,11-Bis(4-pyridinylmethyl)-5H-dibenzo[a,d]cyclohepten-10(11H)-one, dihydrochloride
To a suspension of sodium hydride (60% oil disper- sion, 1.6 g, 0.04 mol) in 30 ml of dry 1,2-dimethoxyethane was added a solution of 5,11-dihydro-10H-dibenzo[a,d]cyclohepten-10-one [Leonard, et. al., J. Am. Chem. Soc. 77, 5078 (1955)], (4.16 g, 0.02 mol) in 30 ml of dry 1,2-dimethoxyethane dropwise. After all the ketone was added, the mixture was gently heated at reflux for 1 hr. A solution of 4-picolyl chloride was prepared by dissolving 4-picolyl chloride hydrochloride (6.56 g, 0.04 mol) in 100 ml of water, basifying the solution with sodium bicarbonate, and extracting the free base into ether (200 ml). After drying over sodium sulfate, the mixture was filtered, and the ether was removed by rotary evaporation. The residue was immediately redissolved in 1,2-dimethoxyethane (30 ml). This solution was added dropwise to the hot reaction mixture, and the mixture was heated at reflux for 6 h. The reaction mixture was cooled, and methanol (10 ml) was added to decompose excess sodium hydride. The solvents were evaporated, and the residue was dissolved in 200 ml of dichloromethane. The organic phase was washed with water and dried over sodium sulfate. After filtration and rotary evaporation, the crude product was purified by column chromatography (silica gel, 10% methanol/dichloromethane). The product thus obtained was a thick oil. NMR (200 MHz, CDCl 3 ) δ 3.43-3.49 (d, 1H); 3.76-3.82 (d, 1H); 4.16-4.19 (d, 1H); 4.42-4.49 (d, 1H); 4.86-4.93 (m, 2H); 7.02-7.88 (m, 8H); 8.52 (d, 2H); 8.55 (d, 2H). IR (neat) 1675, 1598 cm -1 .
The oil was dissolved in ether and treated with ethereal hydrogen chloride to give the title dihydrochloride salt as an amorphous, hygroscopic solid, m.p. >300°.
The compound of Example 386, and other compounds which can be prepared by the methods described above, are illustrated in Table VIII. The table is intended to illustrate the invention, but not to limit its breadth.
TABLE VIII__________________________________________________________________________ ##STR922##Ex. Q A W Z Het.sup.1 Het.sup.2 mp °C.__________________________________________________________________________386 O CH.sub.2 CH.sub.2 H H ##STR923## ##STR924## >300387 O CH.sub.2 H H ##STR925## ##STR926## >300388 O CH.sub.2 8-Cl H ##STR927## ##STR928##389 O CHCH.sub.3 H H ##STR929## ##STR930##390 O O 8-OCH.sub.3 H ##STR931## ##STR932##391 O NC.sub.2 H.sub.5 H H ##STR933## ##STR934##392 O S H 3-Cl ##STR935## ##STR936##393 O O 9-F 3-Cl ##STR937## ##STR938##394 O S H 1-OCH.sub.3 ##STR939## ##STR940##395 O NCH.sub.2 Ph H H ##STR941## ##STR942##396 CH.sub.2 O H H ##STR943## ##STR944##397 CH.sub.2 S H H ##STR945## ##STR946##398 CH.sub.2 NC.sub.2 H.sub.5 H H ##STR947## ##STR948##399 CHPh CH.sub.2 8-Cl H ##STR949## ##STR950##400 O S H 2-CH.sub.3 ##STR951## ##STR952##401 OH S H 1-CH.sub.3 ##STR953## ##STR954##402 CH.sub.2 S 8-I 3-iPr ##STR955## ##STR956##403 O O H 2-F ##STR957## ##STR958##404 O NH 9-Cl 2-Cl ##STR959## ##STR960##405 CHPh S H 2-OCH.sub.3 ##STR961## ##STR962##406 OCOCH.sub.3 NCH.sub.3 H H ##STR963## ##STR964##407 O O 8-NO.sub.2 1-OCH.sub.3 ##STR965## ##STR966##408 O CH.sub.2 H 2,3-di-OCH.sub.3 ##STR967## ##STR968##409 CH.sub.2 CH.sub.2 H H ##STR969## ##STR970##410 CHPh O H 2-F ##STR971## ##STR972##411 CH.sub.2 Ph NCH.sub.2 Ph H H ##STR973## ##STR974##412 OH N-iPr H H ##STR975## ##STR976##413 OCOCH.sub.3 S 8-Ac H ##STR977## ##STR978##414 O S H 3-CH.sub.2 CO.sub.2 Et ##STR979## ##STR980##415 O O H 3-Br ##STR981## ##STR982##416 O O H 3-NO.sub.2 ##STR983## ##STR984##417 CHPh O H 3-NH.sub.2 ##STR985## ##STR986##418 OCOCH.sub.3 S H 2-I ##STR987## ##STR988##419 O NCH.sub.3 H H ##STR989## ##STR990##420 CH.sub.2 O H 3-C.sub.2 H.sub.5 ##STR991## ##STR992##421 (Ph)(OH) CH.sub.2 H 2,3-di-OAc ##STR993## ##STR994##422 O S H OCH.sub.3 ##STR995## ##STR996##423 CHPh S 8-Ac H ##STR997## ##STR998##424 O O 9-F 3-Cl ##STR999## ##STR1000##425 OCOCH.sub.3 O 8-NO.sub.2 1-OCH.sub.3 ##STR1001## ##STR1002##426 CH.sub.2 CH.sub.2 CH.sub.2 H H ##STR1003## ##STR1004##427 OCOCH.sub.3 CH.sub.2 CH.sub.2 H H ##STR1005## ##STR1006##428 CH.sub.2 (CH.sub.2).sub.3 H H ##STR1007## ##STR1008##429 CHPh CH.sub.2 8-Cl H ##STR1009## ##STR1010##430 O (CH.sub.2).sub.3 H H ##STR1011## ##STR1012##431 OH (CH.sub.2).sub.3 H H ##STR1013## ##STR1014##432 O S H 1-C.sub.2 H.sub.5 ##STR1015## ##STR1016##433 CHPh S H 3-I ##STR1017## ##STR1018##434 CHCH.sub.3 O H 3-NO.sub.2 ##STR1019## ##STR1020##435 CH.sub.2 CH.sub.2 8-Cl H ##STR1021## ##STR1022##436 O (CH.sub.2).sub.0 H H ##STR1023## ##STR1024##437 O (CH.sub.2).sub.0 H H ##STR1025## ##STR1026##438 CH.sub.2 (CH.sub.2).sub.0 H H ##STR1027## ##STR1028##439 CH.sub.2 (CH.sub.2).sub.0 H H ##STR1029## ##STR1030##__________________________________________________________________________
EXAMPLE 440
9,9-Bis(4-pyridinylmethyl)anthrone
A quantity of 35.2 ml (0.44 mole) of 12.5N sodium hydroxide was added dropwise with vigorous stirring during one hour to a mixture of 19.4 g (0.1 mole) of anthrone, 4.5 g (0.02 mole) of benzyltriethyl ammonium chloride, 33.5 g (0.2 mole) of 4-picolylchloride hydrochloride and 200 ml of toluene. During the addition, the temperature rose to 50°. After completion of addition, the mixture was vigorously stirred at 60° for six hours. Then 200 ml of water was added in one portion, the layers were separated and product crystallized out of the toluene layer as it cooled to room temperature. After cooling in an ice bath, the solid was filtered, washed with water, taken through an acid-base wash, and decolorized with 35 g of Magnesol® to yield 28 g of product, melting at 205°-206°. This was recrystallized from toluene (1.0 g/22.0 ml toluene) to yield 21 g of title product melting at 207°-208°.
EXAMPLE 441
9,9-Bis(4-pyridinylmethyl)anthrone dihydrochloride
A quantity of 3 ml of 25% hydrochloric acid in ethanol was added to a solution of 2.0 g of 9,9-bis(4-pyridinylmethyl)anthrone in 10 ml of ethanol plus 5 ml of isopropanol. The solution was heated briefly to boiling and allowed to cool, during which time the product crystallized out as colorless crystals. After cooling at 0° for one hour, the crystals were filtered off, washed with a small amount of isopropanol, and recrystallized from ethanol isopropanol to yield 2.0 g of the title product, m.p. 275°-277°.
EXAMPLE 442
9,9-Bis(4-pyridinylmethyl)xanthane
An amount of 5.1 g (0.028 mole) of xanthane was dissolved in 50 ml of dry tetrahydrofuran and cooled to -30°. 3.11 g (0.029 mole) of lithium diisopropylamide was weighed into a dropping funnel and dissolved in 30 ml of tetrahydrofuran. This solution was added dropwise during 30 minutes to the xanthane solution at -30°. After completion of addition, the reaction was warmed to room temperature and kept there for 15 minutes. It was recooled to -30° and 5.05 g (0.03 mole) of 4-picolylchloride in 15 ml of tetrahydrofuran was added dropwise during 30 minutes at -30°. After completion of addition, the reaction mixture was warmed to room temperature and kept there for 30 minutes. Again the reaction was cooled to -30° and a further batch of 3.11 g (0.029 mole) of lithium diisopropylamide in 30 ml of tetrahydrofuran was added dropwise during 30 minutes at -30°. After completion of addition, it was warmed to room temperature and kept there for 15 minutes. After cooling again to -30°, a further quantity of 4-picolylchloride (0.03 mole) in 15 ml of tetrahydrofuran was added dropwise during 30 minutes at -30°. After completion of addition, the reaction mixture was warmed to room temperature and kept there until thin layer chromatography showed completion of reaction, about ten hours. Excess anion was carefully destroyed by the addition of 50 ml of saturated ammonium chloride solution and the tetrahydrofuran was evaporated in vacuo. The residue was taken up in methylene chloride and product was extracted with 3×100 ml of 0.5N hydrochloric acid. The combined hydrochloric acid portions were made basic with 50% sodium hydroxide to ph 12 and the product was extracted with methylene chloride. The methylene chloride extracts were combined, washed with water, dried (MgSO 4 ), filtered and evaporated. The crude product was triturated with ether to produce 2.0 g of product. This material was chromatographed on silica with hexane/ethylacetate (70:30). Fractions containing product were combined and evaporated to yield 1.7 g of disubstituted product. This was recrystallized from chlorobutane to yield 1.1 g, m.p. 212°-213°, of titled dialkylated xanthane.
EXAMPLE 443
9,9-Bis(4-pyridinylmethyl)fluorene
A quantity of 3.0 g (18.0 mmole) of fluorene was dissolved in 20 ml of tetrahydrofuran (THF) and cooled to -20° under nitrogen. n-Butyllithium (11.5 ml, 1.57M) was added dropwise during 15 minutes. After stirring for 30 minutes, this was cannulated into a solution of 18.0 mmole of 4-picolylchloride in 20 ml of THF at -78°. After allowing the reaction to warm to room temperature, thin layer chromatography (TLC) (ether-hexane 1:1) showed disappearance of fluorene. The reaction was cooled again to -20° and a second batch of 11.5 ml of n-butyllithium (1.57M) was added dropwise during 15 minutes. After stirring for 30 minutes, this reaction mixture was cannulated into a solution of 18.0 mmole of 4-picolylchloride in 20 ml of THF at -78°. The resulting mixture was allowed to warm to room temperature and stirred at ambient temperature overnight (17 hours). The reaction was quenched with saturated ammonium chloride and extracted with ether. The crude combined extracts were chromatographed with methylene chloride/methanol (30:1) to (25:1) yielding 2.9 g of pure title dialkylated fluorene. HRMS: 348.1615 (M + ), 256.1131 (M--C 6 H 6 N).
EXAMPLE 444
2-Nitro-9,9-Bis(4-pyridinythyl)fluorene
A quantity of 0.5 g (2.37 mole) of 2-nitrofluorene, 0.86 g (5.2 mmole) of 4-picolylchloride hydrochloride, 60 mg of cetyl tri-n-butyl phosphonium bromide and 10 ml of toluene were combined and heated to 50°. With vigorous stirring 5.0 ml of 50% sodium hydroxide was added dropwise at 50° during 30 minutes. Heating was continued for one hour. A quantity of 10 ml of water was added, the reaction cooled to room temperature and partitioned with methylene chloride. The combined organic layer was extracted with 3×25 ml of 0.5N HCl and the combined aqueous extracts basified with sodium hydroxide. The precipitated product was chromatographed (silica, methylene chloride/methanol 100:1) to yield 0.6 g of the title product, m.p. 260°-264°. HRMS-measured, 393.1465; calculated, 393.1477; assigned C 25 H 19 N 3 O 2 (M + ).
The dialkylated fluorene was converted to its dihydrochloride salt by dissolving 0.5 g of the base in ethanol and adding 2 ml of 25% hydrochloric acid in ethanol. Addition of ether produced product, which was recrystallized from methanol/ethyl acetate to yield 0.4 g, m.p., >300°.
EXAMPLE 445
9,9-Bis(4-pyridinylmethyl)thioxanthene
Part A: 9-(4-pyridinylmethyl)thioxanthene
A quantity of 4.96 g (0.025 mole) of thioxanthane was dissolved in 25 ml of tetrahydrofuran (THF) and cooled to -20°. With stirring, 18 ml of a 1.4M solution of potassium hexamethyldisilazide was added dropwise during 30 minutes. After completion of addition, the reaction mixture was warmed to room temperature and it was kept there for 15 minutes. It was then cooled to -20° and a solution of 4-picolylchloride (28.0 mmoles) base in 20 ml of THF was added dropwise during 30 minutes at -20°. After addition, the reaction mixture was warmed to room temperature and kept there for one hour. The reaction was quenched with 50 ml saturated ammonium chloride and evaporated. The residue was extracted with methylene chloride, put through an acid-base sequential wash with 0.5N hydrochloric acid and 50% sodium hydroxide. The organic layer was dried (MgSO 4 ) and evaporated to yield 5.1 g of the titled monoalkylated product.
Part B: 9,9-Bis(4-pyridinylmethyl)thioxanthene
A quantity of 0.38 g (8.0 mmole) of 50% sodium hydride oil dispersion was added slowly during 15 minutes to 20 ml of ethyl sulfoxide at room temperature. After completion of addition, the reaction mixture was heated at 45° for 30 minutes. It was cooled to 15° and a solution of 2.3 g (8.0 mmole) of 9-(4-pyridinylmethyl)thioxanthene in 10 ml of dimethylsulfoxide was added dropwise during 15 minutes at room temperature. After completion of addition, the reaction mixture was stirred 30 minutes at room temperature. Then a solution of 4-picolylchloride (8.75 mmole) in 5 ml of dimethylsulfoxide was added dropwise during 30 minutes at ambient temperature. The reaction was then heated at 40° for 30 minutes. The reaction was quenched by addition of water (50 ml). Trituration of the precipitated oil yielded a crystalline solid, which was filtered off, washed with water and dried. The tan solid was dissolved in benzene and decolorized by stirring with 1 g of Magnesol® for 30 minutes. Filtration and evaporation yielded a colorless product (2.0 g) which was recrystallized from ethylacetate, m.p., 201.4°-203.4°.
EXAMPLE 446
9,9-Bis(4-pyridinylmethyl)-1-methylfluorene dihydrochloride
The title compound was prepared following the procedure of Example 5 from 0.5 g (2.77 mmole) of 1-methylfluorene, 1.0 g of picolylchloride hydrochloride, 4 ml sodium hydroxide (50% solution), 68 mg of cetyltri-n-butyl phosphonium bromide, and 4 ml toluene by reaction at 50° for 1 hr. The product was chromatographed (silica, CH 2 Cl 2 /CH 3 OH, 100:1), m.p. (dihydrochloride) >300°, NMR (200 MHz, CDCl 3 ) δ: 2.82(s,3H), 3.60(dd,4H), 6.39(m,4H), 7.0-7.5(m,7H--arom.), 8.0(m,4H). HRMS calculated for C 26 H 22 N 2 : 362.1783 Found: 362.1779
EXAMPLE 447
9,9-Bis(4-pyridinylmethyl)-2-bromofluorene dihydrochloride
The title compound was prepared following the procedure of Example 5 from 1.0 g (4.08 mmole) of 2-bromofluorene, 1.5 g of 4-picolylchloride hydrochloride, 100 mg of cetyl tri-n-butyl phosphonium bromide, 20 ml of 50% sodium hydroxide solution, and 20 ml toluene by reaction at 50° for 1 hr. The product was chromatographed (silica, CH 2 Cl 2 /CH 3 OH, 100:1), m.p. (dihydrochloride) >300° NMR (200 MHz, CDCL 3 ) δ: 3.39(dd,4H), 6.48(d,4H), 7.10-7.67 (m, 7H-arom.), 8.12(d,J=5.7 Hz,4H). HRMS calculated for C 25 H 19 BrN 2 : 426.0758 Found: 426.0758
EXAMPLE 448
9,9-Bis(4-pyridinylmethyl)-2-fluorene
1.68 g (4.27 mmole) of 9,9-bis(4-pyridinylmethyl)-2-nitrofluorene was suspended in 5 ml of ethanol/water (1:1) and 1.43 g of powdered iron was added. The mixture was heated to boiling and 0.3 ml conc. hydrochloric acid was added dropwise. After completion of addition, the mixture was refluxed 2 hrs. The cooled mixture was basified with KOH, iron hydroxide filtered off and the filtrate evaporated. The residue was dissolved in ether--CH 2 Cl 2 (3:1), washed with water, saturated sodium chloride, dried (MgSO 4 ) and evaporated to yield 1.28 g of the title product. NMR (CDCl 3 , 200 MHz) δ: 3.33(s,4H), 6.53(dd,4H), 6.60(d,J=2.0 Hz,1H), 6.79(d,J=2.0 Hz,1H), 7.18(m, 4H), 7.37(dd, 1H), 8.11(dd,4H), m.p. (trihydrochloride) >300°. HRMS calculated for C 25 H 21 N 3 : 363.1735 Found: 363.1728.
EXAMPLE 449
9,9-Bis(4-pyridinylmethyl)-2-acetamido-fluorene dihydrochloride
0.38 g of 9,9-bis(4-pyridinylmethyl)-2-aminofluorene was added to 4 ml acetic anhydride and heated at 70° overnight. The reaction was quenched into a pH 7 buffer and extracted with ethyl acetate. Following an acid-base wash, the product was chromatographed (silica, CH 2 Cl 2 /MeOH, 10:1) to yield 0.3 g after conversion to the dihydrochloride, m.p., >300°.
EXAMPLE 450
9,9-Bis(4-pyridinylmethyl)-2-acetylfluorene dihydrochloride
The title compound was prepared following the procedure of Example 1 from 5.0 g (24 mole) of 2-acetylfluorene, 10 g of 4-picolylchloride hydrochloride, 120 ml benzene, 200 mg of benzyltriethylammonium chloride, and 20 ml of 50% sodium hydroxide by reaction solution at 20° for 17 hrs. The title compound was obtained after an acid-base wash and crystallization from benzene-hexane (Magnesol®), m.p., >300°. NMR (CDCl 3 , 200 MHz) δ: 2.68(S,3H), 3.46(S,4H), 6.44(d,J=5.9 Hz,4H), 7.29-7.87(m, 6H), 8.05(d,J=5.9 Hz,4H), 8.22(d, 1H). HRMS calculated for C 27 H 22 N 2 O: 390.1732 Found: 390.1720.
EXAMPLE 451
9,9-Bis(4-pyridinylmethyl)-2-fluorofluorene hydrochloride
The title compound was prepared following the method of Example 1 from 4.0 g (21.74 mmole) of 2-fluorofluorene, 8.92 g of 4-picolylchloride hydrochloride, 120 ml of toluene, 200 mg of benzyltriethylammonium chloride, and 20 ml of 50% sodium hydroxide by reaction at 22° for 17 hrs. The product was chromatographed (silica, CH 2 Cl 2 /MeOH, 10:1) to yield 2.9 g which was recrystallized (ethanol-acetone) and converted to the dihydrochloride, m.p.>300°.
EXAMPLE 452
9,9-Bis(4-pyridinylmethyl)-2-difluoromethyl fluorene
The title compound was prepared following the method of Example 1 from 0.6 g (2.78 mole) of 2-difluoromethylfluorene, 1.14 g of 4-picolylchloride hydrochloride, 32 mg benzyltriethylammonium chloride, 4 ml of 50% sodium hydroxide solution, and 25 ml of toluene by reaction at 50° for 6 hrs. The product was chromatographed (silica, CH 2 Cl 2 /MeOH, 10:1) to yield 0.5 g, m.p. >300°; NMR (CDCl 3 , 200 MHz) δ: 3.43(S,4H), 6.45(d,J=5.7 Hz,4H), 6.74(t,J=56.6 Hz,1H), 7.26-7.70(m.arom.), 8.1(d,J=5.7 Hz,4H). HRMS calculated for C 26 H 20 N 2 F 2 : 398.1595 Found: 398.1583.
EXAMPLE 453
9,9-Bis(4-pyridinylmethyl)-2-(1-hydroxyethyl)fluorene
To 300 mg of 9,9-bis(4-pyridinylmethyl)-2-acetylfluorene was dissolved in 5 ml of ethanol cooled to 0° was added 100 mg of sodium borohydride. The reaction mixture was warmed to room temperature overnight, quenched with water and methanol and the solvents evaporated. The residue was partitioned between ethyl acetate and 1N NaOH, washed with water, brine, dried (MgSO 4 ) and evaported. Recrystallization from ethanol yielded product. NMR (CDCl 3 , 200 MHz) δ: 1.50(d,J=6.5 Hz,3H), 3.39(s,4H), 4.92(q,J=6.4 Hz,1H), 6.43(2d,4H), 7.08-7.58(m, arom.), 7.87(d,2H), 7.97(d,2H).
EXAMPLE 454
9,9-Bis(4-pyridinylmethyl)-2-methylfluorene
The title compound was prepared following the procedure of Example 5 from 0.95 g of 2-methylfluorene, 2.17 g of 4-picolylchloride hydrochloride, 50 mg of cetyl(Bu) 3 PBr, 30 ml toluene, and 5 ml 50% NaOH by reaction at 50° for 6 hrs. The material was chromatographed to yield 0.2 g product. NMR (CDCl 3 , 200 MHz) δ: 2.47(s,3H), 3.37(s,4H), 6.49(d,J=5.3 Hz,4H), 7.03-7.45(arom.H), 8.09(d,4H). HRMS calculated for C 26 H 22 N 2 : 362.1783 Found: 362.1778
EXAMPLE 455
9,9-Bis(4-pyridinylmethyl)-2-ethylfluorene
The title compound was prepared following the procedure described in Example 5 from 2.39 g (12.32 mmole) of 2-ethylfluoroene, 4.0 g of 4-picolylchloride .HCl, 110 mg of cetyl Bu 3 PBr, 20 ml of 50% NaOH, and 30 ml of toluene by reaction at 50° for 6 hrs. The product was chromatographed (silica, CH 2 Cl 2 /MeOH,95:5) to yield 2.0 g of product. NMR (CDCl 3 , 200 MHz) δ: 1.30(t,J=7.8 Hz,3H), 2.74(q,J=7.6 Hz,2H), 3.37(s,4H), 6.49(d,J=5.9 Hz,4H), 7.04-7.48(m, arom. 7H), 8.09(d,J=5.4 Hz,4H). HRMS calculated for C 27 H 24 N 2 : 376.1940 Found: 376.1927
EXAMPLE 456
9,9-Bis(4-pyridinylmethyl)-2-methylfluorene dihydrochloride
The title compound was prepared following the procedure of Example 5 from 1.8 g (9.2 mmole) of 2-methoxyfluorene, 3.0 g of 4-picolylchloride.HCl, 20 ml of 50% NaOH, 100 n/of cetyl Bu 3 PBr, and 30 ml of toluene by reaction at 50° for 6 hrs. The material was chromato-graphed to yield 1.6 g of product. δ: 3.37(s,4H), 3.89(s,3H), 6.52(broad, 4H), 6.80(m,1H), 7.01(d,J=2.1 Hz,1H), 7.26(m,5H), 7.45(d,J=7.5 Hz, 1H), 8.11(broad, 4H).
EXAMPLE 457
9,9-Bis(3-pyridinylmethyl)fluorene
The title compound was prepared following the procedure described in Example 5 from 10.0 mmole of fluorene, 22.0 mmole of 3-picolylchloride hydrochloride, 2.0 mmole of cetyl tri-n-butyl phosphonium bromide, 20 ml of 50% sodium hydroxide and 40 ml of toluene by reaction at 50° for 6 hrs. The material was chromatographed (silica, CH 2 Cl 2 /MeOH,95:5) to yield 2.6 g (70%), m.p. 137°-138°. δ: 3.41(s,4H), 6.71-6.97(m,4H), 7.17-7.35(tt,6H), 7.50-7.54(d,J=6.9 Hz,2H), 7.91(s,2H), 8.12-8.15(d,J=5.4 Hx,2H). HRMS calculated for C 25 H 20 N 2 : 348.1632 Found: 348.1626
EXAMPLE 458
9,9-Bis(4-pyridinylmethyl)-1,4-dimethylanthrone
The title compound was prepared following the procedure of Example 5 from 9.34 g (42 mmole) of 1,4-dimethylanthrone, 15.1 g (92 mmole) of 4-picolylchloride.HCl, 14 ml of 50% sodium hydroxide, 1.91 g of cetyl tri-n-butyl phosphonium bromide and 40 ml of toluene by reaction at 60° for 6 hrs. to form 2.9 g of monoalkylated anthrone. The monoalkylated product was reacted with dimsyl sodium (prepared from 10 mmole of sodium hydride, 0.48 g, in 20 ml DMSO), and 1.27 g (10 mmole) of 4-picolylchloride base at 40° for 2 hrs. The reaction was quenched with water and chromatographed (silica, CH 2 Cl 2 /MeOH,10:1) to yield 2.0 g of the title bisalkylated product, m.p. 211°-213°.
EXAMPLE 459
9,9-Bis(4-pyridinylmethyl)-4,5-dichloroanthrone
The title compound was prepared following the procedure of Example 1 from 26.3 g (0.1 mole) of 1,8-dichloroanthrone and 4,5-dichloroanthrone, 32.8 g (0.2 mole) of 4-picolylchloride.HCl, 2.28 g (0.01 mole) of benzyltriethylammonium chloride, 32 ml of 50% sodium hydroxide and 75 ml toluene by reaction at 50° for 6 hrs. The product was chromatographed (silica, CH 2 Cl 2 /MeOH 100:1) to yield 15.7 g, m.p. 170°-172°. NMR (CDCl 3 , 200 MHz) δ: 3.53(s,4H), 6.43(d,4H J=6.1 Hz), 7.33-751(m,arom. 6H), 8.3(d,J=6.2 Hz,4H) HRMS calculated for C 26 H 18 N 2 OCl 2 : 444.0796 Found: 444.0799. Also isolated from above was 9-(4-pyridinylmethyl)-1,8-dichloroanthrone.
EXAMPLE 460
9,9 -Bis(4-pyridinylmethyl)-1,8-dichloroanthrone
The title compound was prepared following the procedure of Example 1 from 9-(4-pyridinylmethyl)-1,8-dichloroanthrone (3.54 g, 10 mmole), 1.64 g (10 mmole) of 4-picolylchloride .HCl, 0.23 g of benzyltriethylammonium chloride, 1.6 ml of 50% sodium hydroxide and 30 ml toluene by reaction at 60° for 6 hrs. The product was chromatographed (silica, EtOAc/Hexane, 30:70) to yield 0.5 g of product. δ: 4.66(s,4H), 6.33(d,J=6.1 Hz,4H), 7.45(t,J=6.6 Hz,2H-arom) 7.79(d,J=7.1 Hz,2H-arom), 8.01(d,J=6.3 Hz,4H), 8.13(d,J=7.1 Hz2H). HRMS calculated for C 26 H 18 N 2 OCl 2 : 444.0796 Found: 444.0806.
EXAMPLE 461
9,9-Bis(3-pyridinylmethyl)anthrone
The title compound was prepared following the procedure of Example 1 from 20.0 mmole of anthrone, 44.0 mmole of 3-picolylchloride hydrochloride, 2.0 mmole of benzyl triethylanmonium chloride, 40 ml of 50% sodium hydroxide, and 50 ml toluene at 60 for 2 hrs. The product was chromatographed (silica, EtOAc/Hexane, 70:30) to yield 1.43 g of product. NMR (CDCl 3 , 200 MHz) δ: 3.77(s,4H), 6.49(d,J=6.9 Hz,2H-arom), 6.66(dd, 7.91,J=4.8 Hz,2H-arom), 7.48(t,J=7.4 Hz,2H-arom), 7.56(m, 1H), 7.79(t,J=7.3 Hz,2H), 8.03(d,J=7.0 Hz,2H), 8.16(mJ=1.8 Hz,4H). HRMS calculated for C 26 H 20 N 2 O: 376.1584 Found: 376.1573
EXAMPLE 462
9,9-Bis(4-pyridinylmethyl)anthrol
To 5 g of 9,9-Bis(4-pyridinylmethyl)anthrone dissolved in 150 ml ethanol was added 2.5 g (0.066 mmole) of sodium borohydride. Addition was portionwise over 1 hr. at ambient temperature. After completion of addition, the solution was refluxed 12 hrs., then stirred overnight (14 hrs.). The reaction was quenched with water, evaporated and partitioned between methylene chloride and water. The organic layer was washed with water, dried (MgSO 4 ) and evaporated to obtain 4.9 g of title product which was recrystallized from 1-propanol to yield 3.12 g, m.p. 196°-197°.
EXAMPLE 463
9,9-Bis(4-pyridinylmethyl)anthrone oxime
To 2.5 ml ethanol was added 500 mg (1.33 mmole) 9,9-bis(4-pyridinylmethyl)anthrone. To the resulting mixture was added 316 mg (5.3 mmole) of hydroxylamine hydrochloride, followed by 2.5 ml pyridine. The resulting solution was refluxed for 24 hrs. Solvents were evaporated, and the residue was triturated with 10 ml water. The solid obtained was recrystallized from ethanol to yield 300 mg of product, m.p. 226°-227°.
EXAMPLE 464
9,9-Bis(4-pyridinylmethyl)cyclopentadienylphenanthrene
The title compound was prepared following the procedure of Example 1 from 5.0 g (0.0263 m) of cyclopentadienylphenanthrene, 9.51 g (58 mmole) 4-picolylchloride .HCl, 11.1 ml 50% sodium hydroxide, 1.2 g benzyltriethylammonium chloride, and 100 ml toluene by reaction at 50° for 6 hrs. The material was chromatographed (silica, EtOAc/MeOH,95:5) to yield 1.9 g of product, m.p. 201°-202°.
EXAMPLE 532
5,5-Bis(4-pyridinylmethyl)-5H-cyclopenta[2,1-b:3,4-b']dipyridine
The title compound was prepared following the procedure of Example 1 from 0.43 g (2.56 mmole) of 4,5-diazafluorene, 0.84 g of 4-picolylchloride hydrochloride, 29.0 mg of benzyltriethylammonium chloride, 3 ml of 50% sodium hydroxide, and 30 ml toluene by reaction at 50 for 6 hrs. The crude product was chromatographed (Ethylacetate/Methanol, 99:1) and recrystallized from isopropyl alcohol. NMR (CDCl 3 , 200 MHz) δ: 3.42(s,4H), 6.52(d,J=5.7 Hz,4H), 7.33(dd,2H), 7.85(d,2H), 8.16(d,J=5.6 Hz,4H), 8.61(d,2H).
EXAMPLE 560
9,9-Bis(4-pyridinylmethyl)cyclopenta-[1,2-b:4,3-b']-dipyridine
Part A: Preparation of 5-methoxy-4,7-phenanthroline
Equipment: 5-liter, multi-neck, round bottom flask fitted with a mechanical stirrer, condenser, thermometer and nitrogen inlet. Provisions should be made so that the flask can be lowered easily into an ice bath at the proper time and then replaced with a heating mantle. To the flask was added 875 ml of water, followed by a solution of 322 g of meta-nitrobenzene sulfonic acid in 828 g of sulfuric acid, keeping the temperature below 40°. Then 161 g (0.68 mole) of 2-methoxy-1,4-phenylenediamine sulfate hydrate was added in one batch with stirring. With strong cooling, 430 g of sulfuric acid was very carefully added with vigorous stirring at a temperature below 50°. Finally, 575 g (6.25 mole) of glycerin was added rapidly through a dropping funnel. The mixture was gently refluxed for 6 hours (boiling point 133°), then cooled to room temperature and poured into 6000 ml of ice and 1000 ml water. The solution was basified to pH 10 with 50% sodium hydroxide, adding more ice if necessary to keep the temperature below 20°. The pH 10 mixture was extracted with chloroform, dried with sodium sulfate and evaporated, yielding 128 g of a black thick oil which soon solidifed. This methoxy-4,7-phenanthroline was taken directly to the next step.
Part B: Hydrolysis of 5-methoxy-4,7-phenanthroline to 4,7-phenanthrolin-5,6-quinone
To a 3-liter, multi-neck, round bottom flask was added 641 ml of concentrated sulfuric acid. Next, 385 ml of fuming nitric acid (d=1.5 g/ml) was added, keeping the internal temperature below 40°. Heating 128 g (0.61 mole) of 5-methoxy-4,7-phenanthroline with a heat gun to liquify it makes it possible to add it to the acid mixture through a dropping funnel during about one hour. A flameless heat gun was used to keep the contents of the dropping funnel liquid. After completion of addition, the solution was refluxed 13 hours (bp about 90°). The original black solution gradually changed to a yellow-orange color after 13 hours. The solution was next cooled to room temperature and poured into 5 liters of ice. It was neutralized to pH 4-5 with 50% sodium hydroxide solution, adding additional ice to keep the temperature below 10°. The precipitated 4,7-phenanthrolin-5,6-quinone was filtered off, washed with water and dried in a vacuum oven under nitrogen at 100°. Yield 72.9 g.
Part C: Preparation of 1,8-diazafluoren-9-one
To a solution of 200 ml of 10% sodium hydroxide was added 10 g (47 mmole) of 4,7-phenanthrolin-5,6-quinone. This was heated in a water bath at 70°-80° with magnetic stirring for 2 hours. Then the reaction was cooled in an ice bath and acidified with concentrated hydrochloric acid to pH 4-5, keeping the mixture below 20°. The precipitate of side product, 5,6-dihydroxy-4,7-phenanthroline was filtered off and the filtrate was extracted with 5×50 ml of chloroform. After drying with sodium sulfate, the solvent was evaporated, yielding 2.6 g of 1,8-diazafluoren-9-one, m.p. 233°-234.5°.
Part D: Preparation of 1,8-diazafluorene
Procedure followed in Example 608, Part C:
A quantity of 3.62 g (20 moles) of 1,8-diazafluoren-9-one and 3.2 g (0.1 mole) of hydrazine was heated in 30 ml of diethyleneglycol at 100° for 1 hour, then heated rapidly to 200 and kept there for one hour (or until TLC showed the complete disappearance of starting material). Yield 2.6 g.
Part E: Preparation of 9,9-Bis(4-pyridinylmethyl)-cyclopenta-[1,2-b:4,3-b ']dipyridine
The alkylation procedure described in Example 608, Part D, was followed.
1.50 g (8.93 mmole) of 1,8-diazafluorene was alkylated in the presence of 1.07 g (22.3 mmole) of 50% sodium hydride by 3.54 g (21.6 mmole) of picolylchloride in 20 ml of benzene and 10 ml of tetrahydrofuran at 55 until TLC showed the reaction was complete (ethyl acetate methanol--90:10)--product Rf 0.1, starting diazafluorene Rf 0.22.
The reaction was decomposed as usual with saturated ammonium chloride. The crude product was flash chromatographed with ethyl acetate, then recrystallized from acetone. Allowed to crystallize overnight, the pure white crystals were filtered off, washed with a small quantity of cold acetone, and dried to yield 940 mg, m.p. 244°-247°. Rf 0.1. ##STR1031##
Difference 0.0003; for C 23 H 18 N 4 .
NMR(200 MHz) δ:3.796(s,4H, (--CH 2 --pyridyl); 6.391-6.421 (dd,4H,β-pyridyls); 7.140-7.203(m, 2H,3-H and 6-H of 1,8-diazafluorene--e.g., meta to the nitrogens); 7.477-7.523(dd,2H,4-H and 5-H of diazafluorene); 8.006-8.014 (d,4H,α-pyridyls); 8.676-8.709(dd,2H,2-H and 7-H of diazafluorene).
EXAMPLE 608
9,9-Bis(4-pyridinylmethyl)indeno-[2,1-b]pyridine
Part A:
A quantity of 47.5 g (0.265 mole) of commercial 4-azaphenanthrene was dissolved in 750 ml glacial acetic acid. With vigorous stirring, 110 g (0.33 mole) of iodine pentoxide was added. The mixture was heated to gentle reflux and kept there for 6 hours.
At the end of this time, the reaction mixture was cooled to room temperature and excess iodine pentoxide was filtered off. The solution was rotary evaporated and the residue was taken up in benzene. This solution was washed with sodium thiosulfate to remove excess iodine. It was then dried with sodium sulfate, filtered and evaporated to yield 20 g of 4-phenanthren-5,6-dione. Recrystallization from ethanol gave 13.0 g of pure dione, m.p. 262°.
Part B: Conversion of 4-azaphenanthren-5,6-dione to 1-azafluoren-9-one.
A solution of 4-azaphenanthren-5,6-dione, 10.76 g (51 mmole) was added to 200 ml of 10% sodium hydroxide in an erlenmeyer flask. This was placed in a bath and heated to 70°-80° for 2 hours. When TIE showed the reaction was finished, it was cooled to room temperature and extracted with chloroform. This was dried with sodium sulfate and evaporated to yield a tan product. Flash chromatography with ethyl acetate yielded 4.79 g, m.p 129°-130°, of pure 1-azafluoren-9-one.
Part C: Reduction of 1-azafluoren-9-one to 1-azafluorene
4.6 g (25.4 mmole) of 1-azafluoren-9-one was added to a solution of 9 ml (0.28 mole) of hydrazine and 50 ml of diethyleneglycol. Heating was started and the temperature was kept at 100° for 15 minutes, then raised to 195° and kept there for 1 hr. TLC showed the reaction was complete. The reaction solution was cooled to below 100 and poured into 300 ml of ice water. The aqueous phase was saturated with salt and extracted with 8×100 ml ether. The ether was dried with sodium sulfate and evaporated to yield 3.73 g of crude product. This was dissolved in hexane and treated with Magnesol, filtered and evaporated and finally recrystallized from hexane to yield 2.83 g of pure 1-azafluorene.
Part D: Preparation of 9,9-Bis-(4-pyridinylmethyl)indeno[2,1-b]pyridine
2.0 g (42 mmole) of 50% sodium hydride was suspended in a 250 ml, 4-neck, round-bottom flask fitted with nitrogen inlet, condenser, thermometer, addition funnel, magnetic stirrer, and 25 ml of sodium dried tetrahydrofuran (THF) containing 2.5 g (15 mmol) of 1-azafluorene. The mixture was allowed to stir at room temperature for one hour. 6.6 g (40 mmole) of4-picolylchloride hydrochloride was dissolved in the minimum amount of water and cooled to 0°-5°. Being very careful to keep the temperature below 5°, it was basified with ammonium hydroxide, quickly extracted with benzene, dried with potassium carbonate and filtered. The benzene solution of 4-picolyl chloride was added to the reaction mixture during 15 min. After completion of addition, the mixture was heated to 60° until TLC showed completion of reaction (ETOAc-CH 3 OH; 90:10) Rf 0.13. Rf 0.13. The reaction mixture was cooled and decomposed with saturated ammonium chloride solution. The layers were separated and the organic phase extracted with benzene. This was dried with potassium carbonate and evaporated to yield 6.0 g crude product. Flash chromatography (ethyl acetate) yielded 4.0 g of product which was recrystallized from butyl chloride to yield 2.49 g, m.p. 204.7°-206.0°. HRMS calculated mass 349.1528, difference 0.0004, C 24 H 19 N 3 . NMR (200 MHz, CDCl 3 ) δ 3.394-3.718[dd,4H,(--CH 2 -pyridyl]; 6.437(d,4H, β-pyridyls); 7.107-7.635 (m,6H,aromatic); 8.027-8.057d, 4H, α-pyridyls); 8.589-8.621 (dd,1H,α--CHN--azafluorene).
EXAMPLE 611
5,5-Bis(4-pyridinylmethyl)indeno-[1,2-b]pyridine
Part A: Preparation of 1-azaphenanthren-5,6-dione
Following the procedure described in Example 608, Part A, 37.5 g (0.153 mole) of commercial 1-azaphenanthrene, 55 g (0.165 mole) of iodine pentoxide in 600 ml glacial acetic acid were refluxed 2 hours. Identical workup yielded 8.4 g, m.p. 215°-216°.
Part B: Conversion of 1-azaphenanthren-5,6-dione to 4-azafluoren-9-one
Following the procedure described in Example 608, Part B, 8.2 g (0.04 mole) of 1-azaphenanthren-5,6-dione and 165 ml of 10% sodium hydroxide were heated in a bath at 80°-90° for 3 hours. Identical workup yielded 3.88 g, m.p. 140°-142° of pure 4-azafluoren-9-one.
Part C: Reduction of 4-azafluoren-9-one to 4-azafluorene
Following the procedure described in Example 608, Part C, 3.45 g (19 mmole), of 4-azafluoren-9-one, 6.8 g (0.213 mole) of hydrazine in 50 ml of diethyleneglycol were combined and heated to 205° over a 30-minute period. TLC showed no remaining starting material. Identical workup yielded 2.33 g of pure 4-azafluorene, Rf-0.46 (hexane ethylacetatetriethylamine, 29.75:69.46:0.79).
Part D: Preparation of 5,5-Bis(4-pyridinylmethyl)-indeno-[1,2-b]pyridine
Following the procedure described in Example 608, Part D, alkylation of 2.1 g (12.6 mmole) of 4-azafluorene, in the presence of 1.51 g (31.45 mmole) of 50% sodium hydride with 5.0 g (30.4 mmole) of 4-picolyl-chloride yielded 2.8 g. Flash chromatography with ethyl acetate yielded 2.0 g of material containing a small amount of color. Recrystallization from butyl chloride yielded 1.5 g of pure compound, m.p. 163°-164°.
HRMS 349.1579 (calculated for C 24 H 19 N 3 )
HRMS 349.1570 (observed)
NMR(200 MHz, CDCl 3 ) δ 3.407(s,4H--CH 2 --pyridyl); 6.498-6.529(dd,4H,β-pyridyls); 7.149-7.770(m, 6H,aromatic); 8.137-8.167(d,4H,α-pyridyls); 8.437-8.469(dd, 1H, α--CHN--azafluorene).
EXAMPLE 624
9,9-Bis(4-pyridinylmethyl)cyclopenta-[1,2-b:3,4-b']-dipyridine
Part A: Preparation of 1,5-diazafluoren-9-one
11.8 g (0.178 mole) of potassium hydroxide was dissolved in 2000 ml of water in a 5-liter multi-neck round bottom flask. To this solution, 18.0 g (0.1 mole) of commercial 1,7-diazaphenanthroline was added. The mixture was heated to boiling, at which time the 1,7-diazaphenanthroline dissolved. To the boiling solution, a solution of 50.6 g (0.32 mole) of potassium permanganate in 800 ml of water was added dropwise with vigorous mechanical stirring at such a rate that the drops of permanganate were rapidly reduced. For this compound, the addition took one hour. The reaction mixture was refluxed 30 minutes longer, then the hot mixture was filtered. The filtrate was cooled to room temperature and extracted with chloroform. It was dried with sodium sulfate and the chloroform rotary evaporated. The crude product was recrystallized from water, then dried in a vacuum dessicator over potassium hydroxide. The yield of pure 1,5-diazafluoren-9-one was 3.3 g, m.p. 158°-159°. The above reaction was repeated and a further 3.3 g of material was obtained, which was combined with the first lot.
Part B: Reduction of 1,5-diazafluoren-9-one to 1,5-diazafluorene
Following the procedure described in Example 608, Part C, 6.0 g (33 mmole) of 1,5-diazafluoren-9-one and 11.8 g (0.37 mole) of hydrazine were combined with 100 ml of diethyleneglycol and heated rapidly to 200°. The reaction was kept at this temperature for 30 minutes, then for 3 hours at 180°. Following the described workup, the crude yield was 4.69 g, m.p. 85°. Recrystallization from cyclohexane yields 4.0 g, m.p. 99°-100° of pure 1,5-diazafluorene.
Part 3: Preparation of 9,9-Bis(4-pyridinylmethyl)-cyclopenta[1,2-b:3,4-b']dipyridine
Following the alkylation procedure described in Example 608, Part D, 2.0 g (12 mmole) of 1,5-diazafluorene, 4.68 g (29 mmole) of 4-picolylchloride, 1.44 g (30 mmole) of 50% sodium hydride were heated at 55 in 10 ml tetrahydrofuran and 25 ml benzene until TLC (ethyl acetate-methanol-90:10) showed appearance of product (Rf 0.065) and disappearance of starting diazafluorene (Rf 0.28). Crude product triturated with ether to yield 2.90 g, m.p. 133°-137°. This was flash chromatographed with ethyl acetate and recrystallized from benzene using charcoal to decolorize. Yield 2.4 g, m.p. 139.8°-140.9°. Rf 0.16 (ethyl acetate-methanol 90:10). NMR (200 MHz,CDCl 3 ) δ 3.397-3.718(dd,4H,(--CH 2 --pyridyl); 6.450-6.475(d,4H,β-pyridyls); 7.240-7.324(m, 2H,the 3- and 7- H's of the 1,5-diazafluorene, each meta to one of the nitrogens); 7.802-7.808 (d, 1H,8-H of diazafluorene); 7.879-7.885(d,1H,4---H of diazafluorene); 8.097-8.122 (d,4H, α-pyridyls); 8.451-8.476(d, 1H,2-H of diazafluorene); 8.741-8.763(d,1H,6-H of diazafluorene). ##STR1032## Difference=0.0003 for C 23 H 18 N 4 .
The compounds of Examples 440-464, 532, 560, 608, 611, 624 and other compounds which can be prepared by the methods described above, are illustrated in Table IX. The compounds of Examples 440-531 in Table IX have J, K, L and M as CH except where an R 1 , R 2 or R 5 substituent group was shown, in which case the substituent group replaces the H at that position.
TABLE IX__________________________________________________________________________ ##STR1033## mp °C.Ex. R.sub.1 R.sub.2 R.sub.5 B D A Het.sup.1 Het.sup.2 (salt__________________________________________________________________________ mp)440 H H H H H ##STR1034## ##STR1035## ##STR1036## 207-208441 H H H H H ##STR1037## ##STR1038## ##STR1039## (275-277)442 H H H H H O ##STR1040## ##STR1041## 212-213443 H H H H H bond ##STR1042## ##STR1043## (>300).sup.a444 2-NO.sub.2 H H H H bond ##STR1044## ##STR1045## 260-264.sup.b (>300)445 H H H H H S ##STR1046## ##STR1047## 201.4-203.4446 1-CH.sub.3 H H H H bond ##STR1048## ##STR1049## (>300).sup.c,d447 2-Br H H H H bond ##STR1050## ##STR1051## (>300).sup.e,f448 2-NH.sub.2 H H H H bond ##STR1052## ##STR1053## (>300).sup.g449##STR1054## H H H H bond ##STR1055## ##STR1056## (>300).sup.h450##STR1057## H H H H bond ##STR1058## ##STR1059## (>300).sup.i,j451 2-F H H H H bond ##STR1060## ##STR1061## (>300).sup.k,l452 2-CHF.sub. 2 H H H H bond ##STR1062## ##STR1063## (>300).sup.m,n453##STR1064## H H H H bond ##STR1065## ##STR1066## .sup.o,p454 2-CH.sub.3 H H H H bond ##STR1067## ##STR1068## .sup.q,r455 2-Et H H H H bond ##STR1069## ##STR1070## .sup.s,t456 2-OCH.sub.3 H H H H bond ##STR1071## ##STR1072## .sup.u457 H H H H H bond ##STR1073## ##STR1074## 137-138.sup.v,w458 1-CH.sub.3 H 4-CH.sub.3 H H ##STR1075## ##STR1076## ##STR1077## 211-213.sup.x459 4-Cl 5-Cl H H H ##STR1078## ##STR1079## ##STR1080## 170-172.sup.y,z460 1-Cl 8-Cl H H H ##STR1081## ##STR1082## ##STR1083## .sup.aa,bb461 H H H H H ##STR1084## ##STR1085## ##STR1086## .sup.cc,dd462 H H H H H ##STR1087## ##STR1088## ##STR1089## 196-197.sup.ee463 H H H H H ##STR1090## ##STR1091## ##STR1092## 226-227.sup.ff mp °C.464 H H H ##STR1093## bond ##STR1094## ##STR1095## 201-202.sup.gg mp °C.465 H H H H H ##STR1096## ##STR1097## ##STR1098##466 H H H H H ##STR1099## ##STR1100## ##STR1101##467 H H H H H ##STR1102## ##STR1103## ##STR1104##468 H H H H H ##STR1105## ##STR1106## ##STR1107##469 H H H H H ##STR1108## ##STR1109## ##STR1110##470 H H H H H ##STR1111## ##STR1112## ##STR1113##471 1-CH.sub.3 H H H H ##STR1114## ##STR1115## ##STR1116##472 H 2-Cl H H H ##STR1117## ##STR1118## ##STR1119##473 2-CH.sub.3 7-CH.sub.3 H H H ##STR1120## ##STR1121## ##STR1122##474 3-Et 6-Et H H H ##STR1123## ##STR1124## ##STR1125##475 4-OCH.sub.3 5-OCH.sub.3 H H H ##STR1126## ##STR1127## ##STR1128##476 4-CF.sub.3 H H H H ##STR1129## ##STR1130## ##STR1131##477 2-CN H H H H ##STR1132## ##STR1133## ##STR1134##478 H 4-NO.sub.2 H H H ##STR1135## ##STR1136## ##STR1137##479 2-NH.sub.2 H H H H ##STR1138## ##STR1139## ##STR1140##480##STR1141## H H H H ##STR1142## ##STR1143## ##STR1144##481##STR1145## H H H H ##STR1146## ##STR1147## ##STR1148##482 H H H H H ##STR1149## ##STR1150## ##STR1151##483 H H H H H ##STR1152## ##STR1153## ##STR1154##484 1-CH.sub.3 H H H H ##STR1155## ##STR1156## ##STR1157##485 2-Cl H H H H ##STR1158## ##STR1159## ##STR1160##486 2-CH.sub.3 7-CH.sub.3 H H H ##STR1161## ##STR1162## ##STR1163##487 3-NMe.sub.2 H H H H ##STR1164## ##STR1165## ##STR1166##488##STR1167## H H H H ##STR1168## ##STR1169## ##STR1170##489 4-Br 5-Br H H H ##STR1171## ##STR1172## ##STR1173##490 4-OCH.sub.3 H H H H ##STR1174## ##STR1175## ##STR1176##491 1-CF.sub.3 H H H H ##STR1177## ##STR1178## ##STR1179##492 1-CH.sub. 3 H H H H ##STR1180## ##STR1181## ##STR1182##493 2-Pr H H H H ##STR1183## ##STR1184## ##STR1185##494##STR1186## H H H H O ##STR1187## ##STR1188##495##STR1189## H H H H O ##STR1190## ##STR1191##496 2-CH.sub.3 H H H H O ##STR1192## ##STR1193##497 3-Br 7-Br H H H O ##STR1194## ##STR1195##498 4-OCH.sub.3 H H H H ##STR1196## ##STR1197## ##STR1198##499 2-CN H H H H ##STR1199## ##STR1200## ##STR1201##500 2-NO.sub.2 H H H H ##STR1202## ##STR1203## ##STR1204##501##STR1205## H H H H ##STR1206## ##STR1207## ##STR1208##502 1-CF.sub.3 H H H H ##STR1209## ##STR1210## ##STR1211##503 3-Pr 6-Pr H H H ##STR1212## ##STR1213## ##STR1214##504##STR1215## H H H H ##STR1216## ##STR1217## ##STR1218##505 3-CH.sub.3 H H H H CH.sub.2 ##STR1219## ##STR1220##506 2-Cl H H H H CH.sub.2 ##STR1221## ##STR1222##507 2-CH.sub.3 7-CH.sub.3 H H H CH.sub.2 ##STR1223## ##STR1224##508 3-Br 6-Br H H H CH.sub.2 ##STR1225## ##STR1226##509 4-OCH.sub.3 H H H H CH.sub.2 ##STR1227## ##STR1228##510 2-CF.sub.3 H H H H CH.sub.2 ##STR1229## ##STR1230##511##STR1231## H H H H CH.sub.2 ##STR1232## ##STR1233##512##STR1234## H H H H CH.sub.2 ##STR1235## ##STR1236##513 2-CN H H H H SO.sub.2 ##STR1237## ##STR1238##514 1-CH.sub.3 8-CH.sub.3 H H SO.sub.2 ##STR1239## ##STR1240##515##STR1241## H H H H SO.sub.2 ##STR1242## ##STR1243##516##STR1244## H H H H SO.sub.2 ##STR1245## ##STR1246##517 3-Br H H H H SO.sub.2 ##STR1247## ##STR1248##518 4-Pr H H H H SO.sub.2 ##STR1249## ##STR1250##519 3-CF.sub.2 CF.sub.3 H H H H ##STR1251## ##STR1252## ##STR1253##520 2-NH.sub.2 H H H H ##STR1254## ##STR1255## ##STR1256##521 1-NO.sub.2 H H H H ##STR1257## ##STR1258## ##STR1259##522 4-CN H H H H ##STR1260## ##STR1261## ##STR1262##523 2-CH.sub.3 7-CH.sub.3 H H H ##STR1263## ##STR1264## ##STR1265##524##STR1266## H H H H ##STR1267## ##STR1268## ##STR1269##525 2-CH.sub.3 H H H H ##STR1270## ##STR1271## ##STR1272##526 3-NMe.sub.2 H H H H ##STR1273## ##STR1274## ##STR1275##527 4-propyl H H H H ##STR1276## ##STR1277## ##STR1278##528##STR1279## H H H H ##STR1280## ##STR1281## ##STR1282##529 3-NO.sub.2 6-NO.sub.2 H H H ##STR1283## ##STR1284## ##STR1285##530 2-Et H H CHCH bond ##STR1286## ##STR1287## mp °C.531##STR1288## H H H H bond ##STR1289## ##STR1290##__________________________________________________________________________Ex. R.sub.1 R.sub.2 R.sub.5 J K L M B D A Het.sup.1 Het.sup.2 mp__________________________________________________________________________ °C.532 H H H C C C N -- -- bond ##STR1291## ##STR1292## .sup.hh533 H H H C C C C ##STR1293## bond ##STR1294## ##STR1295##534 H H H C C C C H H ##STR1296## ##STR1297## ##STR1298##535 H H H C C C C H H S ##STR1299## ##STR1300##536 2-CH.sub.3 H H C C C C H H ##STR1301## ##STR1302## ##STR1303##537 H H H C C C C H H ##STR1304## ##STR1305## ##STR1306##538 ##STR1307## H H C C C C H H ##STR1308## ##STR1309## ##STR1310##539 3-CH.sub.3 H H C C C C H H ##STR1311## ##STR1312## ##STR1313##540 H H H C C C C H H ##STR1314## ##STR1315## ##STR1316##541 H H H C C C C H H ##STR1317## ##STR1318## ##STR1319##542 H H H C C C C H H ##STR1320## ##STR1321## ##STR1322##543 H H H C C C C H H ##STR1323## ##STR1324## ##STR1325##544 H H H C C C C H H ##STR1326## ##STR1327## ##STR1328##545 H H H C C C C H H S ##STR1329## ##STR1330##546 2-NO.sub.2 H H C C C C H H S ##STR1331## ##STR1332##547 ##STR1333## H H C C C C H H S ##STR1334## ##STR1335##548 1-CH.sub.3 H 4-CH.sub.3 C C C C H H S ##STR1336## ##STR1337##549 4-Br H H C C C C H H ##STR1338## ##STR1339## ##STR1340##550 4-Br 5-Br H C C C C H H ##STR1341## ##STR1342## ##STR1343##551 2-Cl H H C C C C H H ##STR1344## ##STR1345## ##STR1346##552 H H H C C C C H H ##STR1347## ##STR1348## ##STR1349##553 H H H C C C C H H ##STR1350## ##STR1351## ##STR1352##554 2-CF.sub.3 H H C C C C H H ##STR1353## ##STR1354## ##STR1355##555 2-CN H H C C C C H H ##STR1356## ##STR1357## ##STR1358##556 3-NMe.sub.2 H H C C C C H H ##STR1359## ##STR1360## ##STR1361##557 H H H C C C C H H bond ##STR1362## ##STR1363##558 2-CH.sub.3 H H C C C C H H bond ##STR1364## ##STR1365##559 1-CH.sub.2 CH.sub.3 H H C C C C H H bond ##STR1366## ##STR1367##560 H H H N C C C H H bond ##STR1368## ##STR1369## 244-7561 H H H C N C C H H bond ##STR1370## ##STR1371##562 H H H C C N C H H bond ##STR1372## ##STR1373##563 ##STR1374## H H C C C N H H bond ##STR1375## ##STR1376##564 1-CH.sub.3 H H C C N C H H bond ##STR1377## ##STR1378##565 4-NHCOCH.sub.3 H H C N C C H H bond ##STR1379## ##STR1380##566 2-NHCOCH.sub.3 H H N C C C H H bond ##STR1381## ##STR1382##567 2-CH.sub.3 H H C C C C H H ##STR1383## ##STR1384## ##STR1385##568 2-Et H H C C C C H H ##STR1386## ##STR1387## ##STR1388##569 ##STR1389## H H C C C C H H ##STR1390## ##STR1391## ##STR1392##570 3-OCH.sub.3 6-OCH.sub.3 H C C C C H H ##STR1393## ##STR1394## ##STR1395##571 H H H C C C C H H CHCH ##STR1396## ##STR1397##572 1-CH.sub.3 H H C C C C H H CHCH ##STR1398## ##STR1399##573 2-Et H H C C C C H H CHCH ##STR1400## ##STR1401##574 ##STR1402## H H C C C C H H CHCH ##STR1403## ##STR1404##575 ##STR1405## H H C C C C H H (CH.sub.2).sub.2 ##STR1406## ##STR1407##576 4-NMe.sub.2 H H C C C C H H (CH.sub.2).sub.2 ##STR1408## ##STR1409##577 H H H C C C C H H (CH.sub.2).sub.2 ##STR1410## ##STR1411##578 H H H C C C C H H (CH.sub.2).sub.2 ##STR1412## ##STR1413##__________________________________________________________________________Ex. R.sub.1 R.sub.2 R.sub.5 J K L M B D A Het.sup.1 Het.sup.2 mp__________________________________________________________________________ °C.579 H H H C C C C H H ##STR1414## ##STR1415## ##STR1416##580 H H H C C C C H H ##STR1417## ##STR1418## ##STR1419##581 H H H C C C C H H ##STR1420## ##STR1421## ##STR1422##582 H H H C C C C H H ##STR1423## ##STR1424## ##STR1425##583 H H H C C C C H H ##STR1426## ##STR1427## ##STR1428##584 H H H C C C C H H ##STR1429## ##STR1430## ##STR1431##585 2-CH.sub.3 H 3-CH.sub.3 C C C C H H ##STR1432## ##STR1433## ##STR1434##586 2-CH.sub.3 6-CH.sub.3 3-CH.sub.3 C C C C H H ##STR1435## ##STR1436## ##STR1437##587 2-OCH.sub.3 7-OCH.sub.3 H C C C C H H ##STR1438## ##STR1439## ##STR1440##588 2-OCH.sub.3 H 3-OCH.sub.3 C C C C H H ##STR1441## ##STR1442## ##STR1443##589 3-Et 6-Et H C C C C H H ##STR1444## ##STR1445## ##STR1446##590 3-Br 6-Br H C C C C H H ##STR1447## ##STR1448## ##STR1449##591 3-OEt 6-OEt H C C C C H H ##STR1450## ##STR1451## ##STR1452##__________________________________________________________________________Ex. R.sub.1 R.sub.2 R.sub.5 J K L M B D A Het.sup.1 Het.sup.2 mp__________________________________________________________________________ °C.592 H H H C C C C H H (CH.sub.2).sub.3 ##STR1453## ##STR1454##593 H H H C C C C H H (CH.sub.2).sub.3 ##STR1455## ##STR1456##594 H H H C C C C H H (CH.sub.2).sub.3 ##STR1457## ##STR1458##595 H H H C C C C H H (CH.sub.2).sub.3 ##STR1459## ##STR1460##596 H H H C C C C H H (CH.sub.2).sub.3 ##STR1461## ##STR1462##597 H H H C C C C H H (CH.sub.2).sub.3 ##STR1463## ##STR1464##598 H H H C C C C H H (CH.sub.2).sub. 3 ##STR1465## ##STR1466##599 2-OH H H C C C C H H bond ##STR1467## ##STR1468##600##STR1469## H H C C C C H H bond ##STR1470## ##STR1471##601##STR1472## H H C C C C H H bond ##STR1473## ##STR1474##602 4-OCH.sub.2 CH.sub.2 CH.sub.3 H H C C C C H H bond ##STR1475## ##STR1476##603 2-CH.sub.2 CF.sub.3 H H C C C C H H bond ##STR1477## ##STR1478##604 3-CF.sub.2 CF.sub.3 H H C C C C H H bond ##STR1479## ##STR1480##605 4-CF.sub.2 CF.sub.2 CF.sub.3 H H C C C C H H bond ##STR1481## ##STR1482##606 1-CF.sub.3 8-CF.sub.3 H C C C C H H bond ##STR1483## ##STR1484##607 2-CH.sub.3 7-CH.sub.3 H C C C C CHCH bond ##STR1485## ##STR1486##__________________________________________________________________________Ex. R.sub.1 R.sub.2 R.sub.5 J.sub.1 K.sub.2 L.sub.3 M.sub.4 J.sub.8 K.sub.7 L.sub.6 M.sub.5 B D A Het.sup.1 Het.sup.2 mp__________________________________________________________________________ °C.608 H H H N C C C C C C C H H bond ##STR1487## ##STR1488## 204.7-206609 H H H C N C C C C C C H H bond ##STR1489## ##STR1490##610 H H H C C N C C C C C H H bond ##STR1491## ##STR1492##611 H H H C C C N C C C C -- H bond ##STR1493## ##STR1494## 163-164612 2-CH.sub.3 H H C C C C N C C C H H bond ##STR1495## ##STR1496##613 4-NH.sub.2 H H C C C C C N C C H H bond ##STR1497## ##STR1498##614 2-NH.sub.2 H H C C C C C C N C H H bond ##STR1499## ##STR1500##615 4-CH.sub.3 H H C C C C C C C N -- H bond ##STR1501## ##STR1502##616 H 2,3-benzo N C C C C C C C H H bond ##STR1503## ##STR1504##617 H 3,4-benzo C N C C C C C C H H bond ##STR1505## ##STR1506##618 H 2,3-benzo C C C C C C N C H H bond ##STR1507## ##STR1508##619 H 3,4-benzo C C C C C C C N -- H bond ##STR1509## ##STR1510##620 H 2,3-benzo C C C C C C C C H H bond ##STR1511## ##STR1512##621 H 3,4-benzo C C C C C C C C H H bond ##STR1513## ##STR1514##622 H H H N C C C C N C C H H bond ##STR1515## ##STR1516##623 H H H N C C C C C N C H H bond ##STR1517## ##STR1518##624 H H H N C C C C C C N H -- bond ##STR1519## ##STR1520## 139.8-140.625 H H H C C N C N C C C H H bond ##STR1521## ##STR1522##626 H H H C C N C C N C C H H bond ##STR1523## ##STR1524##627 H H H C C N C C C C N H -- bond ##STR1525## ##STR1526##628 H H H C N C C N C C C H H bond ##STR1527## ##STR1528##629 H H H C N C C C C N C H H bond ##STR1529## ##STR1530##630 H H H C N C C C C C N H -- bond ##STR1531## ##STR1532##631 H H H C C C N N N C C -- H bond ##STR1533## ##STR1534##632 H H H C C C N C N C C -- H bond ##STR1535## ##STR1536##633 H H H C C C N C C N C -- H bond ##STR1537## ##STR1538##__________________________________________________________________________ FOOTNOTES TO TABLE IX .sup.a HRMS, M.sup.+ =0 348.1615 .sup.b HRMS, M.sup.+ = 393.1465 .sup.c HRMS, M.sup.+ = 362.1779 .sup.d NMR (200 MHz, CDCl.sub.3) 2.82(s,3H), 3.60(dd, 4H), 6.39(m, 4H), 7.0-7.5(m, 4H), 7.0-7.5(m, 7Harom), 8.0(m, 4H) .sup.e HRMS, M.sup.+ = 426.0758 .sup.f NMR (200 MHz, CDCl.sub.3) 3.39(dd, 4H(), 6.48(d, 4H), 7.10-7.67(m, 7Harom), 8.12(d, J=5.7 Hz, 4H) .sup.g HRMS, M.sup.+ = 363.1728 .sup.h NMR (CDCl.sub.3) 2.19(s, 3H), 3.40(s, 4H), 6.50(d, J=5.7 Hz, 4H), 6.92(m, 1H), 7.14-7.33(m, 4H), 7.52(d, 1H), 8.04(d, J=5.8 Hz, 4H), 8.25(s 1H), 8.5(s, 1H, exchangeable with D.sub.2 O). .sup.i HRMS, M.sup.+ = 390.1720 .sup.j NMR 2.68(s, 3H), 3.46(s, 4H), 6.44(d, J=5.9 Hz, 4H), 7.29-7.87(m, 6H), 8.05(d, J=5.9 Hz, 4H), 8.2(d, 1H) .sup.k HRMS, M.sup.+ = 366.1566 .sup.l NMR 3.38(dd, 4H), 6.49(d, J=6.0 Hz, 4H), 6.9(m, 1H), 7.14-7.36(m, arom), 7.5(d, 1H), 8.1(d, J=6.0 Hz, 4H) .sup.m HRMS, M.sup.+ = 398.1583 .sup.n NMR 3.43(s, 4H), 6.45(d, J=5.7 Hz, 4H), 6.74(t, J=5.6 Hz, 1H), 7.26-7.70(m, arom), d, J=5.7 Hz, 4H) .sup.o HRMS, M.sup.+- .sup.p NMR 1.50(d, J=6.5 Hz, 3H), 3.39(s, 4H), 4.92(q, J=6.4 Hz, 1H), 7.08-7.58(n arom), 7.87(d, 2H), 7.97(d, 2H) .sup.q HRMS, M.sup.+ = 362.1779 .sup.r NMR 2.47(s, 3H), 3.37(s, 4H), 6.49(d, J=5.3 Hz, 4H), 7.03-7.45(m, arom), 8.09(d, 4H) .sup.s HRMS, M.sup.+ = 376.1927 .sup.t NMR 1.30(t, J=7.8 Hz, 3H), 2.74(q, J=7.6 Hz, 2H), 3.37(s, 4H), 6.49(d, J=5.9 Hz, 4H), 7.04-7.48(m, 7Harom), 8.09(d, J=5.4 HZ, 4H) .sup.u NMR 3.37(s, 4H), 3.89(s, 3H), 6.52(broad, 4H) 6.80(m, 1H), 7.01(m, 1H), 7.01(d, J=2.1 Hz, 1H), 7.26(m, 5H), 7.45(d, J=7.5 Hz, 1H), 8.11(broad, 4H) .sup.v HRMS, M.sup.+ = 348.1626 .sup.w NMR 3.41(s, 4H), 6.71-6.97(m, 4H), 7.17-7.35(tt, 6H), 7.50-7.54(d, J=6.9 Hz, 2H), 7.91(s, 2H), 8.12-8.15(d, J=5.4 Hz, 2H) .sup.x .sup.y HRMS, M.sup.+ = 440.0799 .sup.z NMR 3.53(s, 4H), 6.43(d, J=6.1 Hz, 4H), 7.33-7.51(m, 6Harom), 8.3(d, J=6.2 Hz, 4H) .sup.aa HRMS, M.sup.+ was 440.0806 .sup.bb NMR 4.66(s, 4H), 6.33(d, J=6.1 Hz, 4H), 7.45(t, J=6.6 Hz, 2Harom) 779(d, J=7.1 Hz, 2Harom), 8.01(d, J=6.3, 4H), 8.13(d, J=7.1 Hz, 2H) .sup.cc HRMS, M.sup.+ 376.1573 .sup.dd NMR 3.77(s, 4H), 6.49(d, J=6.9 Hz, 2Harom), 6.66(dd, J=7.91, J=4.8, 2Harom), 7.48(t, J=7.4 Hz, 2Harom), 7.56(m, 1H), 7.79(t, J=7.3 Hz, 2H), 8.03(d, J=7.0 Hz, 2H), 8.16(m, J=1.8 Hz, 4H) .sup.ee HRMS, M.sup.+ 378.1691 .sup.ff HRMS, M.sup.+ 391.1634 .sup.gg HRMS, M.sup.+ 377.1060 .sup.hh HRMS, M.sup.+ 350.0971
Biochemical Test Procedure
The effect of compounds on the release of acetylcholine (ACh) from rat cerebral cortex slices was tested essentially using a slice superfusion procedure described by Mulder et al, Brain Rest, 70, 372, (1974), as modified according to Nickolson et al, Naunyn Schmied. Arch. Pharmacol., 319, 48 (1982).
Male Wistar rats (Charles River) weighing 175-200 grams were used. They were housed for at least seven days before the experiment in the animal facility under a 12-12 hour light/dark cycle (light on 6.00h, light off 18.00h). They had ad lib access to standard rat chow (Purina) and deionized water.
Rats were decapitated and brains were dissected innately. Slices (0.3 mm thick) from the parietal cortex were prepared manually using a recessed Lucite® guide and subsequently cut into 0.25×0.25 nrn squares.
Slices (approximately 100 mg wet weight) were incubated in 10 ml Krebs-Ringer (KR) medium containing (mM): NaCl (116), KC1 (3), CaCl 2 (1.3), MgCl 2 (1.2), KH 2 PO 4 (1.2), Na 2 SO 4 (1.2), NaHCO 3 (25), glucose (11), to which 10 μCi 3 H-Choline (spec. act. approx. 35 Ci/mmol; NEN) and 10 nmoles unlabelled choline had been added to give a final concentration of 10 -6 M. Incubation was carried out for 30 minutes at 37° C. under a steady flow of 95% O 2 /5% CO 2 . Under these conditions, part of the radioactive choline taken up was converted into radioactive ACh by cholinergic nerve endings, stored in synaptic vesicles and released upon depolarization by high-K + -containing media.
After labelling of the ACh stores, the slices were washed 3 times with non-radioactive KR-medium and transferred to a superfusion apparatus to measure the drug effects on ACh release. The superfusion apparatus consisted of 10 thermostated glass coltrams of 5 mm diameter which were provided with GF/F glass fiber filters to support the slices (approximately 10 mg tissue/column). Superfusion was carried out with KR-medium (0. S ml/min ) containing 10 -5 M hemicholinium-3 (HC-S). HC-3 prevents the uptake of choline, formed during the superfusion from phospholipids and released ACh, which would be converted into unlabelled ACh, and released in preference to the pre-formed, labelled ACh. The medium was delivered by a 25-channel peristaltic pump (Ismatec; Brinkman) and was warmed to 37° C. in a thermostated stainless steel coil before entering the superfusion column. Each column was provided with a 4-way slider valve (Beckman Instruments) which allowed rapid change of low-to high-K + -KR-medium and with two 10-channel, 3-way valves which were used to change from drug-free to drug-containing low-and high-K + -KR-medium.
After 15 minutes washout of non-specifically bound radioactivity, the collection of 4 minute fractions was started. After 3 four-min. collections, the KR medium was changed for KR medium of which the KC1 concentration had been increased to 25 mM (high-K + -KR-medium) (Sl ). Depolarization-induced stimulation of release by high-K+-KR-medium lasted for 4 minutes. Drug free low-and high-K + -KR-medium were then substituted by drug- or vehicle-containing low- and high-K + -KR-medium and superfusion was continued for 3 four-min. collections with low-K + -KR-medium, 1 four-min. collection with high-K+-medium (S2) and 2 four-min. collections with low-K + -KR-medium.
Drug was added to the media by 100-fold dilution of appropriate concentrations of the drug (in 0.9% NaC1/H 20 ) with either low- or high-K + -KR-medium.
All superfusion fractions were collected in liquid scintillation counting vials. After superfusion the slices were removed from the superfusion columns and extracted in 1.0 ml of 0.1 N HCl. To superfusion fractions and extracts 12 ml Liquiscint counting fluid (NEN) was then added and samples were counted in a Packard Tricarb Liquid Scintillation Counter. No corrections were made for quenching.
The ratio of S2/S1 (as conpared to controls where no drug was present during S2) was a measure of the ability of the drug to enhance or depress stimulus-induced acetylcholine release. The in vitro ACh release data was summarized in Table X.
TABIE X______________________________________% INCREASE OF STIMULUS-INDUCED AChRELEASE IN RAT CEREBRAL CORTEX IN VITROExample 10.sup.-6 10.sup.-5 10.sup.-4 (M)______________________________________ 1 -- -- +349* 2 +11 +61* +265* 3 +06 +88* +238* 4 +94* +457* +433* 5 +14 +78* +355* 6 +195* +313* -- 7 -- 0 +30* 8 -- +37* +429* 9 0 +54* +275* 12 -- +11 +48* 13 0 +13 +100* 16 +01 +47* -- 19 +34* +323* -- 43 +34* +210* -- 45 -- +12 +97* 46 +20 +218* -- 49 +16* +49* -- 61 +13 +87 62 +3 +111 -- 63 +105 +338 -- 64 +4 +55 -- 65 +3 +94 --124 +0 +148 --125 +17 +50 --182 +19 +302 --183 -- +471 +607240 +0 +0 --288 +37 +215 --324 +35 +217 --387 -- +14 --440 +695 +501 --441 +695 +501 --442 +222 +340 --443 +345 +221 --444 +228 +467 --445 +71 +233 --446 +470 +465 --447 +288 +259 --448 +513 +429 --449 +387 -- --450 +359 +308 --451 +351 -- --452 +439 -- --453 +45 +261 --454 +264 +375 --455 +167 +460 --456 +125 +429 --457 +0 +69 --458 +410 -- --459 +207 +335 --460 +35 +138 --461 +145 +303 --462 +310 -- --463 +254 +299 --464 +76 +238 --532 +57 +359 --611 +222 +227 --608 +22 +185 --624 +0 +90 --______________________________________ *Significantly different from control P < 0.05, student's ttest.
Using similar test procedures, the compounds of Examples 2 and 4 were also found to enhance the release of acetylcholine from hippocampal slices and that of acetylcholine and dopamine from caudate nucleus slices in vitro. The compound of Example 4, in addition, was found to also enhance the release of serotonin from cortical slices.
Behavioral Test Procedure
The effect of compounds on rat active avoidance (pole-climb) performance was studied as follows: Male Sprague-Dawley rates (Charles River), weighing 150-200 grams, received two blocks of five learning trials daily (1 AM, 1 PM), for four days. A trial consisted of placing a rat in a cage (Coulbourn Model E10-10, equipped with a removable shock gridfloor), facing a pole (wood, with parallel diagonal notches, mounted from the ceiling). The trial was started by closing the cage door and switching on the cage light. After 10 seconds, shock was applied through the gridfloor for 10 seconds by a Coulbourn Model E13-08 shocker. Footshock intensity ranged from 0.6 to 1.2 mA. At the end of the trial, the light and shock were turned off and the rat was removed from the cage. If the rat jumped on the pole prior to the onset of shock, it was considered to have avoided; if it jumped after the shock, it was considered to have escaped. Groups of 6 to 9 rats were subcutaneously treated with various doses of a compound or the corresponding vehicle 30 minutes prior to the first training trial of each block.
Active avoidance performance data were analyzed by regression analysis (see Snedecor and Cochran, Statistical Methods, 6th Edition, page 432) of the cumulative number of avoidances versus blocks of trials curve. The mean slope and SEM (Standard Error of the Mean) of this curve were calculated for each treatment group and taken as a measure of active avoidance performance. Drug effects were expressed as percent change in slope ccrpared to the slope of the control curve. The results are summarized in Table XI.
TABIE XI______________________________________% ENHANCEMENT OF ACTIVE AVOIDANCEPERFORMANCE IN RATSDrug Dose (mg/kg s.c.)Example 0.1 0.3 1 3 5 10 20______________________________________2 -- -- -- 54* 53* 214 +59* +91* +84* +57 -- -- --______________________________________ *Significantly different from control, P < 0.05, student's ttest.
Utility
The foregoing test results suggest that canpounds of this invention have utility in the treatment of cognitive deficiencies and/or neurological function deficits and/or mood and mental disturbances, in patients suffering fran nervous system disorders like Alzheimer's disease, Parkinson's disease, senile-dementia, multi-infarct dementia, Huntington's disease, mental retardation, Myasthenia Gravis etc. Compounds of this invention can be administered to treat said deficiencies by any means that produces contact of the active agent with the agent's site of action in the body of a mammal. The compounds can be administered by any conventional means available for use in conjunction with pharmaceuticals, either as individual therapeutic agents or in a combination of therapeutic agents. They can be administered alone, but are generally administered with a pharmaceutical carrier selected on the basis of the chosen route of administration and standard pharmaceutical practice.
The dosage administered will, of course, vary depending on the use and known factors such as the pharmacodynamic characteristics of the particular agent, and its mode and route of administration; age, health, and weight of the recipient; nature and extent of symptoms, kind of concurrent treatment, frequency of treatment, and the effect desired. For use in the treatment of said diseases, a daily oral dosage of active ingredient can be about 0.001 to 100 mg/kg of body weight. Ordinarily a dose of 0.01 to 10 mg/kg per day in divided doses one to four times a day or in sustained release form is effective to obtain the desired results.
Dosage forms (compositions) suitable for administration contain from about 1 milligram to about 100 milligrams of active ingredient per unit. In these pharmaceutical compositions the active ingredient will ordinarily be present in an amount of about 0.5-95% by weight based on the total weight of the compsition.
The active ingredient can be administered orally in solid dosage forms, such as capsules, tablets, and powders, or in liquid dosage forms, such as elixirs, syrups, and suspensions. It can also be administered parenterally, in sterile liquid dosage forms.
Gelatin capsules contain the active ingredient and powdered carriers, such as lactose, starch, cellulose derivatives, magnesium stearate, stearic acid, and the like. Similar diluents can be used to make compressed tablets. Both tablets and capsules can be manufactured as sustained release products to provide for continuous release of medication over a period of hours. Compressed tablets can be sugar coated or film coated to mask any unpleasant taste and protect the tablet from the atmosphere, or enteric coated for selective disintegration in the gastrointestinal tract.
Liquid dosage forms for oral administration can contain coloring and flavoring to increase patient acceptance.
In general, water, a suitable oil, saline, aqueous dextrose (glucose), and related sugar solutions and glycols such as propylene glycol or polyethylene glycols are suitable carriers for parenteral solutions. Solutions for parenteral administration preferably contain a water soluble salt of the active ingredient, suitable stabilizing agents, and if necessary, buffer substances. Antioxidizing agents such as sodium bisulfite, sodium sulfite, or ascorbic acid, either alone or combined, are suitable stabilizing agents. Also used are citric acid and its salts and sodium EDTA. In addition, parenteral solutions can contain preservatives, such as benzalkonium chloride, methyl- or propyl-paraben, and chlorobutanol.
Suitable pharmaceutical carriers are described in Remington's Pharmaceutical Sciences, A. Osol, a standard reference text in this field.
Useful pharmaceutical dosage-forms for adminstration of the compounds of this invention can be illustrated as follows:
Capsules
A large number of unit capsules are prepared by filling standard two-piece hard gelatin capsules each with 100 milligrams of powdered active ingredient, 150 milligrams of lactose, 50 milligrams of cellulose, and 6 milligrams magnesium stearate.
Soft Gelatin Capsules
A mixture of active ingredient in a digestable oil such as soybean oil, cottonseed oil or olive oil was prepared and injected by means of a positive displacement pumpinto gelatin to form soft gelatin capsules containing 100 milligrams of the active ingredient. The capsules are washed and dried.
Tablets
A large number of tablets are prepared by conventional procedures so that the dosage unit was 100 milligrams of active ingredient, 0.2 milligrams of colloidal silicon dioxide, 5 milligrams of magnesium stearate, 275 milligrams of microcrystalline cellulose, 11 milligrams of starch and 98.8 milligrams of lactose. Appropriate coatings may be applied to increase palatability or delay absorption.
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Cognitive defeciencies or neurological dysfunction in mammals are treated with α,α-disubstituted aromatic or heteroaromatic compounds. The compounds have the formula: ##STR1## or a salt thereof wherein X and Y are taken together to form a saturated or unsaturated carbocyclic or heterocyclic first ring and the shown carbon in said ring is α to at least one additional aromatic ring or heteroaromatic ring fused to the first ring;
one of Het 1 or Het 2 is 2, 3, or 4-pyridyl or 2, 4, or 5-pyrimidinyl and the other is selected from
(a) 2, 3, or 4-pyridyl,
(b) 2, 4, or 5-pyrimidinyl,
(c) 2-pyrazinyl,
(d) 3, or 4-pyridazinyl,
(e) 3, or 4-pyrazolyl,
(f) 2, or 3-tetrahydrofuranyl, and
(g) 3-thienyl.
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FIELD OF THE INVENTION
[0001] The present invention relates generally to a fuel tester. More particularly, the present invention relates to a portable diesel fuel tester.
BACKGROUND OF THE INVENTION
[0002] Ultra-low sulfur diesel (ULSD) is a new standard that has been proposed by the EPA that effects diesel fuel sold for use on-road. This new regulation pertains to diesel fuel, additives and distillate fuels such as kerosene. The previous low diesel sulfur content was 500 p.p.m. (parts per million). The USLD contains only 15 p.p.m., which is about a 97 percent reduction from the 500 p.p.m. level.
[0003] The EPA requires that by Dec. 1, 2010, all highway diesel fuel sold will be ULSD. The use of ULSD will decrease emissions of sulfur compounds, which has been linked to acid rain. The decrease in sulfur content (15 p.p.m.) will reduce the replacement of particulate filters, which are being plugged up at the higher sulfur content of 500 p.p.m. The EPA hopes that the new standard will reduce the nitrogen oxide emissions by 2.6 million tons and particulate matter by 110,000 tons per year. Additionally, ULSD is required to be used in the new diesel engines or the warranty of the engines will be voided.
[0004] There are currently bench size testers that are implemented with a computer that are expensive to purchase and use. The bench size testers are not mobile and thus field inspections cannot be readily be done either at the refineries or the fueling stations. Additionally, the bench size testers require that the samples be sent to its location for analysis and that increases the time in which the results can be made available. The inspections include determining whether there has been sulfur contamination in the fuel refining system or if the fuel is over the legal limit. When sulfur reacts with oxygen it forms SO 2 , which can be used to test the amount of sulfur in the fuel.
[0005] Accordingly, there is a need for an apparatus and method to test diesel fuel in the field that is cost effective and the results can be determined in the field.
SUMMARY OF THE INVENTION
[0006] The foregoing needs are met, to a great extent, by the present invention, wherein in one aspect an apparatus is provided that in some embodiments provides a vehicle diagnostic device that includes a programmable function key in order to control a function on an emission computer workstation.
[0007] In accordance with one embodiment of the present invention, a portable diesel fuel tester is provided, which can include a LCD display that displays testing information, a testing chamber for testing the diesel fuel having a door, the door having vent holes that can vent a gas from the testing chamber, a sample tray located in the testing chamber that can receive a sample of diesel fuel to be tested, the sample tray having a heating element that can heat the diesel fuel to the gas state, a SO 2 sensor that senses SO 2 gas generated by the heating of the diesel fuel, an air pump that can circulate the gas of the heated diesel fuel from the sample tray to the SO 2 sensor, a power source for powering the fuel tester, a processor having a software that can operate the tester, wherein the processor can be in communication with the LCD display, the SO 2 sensor, the heating element, the power source and the air pump, and a housing that can house the LCD display, the testing chamber, the sample tray, the SO 2 sensor, the processor, the power source, and the air pump, wherein the housing is configured so that the tester is portable.
[0008] In accordance with another embodiment of the present invention, a method of testing a sample of diesel fuel is provided and can include depositing a sample of diesel fuel on a sample tray of a portable diesel fuel tester, heating the sample of diesel fuel with a heating element to a gas state that is detectable by a SO 2 sensor, circulating the gas from the sample tray to the SO 2 sensor with an air pump, detecting the gas containing SO 2 with the SO 2 sensor, determining the amount of sulfur in the sample of diesel fuel from the SO 2 gas, and displaying the amount of sulfur in the sample of diesel fuel on a LCD display.
[0009] In accordance with yet another embodiment of the present invention, a portable diesel fuel tester is provided, which can include a means for displaying testing information, a means for containing testing conditions for a sample of diesel fuel having a door, the door having vent holes that can vent a gas from the means for containing testing conditions, a means for receiving the sample of diesel fuel to be tested, the means for receiving having a means for heating the diesel fuel to the gas state, a means for sensing SO 2 gas generated by the heating of the diesel fuel, a means for circulating the gas of the heated diesel fuel from the means for receiving to the means for sensing, a means for powering the portable diesel fuel tester, a means for processing having a software that operates the tester, wherein the means for processing is in communication with the means for displaying, the means for sensing, the means for heating, means for the powering and the means for circulating, and a means for housing that houses the means for displaying, the means for containing, the means for receiving, the means for sensing, the means for processing, the means for powering, and the means for circulating, wherein the means for housing is configured so that the tester is portable.
[0010] There has thus been outlined, rather broadly, certain embodiments of the invention in order that the detailed description thereof herein may be better understood, and in order that the present contribution to the art may be better appreciated. There are, of course, additional embodiments of the invention that will be described below and which will form the subject matter of the claims appended hereto.
[0011] In this respect, before explaining at least one embodiment of the invention in detail, it is to be understood that the invention is not limited in its application to the details of construction and to the arrangements of the components set forth in the following description or illustrated in the drawings. The invention is capable of embodiments in addition to those described and of being practiced and carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein, as well as the abstract, are for the purpose of description and should not be regarded as limiting.
[0012] As such, those skilled in the art will appreciate that the conception upon which this disclosure is based may readily be utilized as a basis for the designing of other structures, methods and systems for carrying out the several purposes of the present invention. It is important, therefore, that the claims be regarded as including such equivalent constructions insofar as they do not depart from the spirit and scope of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 illustrates a diesel fuel tester according to an embodiment of the invention.
[0014] FIG. 2 is a block diagram of the components of the tester.
[0015] FIG. 3 illustrates the steps of the operation of the tester of the present invention.
DETAILED DESCRIPTION
[0016] The invention will now be described with reference to the drawing figures, in which like reference numerals refer to like parts throughout. An embodiment in accordance with the present invention provides a portable diesel fuel tester that can test the sulfur content in the field and display the results to a user.
[0017] FIG. 1 illustrates a diesel fuel tester 100 according to an embodiment of the invention. The tester is configured and designed to be portable. The tester 100 includes a housing 110 to house the components of the tester including a testing portion 128 , a storage compartment 124 , and power switch 132 and a power source 136 , such as a battery (not shown). The tester further includes an LCD screen 112 mounted on an external surface of the housing for viewing by the user. The LCD displays information including the amount of sulfur in the tested diesel fuel. The LCD can also display instructions on the screen for the user to run the test or display any other information desired. The power source can be an internal or external battery or by plugging into a DC or AC source.
[0018] Within the housing 110 is a circulating air pump 114 to circulate the air in the testing portion 128 of the tester 100 . A SO 2 sensor 116 , such as sensors available from Alphasense, Ltd in the United Kingdom can be used to measure the amount of sulfur in the tested diesel fuel. A door 120 , made from Plexiglas, for example, is used to introduce the diesel fuel into a testing chamber 130 . The door 120 can include vent holes 118 therein for the vapor (from the vaporized diesel fuel) to escape the testing chamber 130 to reach the SO 2 sensor. A sample tray 112 that includes a resistive heating element is located at the bottom of the testing chamber 130 .
[0019] The testing portion 128 is used to test a sample of the diesel fuel. Only a small sample, such as 2-10 drops of the diesel fuel is needed. The sample can be collected from any sized liquid dropper. The SO 2 sensor can be any sensor that can measure the vapor or gas of the tested diesel fuel to determine if it is within the 15 p.p.m. required by the EPA. The sensitivity of the sensor can be from about 5 p.p.m. to about 50 p.p.m. or any other sensitivity level can be used by the user so long it is within the desired testing range.
[0020] The door 120 is used to contain the vapor gas until it escapes from the vent holes 118 . The door 120 can include a handle (not shown) and hinges (not shown) for easy opening and closing. The door 120 can be made from any material including polymers, metals or alloys so long as they do not react with the SO 2 or the diesel fuel being tested. Although shown as triangular in shape, the vent holes 118 can be any shape including circular, rectangular, oval, elliptical, and a combination thereof. The size of the vent holes can be any size so long as they allow a detectable amount of vapor to reach the sensor. The holes can range, for example, from 1 mm to 50 mm. However, other larger or smaller sizes are also contemplated by the invention.
[0021] The sample tray 112 can be made from any material so long as it can be heated to a temperature that exceeds the flash point/boiling point of any diesel fuel that is tested. The heating time can range, for example, from about 2 seconds to about 45 seconds. The heating time can be lower or higher then the aforementioned times due to various types of diesel fuel that can be tested.
[0022] The diesel fuel needs to be vaporized so that it mixes with the 02 in the surrounding atmosphere to form SO 2 that the sensor can detect and quantify. The sample tray 122 includes a heating element such as a resistive heating element made from Nichrome. The heating element is used to heat the diesel fuel in the sample tray to the boiling point. The heating element can be integral or separated from the heating tray.
[0023] An air pump is used to circulate the air in the testing chamber 130 so that the SO 2 sample can reach the SO 2 sensor for an accurate reading. The air pump can be any capacity pump so long as it can adequately circulate the air within the testing portion of the tester.
[0024] Within the housing a storage compartment 124 is provided and contains a cleaning tray. The cleaning tray includes alcohol wipes and cleaning cloth. Other wipes and cleaning supplies are within the spirit of the invention. The wipes are used to clean the sample tray and the cleaning cloth is used to dry and remove any remaining residue on the sample tray. The wipes and the cleaning cloth should be the kinds that do not leave any residue, felt or otherwise contaminate the sample tray.
[0025] FIG. 2 is block diagram of the components of the tester 100 . A processor 202 or CPU (central processing unit) is provided to operate the tester 100 . In alternative embodiments, the processor can be an FPGA (Field Programmable Gate Array) or other controllers known in the art. The processor 202 communicates with the power switch 132 , the power source 136 , the sensor 116 , the LCD 112 , and the pump 114 . The processor includes volatile memory (RAM) and non-volatile memory 206 to store programming that operates the tester 100 . The CPU can have an external clock 208 or an internal clock. As stated above, the processor can allow communication between the components in order for the tests to be conducted by the tester and the results displayed on the LCD.
[0026] FIG. 3 illustrates the steps of the operation of the tester of the present invention. At step 302 , a sample of the diesel fuel to be tested is obtained. The sample can be obtained in a dropper known in art. At step 304 , the door is opened and the sample is deposited on the sample tray. The sample can be a few drops in amount from the dropper. The door is closed so the test can be conducted. At step 306 , the tester is turned on via the power switch 132 , which activates the heating element and the air pump. The LCD can also display “Place Sample” and “Press Start” in order to instruct the user. At step 308 , the sample is heated for about 30 seconds or so to its vaporized form. The heating time can be more or less than 30 seconds depending on the type of diesel fuel being tested. The LCD can display “Test In Progress,” to let the user know that the test has begun. The pump helps to circulate the air and helps the vapor to exit the testing chamber through the vent holes in the door.
[0027] At step 310 , the sensor takes a reading of the sample. As the vapor passes the sensor, the sensor senses the amount of SO 2 present. At step 312 , the sensor outputs the reading to the LCD. The LCD can display on one line, the sample letter, for example, “Diesel Sample A,” and on a second line, the sulfur content, for example, “23 p.p.m. sulfur content.” If a reading can not determined accurately, high or low sulfur content can be shown on the display or on another indicator such as an LED (not shown, red for high sulfur and green for low sulfur). The high or low indicator can be based on a 30 p.p.m. cutoff range, wherein below 30 p.p.m., the tester will indicate low sulfur and above 30 p.p.m. the tester will indicate high sulfur. In the mean time, the pump still circulates the air for an additional 30 seconds or so after the diesel fuel vaporized to evacuate any remaining vapors from the testing chamber.
[0028] In other embodiments, additional steps include step 314 , where the user power downs the tester 100 via the power switch 132 . At step 316 , the user can clean the testing chamber and the sample tray with the wipe and cloth stored in the cleaning tray. After cleaning, the tester is ready to run the next sample.
[0029] The tester 100 is designed to be portable so that it can be used in the field. A relatively small sample is needed and the results can be determined in the field.
[0030] The many features and advantages of the invention are apparent from the detailed specification, and thus, it is intended by the appended claims to cover all such features and advantages of the invention which fall within the true spirit and scope of the invention. Further, since numerous modifications and variations will readily occur to those skilled in the art, it is not desired to limit the invention to the exact construction and operation illustrated and described, and accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope of the invention.
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A portable diesel fuel tester and a method of its use are provided. A sample of diesel fuel is placed in a sample tray of the tester. The diesel fuel is heated to a gas state and circulated to a SO 2 sensor by an air pump. The SO 2 sensor determines the level of sulfur in the diesel fuel based on the SO 2 levels. The sulfur level is displayed on an LCD screen for viewing by the user.
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This application is a Divisional application of application Ser. No. 457,841, filed Dec. 27, 1989, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to novel optically active compounds and liquid crystal compositions comprising said compounds. The present invention provides, in particular, ferroelectric liquid crystal materials, for example, optically active compounds and liquid crystal compositions comprising said compounds both useful as electrooptic switching elements (e.g. liquid crystal display devices) in liquid crystal optical modulators, as well as liquid crystal optical modulators using liquid crystal compositions comprising said compounds.
2. Related Art Statement
Liquid crystal display devices have various excellent features such as low-voltage operability, lower electricity consumption, being thin and light-weight, being a non-emissive type and easy on the eye, etc. Accordingly, they are in wide use as various display devices.
Liquid crystal display devices using a nematic liquid crystal operating in the so-called twisted nematic mode (TN mode) are in use currently. However, display devices using this kind of nematic liquid crystal have the drawback of being very slow in response as compared to luminescent type display devices such as CRT, EL and the like. When the liquid crystal display devices using a nematic liquid crystal are applied in a large-scale display device capable of displaying a large amount of information, it is impossible to obtain a display of good contrast because of insufficient threshold characteristic. Thus the liquid crystal display devices using a nematic liquid crystal have had a limitation for wide application. There has recently been developed a liquid crystal display device using a nematic liquid crystal operating in the so-called super twisted nematic mode (STN mode) or SBE and capable of giving a display of improved contrast because of improved threshold characteristic. Even in this STN mode liquid crystal display device, however, the response is not sufficiently improved, and therefore said device has a limitation for application to displays capable of displaying a still larger amount of information. Hence, various attempts have been made to develop a new liquid crystal display system which is applicable to large-scale displays capable of displaying a large amount of information.
Ferroelectric liquid crystals have a memory characteristic and give a high speed response, and accordingly their application to large-scale displays is highly expected. As liquid crystals having ferroelectric properites, there are known those showing a chiral smectic C phase, a chiral smectic H phase, a chiral smectic J phase, etc. Of these ferroelectric liquid crystals, those showing a chiral smectic C phase are thought to have highest practical utility. Ferroelectric liquid crystals showing a chiral smectic C phase were first synthesized in 1975 by R. B. Meyer et al.; one typical example thereof is 2-methylbutyl 4-(4'-n-decyloxybenzylideneamino)cinnamate (hereinafter abbreviated to DOBAMBC) [J. Physique, 36, L-69 (1975)]. A thin film liquid crystal cell was prepared using DOBAMBC and was found to have a high speed response in the order of μsec and a memory characteristic [N. A. Clark et al., Appl. Phys. Lett., 36, 89 (1980)].
Since that time, there was started the development of optical modulation devices (e.g. liquid crystal display devices, photo-printer heads) using a ferroelectric liquid crystal showing a chiral smectic C phase (hereinafter may be referred to simply as "ferroelectric liquid crystal").
As a result, a number of ferroelectric liquid crystal compounds showing a chiral smectic C phase have been developed since then, and various ferroelectric liquid crystal compounds are already known. However, no ferroelectric liquid crystal compound is found yet which has satisfactory reliability and capability for use in large-scale displays, etc.
In order for a ferroelectric liquid crystal to be practically used in a liquid crystal display device, etc., the liquid crystal must be superior in high speed response, orientation, memory characteristic, characteristic of threshold voltage, temperature dependences of these properties, etc. Also, the ferroelectric liquid crystal is required to show a chiral smectic C phase over a wide temperature change so that it can operate within a sufficiently wide temperature range including room temperature, and further to have excellent physical and chemical stabilities.
Of these requirements, particularly important are physical and chemical stabilities and stable expression of high speed response and memory characteristic.
It is reported by Clarkl et al. based on their experiment that a response in the order of μsec is possible under certain conditions. However, even if the conditions used by Clark et al. could have materialyzed a large-scale display capable of displaying a large amount of information, i.e. a display having a very large number of pixels, the display must show a faster response.
The response time (τ) of a ferroelectric liquid crystal is approximately given by the following formula when a torque generated by the dielectric anisotropy and an external electric field is neglected.
τ=η/PsE
(τ is a response time, η is a viscosity coefficient, Ps is a spontaneous polarization, and E is an applied electric field). Therefore, increase in spontaneous polarization is effective to obtain a faster (shorter time) response.
Meanwhile, memory characteristic is considered to improve dependently upon the value of spontaneous polarization. Increase in spontaneous polarization gives rise to increase in polarization electric field, which brings about uniformity of dipole moment, i.e. stabilization of memory condition.
Thus, increase in spontaneous polarization is very effective for the simultaneous solution of the two tasks perculiar to ferroelectric liquid crystals. Hence, development of ferroelectric liquid crystal compounds with increased spontaneous polarization has recently been pushed forward. As a result, there have been reported, for example, ferroelectric liquid crystal compounds of ester type using, as an optically active group, (R)- or (S)-1-methyl butanol or (R)- or (S)-1-methylheptanol, which are stable physically and chemically [K. Terashima et al., Mol. Cryst. Liq. Cryst., 141, 237 (1986)]. These compounds have a relatively high spontaneous polarization of 50 nC/cm 2 or more, but the value is not sufficient.
In order to obtain a larger spontaneous polarization, there have been synthesized compounds having two asymmetric carbon atoms in the optically active group which is essential for the expression of a chiral smectic C phase. These compounds include, for example, liquid crystal compounds having a dichiral epoxide side chain [David M. Walba et al., Journal of American Chemical Society, 108, 7424 (1986)], and liquid crystal compounds having a halogen atom and a methyl group on two adjacent asymmetric carbon atoms [cf. e.g. JP-A-168780/1985, 218358/1985, 68449/1986, 30740/1987, 46/1987, 103043/1987, 111950/1987, 142131/1987, 175443/1987].
A typical example of the above liquid crystal compounds is 4'-octylcarbonyloxy-4-biphenyl (S)-3-methyl-2-chloropentanoate [JP-A-68449/1986]. This liquid crystal compound has a very large spontaneous polarization of 180 nC/cm 2 , but, being an aliphatic chloro compound, has poor chemical stability. Hence, there has been synthesized 4'-octylarbonyloxy-4-[(S)-2-methoxy-(S)-3-methylpentyloxycarbonyl]biphenyl [JP-A-228036/1987]. This compound has excellent chemical stability but has a small spontaneous polarization of 17 nC/cm 2 . Thus, no compound has been developed yet which is chemically stable and yet has a large spontaneous polarization.
OBJECT AND SUMMARY OF THE INVENTION
The present inventors made investigation in order to find out a ferroelectric liquid crystal compound having excellent physical and chemical stabilities and a large spontaneous polarization, and have reached the present invention. That is, the present inventors made investigation on liquid crystal compounds wherein a chemically stable ester compound and an optically active group having two asymmetric carbon atoms are combined, particularly on the correlation of the chemical structure of the optically active group and the spontaneous polarization of the resulting liquid crystal compound, and have reached the present invention based on the results of the investigation.
The spontaneous polarization of a ferroelectric liquid crystal depends on the dipole moment of the ether group or carboxylic acid ester group bonding to the asymmetric carbons. When a polar group such as ether group, carboxylic acid ester group or the like is allowed to bond to each of the two asymmetric carbons, the correlation of the dipole moment vectors of the two polar groups is important. That is, it was found that fixing the steric conformation of the two polar groups, i.e. preventing the free rotation of the bond between the two asymmetric carbon atoms is very effective to obtain a large spontaneous polarization. Thus, a large spontaneous polarization has been successuflly obtained by fixing the steric conformation of the polar groups on the asymmetric carbon atoms, without using a halogen-atom bond which has poor chemical stability.
BRIEF DESCRIPTION OF DRAWING
FIG. 1 is a schematic illustration of an example of the liquid crystal display device according to the present invention. 1 and 2 are each a polarization plate; 2 is a front side glass; 3 and 6 are each a transparent electrode; 4 is a ferroelectric liquid crystal phase; 5 is a seal; 7 is a back side glass.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The present invention relates to optically active compounds represented by the general formula ##STR3## wherein R 1 is an alkyl group, an alkenyl group or an alkynyl group each of 3-14 carbon atoms; R 2 is an alkyl group of 1-10 carbon atom, an alkenyl group of 2-10 carbon atoms an alkynyl group of 2-10 carbon atoms; ##STR4## is a five- to eight-membered ring which may contain heteroatom(s) or double bond(s); Q 1 is a single bond, a (thio)ether group, a carboxylic acid ester group, a carbony group or a carbonyldioxy group; Q 2 and Q 3 are independently a single bond, a (thio)ether group, a carboxylic acid ester group, a carbonyl group, a carbonyldioxy group or a methyleneoxy group; M is ##STR5## X and Y are independently a single bond, a carboxylic acid ester group, a methyleneoxy group or an ethylene group, and ##STR6## are independently a homocyclic or heterocyclic six-membered ring-1,4-diyl group which may contain 1-2 oxygen or nitrogen atoms as ring-forming atoms); the carbon atoms with the asterisk (*) denote asymmetric carbon atoms; the hydrogen atoms bonding to the asymmetric carbon atoms may be substituted with a lower alkyl group of 1-6 carbon atoms or a lower alkenyl group of 2-6 carbon atoms.
The liquid crystal compounds I of the present invention have properties essential for ferroelectric liquid crystal compounds, despite the steric conformation of the polar groups on the asymmetric carbon atoms of the ring portion, and are characterized by expressing a large spontaneous polarization when the two polar groups on the asymmetric carbon atoms are in a same direction steric conformation. For example, when steric conformation of the two polar groups on the asymmetric carbon atoms of the ring portion is formed in such a way that a 5-membered ring or the like is formed using two adjacent asymmetric carbon atoms and Q 2 and Q 3 are allowed to be in the same direction relative to the plane of the ring, i.e. in a cis form, the vectors of the dipole moments of Q 2 and Q 3 have the same direction and as a result a large spontaneous polarization can be obtained.
Therefore, the first aspect of the present invention lies in liquid crystal compounds having a large spontaneous polarization; the second aspect lies in liquid crystal compositions comprising at least one of said optically active compounds; the third aspect lies in liquid crystal optical modulators using said liquid crystal compositions.
The compounds I relating to the first aspect of the present invention can be classified into the following compounds I' and I", depending upon the basic skeleton M. ##STR7##
In the above compounds I, I' and I", the alkyl groups of 3-14 carbon atoms, represented by R 1 can be of straight chain or branched chain. Specifically, there can be mentioned straight chain alkyl groups such as propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl and the like, as well as branched chain alkyl groups such as isopropyl, isobutyl, sec-butyl, tert-butyl, isopentyl, neopentyl, tert-pentyl, isohexyl, 1-methylpentyl, 2-methylpentyl, 5-methylhexyl, 2,3,5-trimethylhexyl, 2,7,8-trimethyldecyl, 4-ethyl-5-methylnonyl and the like. Of these, preferable are straight chain alkyl groups of 6-12 carbon atoms, such as hexyl, heptyl, octyl, decyl, undecyl, dodecyl and the like.
As the alkenyl groups and alkynyl groups represented by R 1 , there can be mentioned, for example, those alkenyl and alkynyl groups corresponding to the above alkyl groups.
The alkyl groups of 1-10 carbon atoms represented by R 2 can be of straight chain or branched chain. Specifically, there can be mentioned straight chain alkyl groups such as methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl and the like, as well as branched chain alkyl groups such as isopropyl, isobutyl, sec-butyl, tert-butyl, isopentyl, neopentyl, tert-pentyl, isohexyl, 1-methylpentyl, 2-methylpentyl, 5-methylhexyl, 4-ethylhexyl, 2,3,5-trimethylhexyl, 4-ethyl-5-methylhexyl and the like. Of these, preferable are straight chain alkyl groups of 1-8 carbon atoms, such as methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl and octyl.
As the alkenyl and alkynyl groups represented by R 2 , there can be mentioned, for example, those alkenyl and alkynyl groups corresponding to the above alkyl groups.
Q 1 , Q 2 and Q 3 each represent a single bond, a (thio)ether group, a carboxylic acid ester group, a carbonyl group, a carbonyldioxy group or a methyleneoxy group.
As the carboxylic acid ester group, there can be mentioned a ##STR8## ester group and a ##STR9## ester group.
As the methylenoxy group, there can be mentioned a --CH 2 O-- group and a --OCH 2 -- group.
With respect to the various bond and groups which can be taken by Q 1 , Q 2 and Q 3 , Q 1 is preferably a single bond, a (thio)ether group or a ##STR10## ester group; Q 2 is preferably a ##STR11## ester group, a ##STR12## ester group or an ether group; and Q 3 is preferably a (thio)ether group, a ##STR13## ester group or a ##STR14## ester group.
As the carboxylic acid ester group represented by X or Y, there can be mentioned a ##STR15## ester group and a ##STR16## ester group. As the methylenoxy group represented by X or Y, there can be mentioned a --CH 2 O-- group and a --OCH 2 -- group.
As the six-membered ring-1,4-diyl group represented by ##STR17## there can be specifically mentioned, for example, p-phenylene, 1,4-cyclohexylene, 2,5-(1,3-dioxane)diyl, 2,5-pyridinediyl, 2,5-pyrimidinediyl, 2,5-(1,4-pyrazine)diyl and 3,6-(1,2-pyridazine)diyl. These rings may be substituted with halogen, cyano, methyl or methoxy. ##STR18## may be the same or different.
2,5-(1,3-Dioxane)diyl can be ##STR19## 2,5-pyridinediyl cab be ##STR20## 2,5-pyrimidinediyl can be ##STR21##
When M is ##STR22## preferable combinations of ##STR23## X and Y include the case where one of X and Y is a single bond, the other of them is a carboxylic acid ester bond, and all of ##STR24## are p-phenylene or one of them is 2,5-pyrimidinediyl. When M is ##STR25## preferable combinations of and X include the case where X is a single bond and both of ##STR26## are p-phenylene or one of them is 2,5-pyrimidinediyl.
The compounds I have two asymmetric carbon atoms within the molecule and therefore have four different optical isomers, that is, (R,R) type (R,S) type, (S,R) type and (S,S) type.
The compounds I of the present invention can be produced according to, for example, the following processes.
Method 1
Compounds of the general formula I wherein Q 2 is a ##STR27## ester group. ##STR28## (R 1 , R 2 , Q 1 , Q 3 and M have the same definitions as above. The same applies hereinafter.)
As shown in the above scheme 1, the compound I can be obtained by subjecting a carboxylic acid II and an optically active dichiral alcohol III to a condensation reaction. This condensation reaction per se is known and can be effected according to a conventional method. For example, the carboxylic acid II and the dichiral alcohol III are condensed in an organic solvent in the presence of a proton acid. As the proton acid, there can be used, for example, inorganic acids such as sulfuric acid, hydrochloric acid, perchloric acid and the like; organic sulfonic acids such as p-toluene-sulfonic acid, benzenesulfonic acid, trifluoromethane-sulfonic acid, methanesulfonic acid and the like; and strongly acidic ion exchange resins such as Amberlist® and the like. As the organic solvent, there can be mentioned, for example, hydrocarbons such as hexane, benzene, toluene and the like, halogenated hydrocarbons such as chloroform, methylene chloride, carbon tetrachloride, 1,2-dichloroethane and the like, ethers such as diethyl ether, tetrahydrofuran, dioxane and the like, ethyl acetate, acetonitrile and dimethylformamide. It is possible that the carboxylic acid II be converted to an acid halide with, for example, a halogenating agent such as phosphorus pentachloride, thionyl chloride, thionyl bromide or the like and the halide be reacted with the dichiral alcohol III in the above mentioned organic solvent in the presence of, for example, a tertiary amine such as pyridine, triethylamine or the like. It is further possible that the alcohol III be converted to a trimethylsilyl ether derivative ##STR29## and the ether be condensed with an acid halide derivative of the carboxylic acid II in the presence of a Lewis acid such as zinc chloride or the like.
It is furthermore possible that the carboxylic acid II and the alcohol III be reacted with an activating agent such as N,N'-dicyclohexylcarbodiimide (DCC), Mukaiyama's reagent illustrated by a 1-methyl-2-halopyridium iodide, diethyl azodicarboxylate (DEAD) and triphenylphosphine (Ph 3 P) (Mitsunobu's reagent), triphenylphosphine dibromide or the like.
These methods are described in, for example, J. Org. Chem., 27, 4675 (1962); Tetrahedron Lett., 1978, 4475; Chemistry Lett., 1975, 1045; Chemistry Lett., 1976, 13; Bull. Chem. Soc. Japan, 50, 1863 (1977); Bull, Chem. Soc. Japan. 40, 2380 (1967); Syn. Commun., 16, 1423 (1986); and Syh. Commun., 16, 659 (1986).
Method 2
Compounds of the general formula I wherein Q 2 is a ##STR30## group. ##STR31##
As shown in the above scheme 2, the compound I can be obtained by subjecting a hydroxyl group-containing compound IV and an optically active dichiral carboxylic acid V to a condensation reaction. This condensation reaction per se is known and can be effected according to a conventional method.
Method 3
Compounds of the general formula I wherein Q 2 is an ether group (--O--). ##STR32##
As shown in the above scheme 3, the compound I can be obtained by subjecting a hydroxyl group-containing compound IV and an optically active dichiral alcohol III to an etherification reaction. This etherification reaction per se is known and can be effected according to a conventional method. For example, the reaction can be effected with diethyl azodicarboxylate (DEAD) and triphenylphosphine (Ph 3 P) (S. Bittner et al., Chem. & Ind., 1975, 281).
It is also possible that the dichiral alcohol III and an organic sulfonyl chloride be reacted in an organic solvent in the presence of an organic base (e.g. pyridine, triethylamine) or an inorganic base (e.g. sodium hydride) to obtain a corresponding organic sulfonic acid ester and the ester be reacted with the hydroxyl group-containing compound IV. This reaction is conducted in an organic solvent in the presence of an inorganic base (e.g. potassium carbonate, sodium hydride) or an organic base (e.g. pyridine, triethylamine). As the organic sulfonyl chloride usable in the reaction, there can be mentioned, for example, aromatic sulfonyl chlorides such as p-toluenesulfonyl chloride, o-toluenesulfonyl chloride, p-chlorobenzenesulfonyl chloride, benzenesulfonyl chloride, α-naphthalenesulfonyl chloride, β-naphthalenesulfonyl chloride and the like, as well as aliphatic sulfonyl chlorides such as methanesulfonyl chloride, trifluoromethanesulfonyl chloride and the like.
As the organic solvent usable in the etherification reaction, there can be mentioned, for example, aliphatic hydrocarbons (e.g. hexane, cyclohexane), halogenated hydrocarbons (e.g. chloroform, methylene chloride, carbon tetrachloride, 1,2-dichloroethane), ethers (e.g. diethyl ether, tetrahydrofuran, dioxane), aromatic hydrocarbons (e.g. benzene, toluene), ethyl acetate, acetonitrile, dimethylformamide (DMF), dimethyl sulfoxide (DMSO) and hexamethylphosphoric triamide (HMPA).
In the etherification reaction, the activation of the dichiral alcohol III can be effected not only by converting the dichiral alcohol III to the above mentioned organic sulfonic acid ester but also by converting the alcohol III to a halogen derivative. The conversion to a halogen derivative can be effected by, for example, reacting the organic sulfonic acid ester with a metal halide (e.g. sodium iodide, potassium iodide). Or, the dichiral alcohol III can be directly reacted with a halogenating agent such as phosphorus pentachloride, thionyl chloride, thionyl bromide or the like. The thus obtained halogen derivative can be reacted with the hydroxyl group-containing compound IV in organic solvent in the presence of the above mentioned inorganic or organic base.
Q 2 also represents a single bond, a carbonyl group, a carbonyldioxy group or a methyleneoxy group, and those compounds of the general formula I having, as Q 2 one of these bonds or groups can also be produced according to a conventional method.
The compounds I obtained by the above processes can be separated from the reaction mixture and purified by ordinary separation and purification methods such as extraction, solvent operation, column chromatography, liquid chromatography, recrystallization and the like.
All of the starting materials II, III, IV and V for production of the optically active compounds I of the present invention are known substances or can be easily derived from known substances. For example, the optically active dichiral compound III or V is a novel compound and can be derived from known optically active dichiral compounds, and can also be obtained by, for example, a chemical asymmetric synthesis [J. D. Morrison et al., Asymmetric Synthesis, vol. 1 (1983) to vol. 5 (1985); B. Bosnich et al., Asymmetric Catalysis (1986); M. A. Sutter et al., Ann., 1983, 939], a biological asymmetric synthesis using an enzyme or a microorganism [J. B. Jones et al., "Applications of Biochemical Systems in Organic Chemistry", John Wiley, New York (1976); G. Frater et al., Tetrahedron, 40, 1269 (1984); R. W. Hoffman et al., Chem. Bet., 114, 2786 (1981); K. Nakamura et al., Tetrahedron Lett., 27, 3155 (1986)], and an optical resolution [J. Jacques et al., "Enantiomers, Racemates and Resolutions", John Wiley & Sons (1981); A. W. Ingersoll, Org. Synth., Coll. vol., 2, 506 (1943); H. Nohira et al., Chemistry Lett., 1981, 875, 951]. The thus obtained dichiral compound III or V can be subjected to inversion of configuration on asymmetric carbon by a chemical or biological method convert it into other optical isomer(s). As the typical methods for inverting the hydroxyl group of optically active secondary alcohol, there are known, for example, method in which the hydroxyl group is converted into an organic sulfonic acid ester and then subjected to an intramolecular nucleophillic substitution reaction to effect inversion [E. J. Corey et al., Tetrahedron Lett., 1975, 3183; D. T. Sawyer and M. J. Gibian, Tetrahedron, 35, 471 (1979); W. H. Kruizinger et al., J. Org. Chem., 46, 4321 (1981); J. W. Hoffman and R. C. Desai, Syn. Commun., 13, 553 (1983)], a method in which an optically active secondary alcohol is activated by N,N'-dicyclohexylcarbodiimide (DCC) in the presence of cuprous chloride and then reacted with an appropriate carboxylic acid to effect inversion [J. Kaulen, Angew. Chem., 99, 800 (1987)], and a method in which an optically active secondary alcohol is reacted with diethyl azodicarboxylate (DEAD), triphenylphosphine (Ph 3 P) and an appropriate carboxylic acid to effect inversion [O. Mitsunobu and E. Eguchi, Bull. Chem. Soc. Japan, 44, 3427 (1971); O. Mitsunobu, Synthesis, 1981, 1].
In the optically active dichiral secondary alcohol III and optically active dichiral carboxylic acid V which are both the important materials for the dichiral portion of the optically active compounds of the present invention, the ##STR33## is a five- to eight-membered alicyclic compound, a five- to eight-membered cyclic compound containing heteroatom(s) or a five- to eight-membered cyclic compound containing double bond(s)
These cyclic compounds may have, on the asymmetric carbon atoms and other ring-forming atoms, substituent(s) such as lower alkyl group of 1-6 carbon atoms, alkenyl group of 2-6 carbon atoms and the like.
When the ##STR34## is an alicyclic compound, it may be any of five- to eight-membered rings, but is preferably a five- or six-membered ring. It is specifically as follows when shown by the general formula. ##STR35## In the above formula, however, when m=n and the ring group has no substituent, the carbon atoms with the asterisk (*) are not asymmetric carbon atoms; therefore, such an alicyclic compound is excluded from the present invention.
When the ##STR36## is an alicyclic compound, examples of the compounds represented by the general formula III and the general formula V are as follows.
Examples of the optically active dichiral secondary alcohol III wherein Q 3 is an ether group (--O--), are as follows. ##STR37##
Specific examples of this alcohol include straight chain alkyloxy cyclopentanols such as 2-methoxy cyclopentanol, 2-ethoxycyclopentanol, 2-propoxycyclopentanol, 2-butoxycyclopentanol, 2-pentyloxycyclopentanol, 2-hexyloxycyclopentanol, 2-heptyloxycyclopentanol, 2-octyloxycyclopentanol, 2-nonyloxycyclopentanol, 2-decyloxycyclopentanol and the like, as well as branched chain alkyloxycyclopentanols such as 2-isopropoxycyclopentanol, 2-isobutoxycyclopentanol, 2-tert-butoxycyclopentanol, 2-(2-methylpentyloxy)cyclopentanol, 2-(3-methylpentyloxy)cyclopentanol and the like. ##STR38##
Specific examples of this compound include straight chain alkyloxycyclohexanols such as 2-methoxycyclohexanol, 2-ethoxycyclohexanol, 2-propoxycyclohexanol, 2-butoxycyclohexanol, 2-pentyloxycyclohexanol, 2-hexyloxcyclohexanol, 2-heptyloxycyclohexanol, 2-octyloxycyclohexanol, 2-nonyloxycyclohexanol, 2-decyloxycyclohexanol and the like, as well as branched chain alkyloxycyclohexanols such as 2-isopropoxycyclohexanol, 2-isobutoxycyclohexanol, 2-tert-butoxycyclohexanol, 2-(2-methylpentyloxy)cyclohexanol, 2-(3-methylpentyloxy)cyclohexanol and the like. ##STR39##
Specific examples of this compound include straight chain alkyloxycycloheptanols such as 2-methoxycycloheptanol, 2-ethoxycycloheptanol, 2-propoxycycloheptanol, 2-butoxycycloheptanol, 2-pentyloxycycloheptanol, 2-hexyloxycycloheptanol, 2-heptyloxycycloheptanol, 2-octyloxycycloheptanol, 2-nonyloxycycloheptanol, 2-decyloxycycloheptanol and the like, as well as branched chain alkyloxycycloheptanols such as 2-isopropoxycycloheptanol, 2-isobutoxycycloheptanol, 2-tert-butoxycycloheptanol, 2-(2-methylpentyloxy)cycloheptanol, 2-(3-methylpentyloxy)cycloheptanol and the like. ##STR40##
Specific examples of this compound include straight chain alkyloxycyclooctanols such as 2-methoxycyclooctanol, 2-ethoxycyclooctanol, 2-propoxycyclooctanol, 2-butoxycyclooctanol, 2-pentyloxycyclooctanol, 2-hexyloxycyclooctanol, 2-heptyloxycyclooctanol, 2-octyloxycyclooctanol, 2-nonyloxycyclooctanol, 2-decyloxycyclooctanol and the like, as well as branched alkyloxycyclooctanols such as 2-isopropoxycyclooctanol, 2-isobutoxycyclooctanol, 2-tert-butoxycyclooctanol, 2-(2-methylpentyloxy)cyclooctanol, 2-(3-methylpentyloxy)cyclooctanol and the like. ##STR41##
Specific examples of this compound include straight chain alkyloxycyclopentanols such as 3-methoxycyclopentanol, 3-ethoxycyclopentanol, 3-propoxycyclopentanol, 3-butoxycyclopentanol, 3-pentyloxycyclopentanol, 3-hexyloxycyclopentanol, 3-heptyloxycyclopentanol, 3-octyloxycyclopentanol, 3-nonyloxycyclopentanol, 3-decyloxycyclopentanol and the like, as well as alkyloxycyclopentanols such as 3-isopropoxycyclopentanol, 3-isobutoxycyclopentanol, 3-tert-butoxycyclopentanol, 3-(2-methylpentyloxy)cyclopentanol, 3-(3-methylpentyloxy)cyclopentanol and the like.
Specific examples of other homologues of the alicyclic secondary alcohol III wherein Q 3 is an ether group, are as follows. ##STR42##
Specific examples of the optically active dichiral secondary alcohol III wherein Q 3 is a ##STR43## ester group, are as follows. ##STR44##
Specific examples of the optically active dichiral secondary alochol III wherein Q 3 is a ##STR45## ester group, are as follows. ##STR46##
Examples of the optically active cyclic dichiral carboxylic acid V are as follows.
Examples of the optically active cyclic dichiral carboxylic acid V wherein Q 3 is an ether group (--O--), are as follows ##STR47##
Specific examples of this compound include straight chain alkyloxycyclopentanecarboxylic acids such as 2-methoxycyclopentanecarboxylic acid, 2-ethoxycyclopentanecarboxylic acid, 2-propoxycyclopentanecarboxylic acid, 2-butoxycyclopentanecarboxylic acid, 2-pentyloxycyclopentanecarboxylic acid, 2-hexyloxycyclopentanecarboxylic acid, 2-heptyloxycyclopentanecarboxylic acid, 2-octyloxycyclopentanecarboxylic acid, 2-nonyloxycyclopentanecarboxylic acid, 2-decycloxycyclopentanecarboxylic acid and the like, as well as branched chain alkyloxycyclopentanecarboxylic acids such as 2-isopropoxycyclopentanecarboxylic acid, 2-isobutoxycyclopentanecarboxylic acid, 2-tert-butoxycyclopentanecarboxylic acid, 2-(2-methylpentyloxy)cyclopentanecarboxylic acid, 2-(3-methylpentyloxy)cyclopentanecarboxylic acid and the like. ##STR48##
Specific examples of this compound include straight chain alkyloxycyclohexanecarboxylic acids such a 2-methoxycyclohexanecarboxylic acid, 2-ethoxycyclohexanecarboxylic acid, 2-propoxycyclohexanecarboxylic acid, 2-butoxycyclohexanecarboxylic acid, 2-pentyloxycyclohexanecarboxylic acid, 2-hexyloxycyclohexanecarboxylic acid, 2-heptyloxycyclohexanecarboxylic acid, 2-octyloxycyclohexanecarboxylic acid, 2-nonyloxycyclohexanecarboxylic acid, 2-decyloxycyclohexanecarboxylic acid and the like, as well as branched chain alkyloxycyclohexanecarboxylic acids such as 2-isopropoxycyclohexanecarboxylic acid, 2-isobutoxycyclohexanecarboxylic acid, 2-tert-butoxycyclohexanecarboxylic acid, 2-(2-methylpentyloxy)cyclohexanecarboxylic acid, 2-(3-methylpentyloxy)cyclohexanecarboxylic acid and the like. ##STR49##
Specific examples of this compound include straight chain alkyloxycycloheptanecarboxylic acid such as 2-methoxycycloheptanecarboxylic acid, 2-ethoxycycloheptanecarboxylic acid, 2-propoxycycloheptanecarboxylic acid, 2-butoxycycloheptanecarboxylic acid, 2-pentyloxycycloheptanecarboxylic acid, 2-hexyloxycycloheptanecarboxylic acid, 2-heptyloxycycloheptanecarboxylic acid, 2-octyloxycycloheptanecarboxylic acid, 2-nonyloxycycloheptanecarboxylic acid, 2-decyloxycycloheptanecarboxylic acid and the like, as well as branched chain alkyloxycycloheptanecarboxylic acids such as 2-isopropoxycycloheptanecarboxylic acid, 2-isobutoxycycloheptanecarboxylic acid, 2-tert-butoxycycloheptanecarboxylic acid, 2-(2-methylpentyloxy)cycloheptanecarboxylic acid, 2-(3-methylpentyloxy)cycloheptanecarboxylic acid and the like. ##STR50##
Specific examples of this compound include straight chain alkyloxycyclooctanecarboxylic acids such as 2-methoxycyclooctanecarboxylic acid, 2-ethoxycyclooctanecarboxylic acid, 2-propoxycyclooctanecarboxylic acid, 2-butoxycyclooctanecarboxylic acid, 2-pentyloxycyclooctanecarboxylic acid, 2-hexyloxycyclooctanecarboxylic acid, 2-heptyloxycyclooctanecarboxylic acid, 2-octyloxycyclooctanecarboxylic acid, 2-nonyloxycyclooctanecarboxylic acid, 2-decycloxycyclooctanecarboxylic acid and the like, as well as branched chain alkyloxycyclooctanecarboxylic acids such as 2-isopropoxycyclooctanecarboxylic acid, 2-isobutoxycyclooctanecarboxylic acid, 2-tert-butoxycyclooctanecarboxylic acid, 2-(2-methylpentyloxy)cyclooctanecarboxylic acid, 2-(3-methylpentyloxy)cyclooctanecarboxylic acid and the like.
Examples of the optically active cyclic dichiral carboxylic acid V wherein Q 3 is a ##STR51## ester group, are as follows. ##STR52##
Specific examples of the optically active cyclic dichiral carboxylic acid V wherein Q 3 is a ##STR53## ester group, are as follows. ##STR54##
The optically active cyclic dichiral carboxylic acid V wherein Q 3 is an ether group (--O--), also includes the followings. ##STR55##
Specific examples of this compound include straight chain alkyloxycyclopentanecarboxylic acids such as 3-methoxycyclopentanecarboxylic acid, 3-ethoxycyclopentanecarboxylic acid, 3-propoxycyclopentanecarboxylic acid, 3-butoxycyclopentanecarboxylic acid, 3-pentyloxycyclopentanecarboxylic acid, 3-hexyloxycyclopentanecarboxylic acid, 3-heptyloxycycloheptanecarboxylic acid, 3-octyloxycyclopentanecarboxylic acid, 3-nonyloxycyclopentanecarboxylic acid, 3-decyloxycyclopentanecarboxylic acid and the like, as well as branched chain alkyloxycyclopentanecarboxylic acids such as 3-isopropoxycyclopentanecarboxylic acid, 3-isobutoxycyclopentanecarboxylic acid, 3-tert-butoxycyclopentanecarboxylic acid, 3-(2-methylpentyloxy)cyclopentanecarboxylic acid, 3-(3-methylpentyloxy)cyclopentanecarboxylic acid and the like.
Specific examples of other homologues of the 3-alkyloxycyclopentanecarboxylic acid are as follows. ##STR56##
The optically active cyclic dichiral carboxylic acid V wherein Q 3 is a ##STR57## ester bond, also includes the following compounds. ##STR58##
The optically active cyclic dichiral carboxylic acid V wherein Q 3 is a ##STR59## ester group, also includes the following compounds. ##STR60##
The optically active cyclic dichiral carboxylic acid V wherein Q 3 is an ether group (--O--), further includes the following compounds. ##STR61##
The optically active cyclic dichiral carboxylic acid V wherein Q 3 is a ##STR62## ester group, further includes the following compounds. ##STR63##
The optically active cyclic-dichiral carboxylic acid V wherein Q 3 is a ##STR64## ester group, further includes the following compounds. ##STR65##
When ##STR66## is five to eight-membered heterocyclic compound, there can be mentioned a sulfur or oxygen atom as the hetero-atom in the heterocyclic ring.
When ##STR67## is heterocyclic compound containing a hetero-atom, examples of the compounds represented by the general formula IV and V are as follows.
When ##STR68## is five-membered ring containing a hetero-atom, for example, a sulfur atom and Q 3 is an ether group (--O--), there can be mentioned the following example. ##STR69##
Specific examples of this compound include straight chain 4-alkyloxytetrahydrothiophen-3-ols such as 4-methoxytetrahydrothiophen-3-ol, 4-ethoxytetrahydrothiophen-3-ol, 4-propoxytetrahydrothiophen-3-ol, 4-butoxytetrahydrothiophen-3-ol, 4-pentyloxytetrahydrothiophen-3-ol, 4-hexyloxytetrahydrothiophen-3-ol, 4-heptyloxytetrahydrothiophen-3-ol, 4-octyloxytetrahydrothiophen-3-ol, 4-nonyloxytetrahydrothiophen-3-ol, 4-decyloxytetrahydrothiophen-3-ol and the like, as well as branched chain 4-alkyloxytetrahydrothiophen-3-ols such as 4-isopropoxytetrahydrothiophen-3-ol, 4-isobutoxytetrahydrothiophen-3-ol, 4-tert-butoxytetrahydrothiophen-3-ol, 4-(2-methylpentyloxy)tetrahydrothiophen-3-ol, 4-(3-methylpentyloxy)tetrahydrothiophen-3-ol and the like.
When ##STR70## is a five-membered ring containing a sulfur atom and Q 3 is a ##STR71## ester group, there can be mentioned the following example. ##STR72##
Specific examples of this compound include straight chain alkyl ester derivatives such as methyl 4-hydroxytetrahydrothiophene-3-carboxylate, ethyl 4-hydroxytetrahydrothiophene-3-carboxylate, propyl 4-hydroxytetrahydrothiophene-3-carboxylate, butyl 4-hydroxytetrahydrothiophene-3-carboxylate, pentyl 4-hydroxytetrahydroxythiophene-3-carboxylate, hexyl 4-hydroxytetrahydrothiophene-3-carboxylate, heptyl 4-hydroxytetrahydrothiophene-3-carboxylate, octyl 4-hydroxytetrahydrothiophene-3-carboxylate, nonyl 4-hydroxytetrahydrothiophene-3-carboxylate, decyl 4-hydroxytetrahydrothiophene-3-carboxylate and the like, as well as branched chain alkyl ester derivatives such as isopropyl 4-hydroxytetrahydrothiophene-3-carboxylate, isobutyl 4-hydroxytetrahydrothiophene-3-carboxylate, tert-butyl 4-hydroxytetrahydrothiophene-3-carboxylate, 2-methylpentyl 4-hydroxytetrahydrothiophene-3-carboxylate, 3-methylpentyl 4-hydroxytetrahydrothiophene-3-carboxylate, and the like.
When ##STR73## is five-mentioned ring containing a sulfur atom and Q 3 is a ##STR74## ester group, there can also be mentioned the following example. ##STR75##
Specific examples of this compound include straight chain alkyl ester derivatives such as methyl 3-hydroxytetrahydrothiophene-2-carboxylate, ethyl 3-hydroxytetrahydrothiophene-2-carboxylate, propyl 3-hydroxytetrahydrothiophene-2-carboxylate, butyl 3-hydroxytetrahydrothiophene-2-carboxylate, pentyl 3-hydroxytetrahydrothiophene-2-carboxylate, hexyl 3-hydroxytetrahydrothiophene-2-carboxylate, heptyl 3-hydroxytetrahydrothiophene-2-carboxylate, octyl 3-hydroxytetrahydrothiophene-2-carboxylate, nonyl 3-hydroxytetrahydrothiophene-2-carboxylate, decyl 3-hydroxytetrahydrothiophene-2-carboxylate and the like, as well as branched chain alkyl ester derivatives such as isopropyl 3-hydroxytetrahydrothiophene-2-carboxylate, isobutyl 3-hydroxytetrahydrothiophene-2-carboxylate, tert-butyl 3-hydroxytetrahydrothiophene-2-carboxylate, 2-methylpentyl 3-hydroxytetrahydrothiophene-2-carboxylate, 3-methylpentyl 3-hydroxytetrahydrothiophene-2-carboxylate and the like.
When ##STR76## is a five-membered righ containing a sulfur atom and Q 3 is a ##STR77## ester group, there can be mentioned the following example. ##STR78##
Specific examples of this compound include straight chain acyloxy derivatives such as 4-acetyloxytetrahydrothiophen-3-ol, 4-propionyloxytetrahydrothiophen-3-ol, 4-butyryloxytetrahydrothiophen-3-ol, 4-valeryloxytetrahydrothiophen-3-ol, 4-heptanoyloxytetrahydrothiophen-3-ol, 4-octanoyloxytetrahydrothiophen-3-ol, 4-nonanoyloxytetrahydrothiophen-3-ol, 4-decanoyloxytetrahydrothiophen-3-ol and the like, as well as branched chain acyloxy derivatives such as 4-isobutyryloxytetrahydrothiophen-3-ol, 4-isovaleryloxytetrahydrothiophen-3-ol, 4-pivaloyloxytetrahydrothiophen-3-ol, 4-(2-methylpentanoyloxy)tetrahydrothiophen-3-ol, 4-(3-methylpentanoyloxy)tetrahydrothiophen-3-ol and the like.
In the above, there were described specific examples of the optically active cyclic secondary alcohol III wherein ##STR79## is a five-membered ring containing a sulfur atom and Q 3 is an ether group, a ##STR80## ester group or a ##STR81## ester group. However, the alcohol III is not restricted to these examples. For example when ##STR82## is a five-mentioned ring containing sulfur atom of high oxidation degree, i.e. a sulfoxide or a sulfone, there can be mentioned the following examples. ##STR83##
Also when ##STR84## is a six-mentioned ring containing a sulfur atom, there can be membered similar derivatives.
Also when ##STR85## is a five or six-mentioned ring containing a hetero-atom other than sulfur atom, for example, an oxygen atom, there can be mentioned similar derivatives.
When ##STR86## is a five- to eight-membered ring compound containing double bond(s), there are preferably selected five- or six-membered ring compounds. At that time, the number of double bonds is not restricted but is preferably 1 or 2.
Particularly preferable examples are shown below.
When ##STR87## is a five-membered ring containing a double bond, there can be mentioned the following examples. ##STR88##
When ##STR89## is a six-membered ring containing double bond(s), there can be mentioned the following examples. ##STR90##
Examples of the optically active cyclic secondary alcohol III were shown above, but the alcohol III is not restricted to these examples.
As specific examples of the optically active cyclic carboxylic acid V wherein the ##STR91## ring contains a hetero-atom or double bond(s), there can be mentioned the following compounds. However, the carboxylic acid V is not restricted to these examples.
When ##STR92## is a five-membered ring containing a hetero-atom, for example, a sulfur atom and Q 3 is an ether group (--O--), there can be mentioned the following compounds. ##STR93##
Specific examples of this compound include straight chain alkyloxy derivatives such as 4-methoxytetrahydrothiophene-3-carboxylic acid, 4-ethoxytetrahydrothiophene-3-carboxylic acid, 4-propoxytetrahydrothiophene-3-carboxylic acid, 4-butoxytetrahydrothiophene-3-carboxylic acid, 4-pentyloxytetrahydrothiophene-3-carboxylic acid, 4-hexyloxytetrahydrothiophene-3-carboxylic acid, 4-heptyloxytetrahydrothiophene-3-carboxylic acid, 4-octyloxytetrahydrothiophene-3-carboxylic acid, 4-nonyloxytetrahydrothiophene-3-carboxylic acid, 4-decyloxytetrahydrothiophene-3-carboxylic acid and the like, as well as branched chain alkyloxy derivatives such as 4-isopropoxytetrahydrothiophene-3-carboxylic acid, 4-isobutoxytetrahydrothiophene-3-carboxylic acid, 4-tert-butoxytetrahydrothiophene-3-carboxylic acid, 4-(2-methylpentyloxy)tetrahydrothiophene-3-carboxylic acid, 4-(3-methylpentyloxy)tetrahydrothiophene-3-carboxylic acid and the like. ##STR94##
Specific examples of this compound include straight chain alkyloxy derivatives such as 3-methoxytetrahydrothiophene-2-carboxylic acid, 3-ethoxytetrahydrothiophene-2-carboxylic acid, 3-propoxytetrahydrothiophene-2-carboxylic acid, 3-butoxytetrahydrothiophene-2-carboxylic acid, 3-pentyloxytetrahydrothiophene-2-carboxylic acid, 3-hexyloxytetrahydrothiophene-2-carboxylic acid, 3-heptyloxytetrahydrothiophene-2-carboxylic acid, 3-octyloxytetrahydrothiophene-2-carboxylic acid, 3-nonyltetrahydrothiophene-2-carboxylic acid, 3-decyloxytetrahydrothiophene-2-carboxylic acid and the like, as well as branched chain alkyloxy derivatives such as 3-isopropoxytetrahydrothiophene-2-carboxylic acid, 3-isobutoxytetrahydrothiophene-2-carboxylic acid, 3-tert-butoxytetrahydrothiophene-2-carboxylic acid, 2-(2-methylpentyloxy)tetrahydrothiophene-2-carboxylic acid, 3-(3-methylpentyloxy)tetrahydrothiophene-2-carboxylic acid and the like.
When ##STR95## is a five-membered ring containing a sulfur atom and Q 3 is a ##STR96## ester group, there can be mentioned the following compound. ##STR97##
Specific examples of this compound include straight chain alkyloxycarbonyl derivatives such as 4-methoxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-ethoxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-propoxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-butoxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-pentyloxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-hexyloxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-heptyloxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-octyloxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-nonyloxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-decyloxycarbonyltetrahydrothiophene-3-carboxylic acid and the like, as well as branched chain alkyloxycarbonyl derivatives such as 4-isopropoxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-isobutoxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-tert-butoxycarbonyltetrahydrothiophene-3-carboxylic acid, 4-(2-methylpentyloxy)carbonyltetrahydrothiophene-3-carboxylic acid, 4-(3-methylpentyloxy)carbonyltetrahydrothiophene-3-carboxylic acid and the like.
When ##STR98## is a five-membered ring containing a sulfur atom and Q 3 is a ##STR99## ester group, there can also be mentioned the following compounds. ##STR100##
When ##STR101## is a five-membered ring containing a sulfur atom and Q 3 is a ##STR102## ester group, there can be mentioned the following compound. ##STR103##
Specific examples of this compound include straight chain acyloxy derivatives such as 4-acetyloxytetrahydrothiophene-3-carboxylic acid, 4-propionyloxytetrahydrothiophene-3-carboxylic acid, 4-butyryloxy-tetrahydrothiophene-3-carboxylic acid, 4-valeryloxytetrahydrothiophene-3-carboxylic acid, 4-heptanoyloxytetrahydrothiophene-3-carboxylic acid, 4-octanoyloxytetrahydrothiophene-3-carboxylic acid, 4-nonanoyloxytetrathiophene-3-carboxylic acid, 4-decanoyloxytetrahydrothiophene-3-carboxylic acid and the like, as well as branched chain acyloxy derivatives such as 4-isobutyryloxytetrahydrothiophene-3-carboxylic acid, 4-isovaleryloxytetrahydrothiophene-3-carboxylic acid, 4-pivaloyloxytetrahydrothiophene-3-carboxylic acid, 4-(2-methylpentanoyloxy)tetrahydrothiophene-3-carboxylic acid, 4-(3-methylpentanoyloxy)tetrahydrothiophene-3-carboxylic acid and the like.
When ##STR104## is a five-membered ring containing a sulfur atom and Q 3 is a ##STR105## ester group, there can also be mentioned the following compound. ##STR106##
Specific examples of this compound include straight chain acyloxy derivatives such as 3-acetyloxytetrahydrothiophene-2-carboxylic acid, 3-propionyloxytetrahydrothiophene-2-carboxylic acid, 3-butyryloxytetrahydrothiophene-2-carboxylic acid, 3-valeryloxytetrahydrothiophene-2-carboxylic acid, 3-heptanoyloxytetrahydrothiophene-2-carboxylic acid, 3-octanoyloxytetrahydrothiophene-2-carboxylic acid, 3-nonanoyloxytetrahydrothiophene-2-carboxylic acid, 3-decanoyloxytetrahydrothiophene-2-carboxylic acid and the like, as well as branched carbon acyloxy derivatives such as 3-isobutyryloxytetrahydrothiophene-2-carboxylic acid, 3-isovaleryloxytetrahydrothiophene-2-carboxylic acid, 3-pivaloyloxytetrahydrothiophene-2-carboxylic acid, 3-(2-methylpentanoyloxy)tetrahydrothiophene-2-carboxylic acid, 3-(3-methylpentanoyloxy)tetrahydrothiophene-2-carboxylic acid and the like.
Specific examples of the optical active cyclic carboxylic acid V were shown above, but the carboxylic acid V is not restricted to these examples. For example, when ##STR107## is a five-membered ring containing a sulfur atom of high oxidation degree, i.e. a sulfoxide or a sulfone, there can be mentioned the following examples. ##STR108##
Also when ##STR109## is a six-membered ring containing a sulfur atom, there can be mentioned similar derivatives.
Also when ##STR110## is a five- or six-membered ring containing a hetero-atom other than a sulfur atom, for example, an oxygen atom, there can be mentioned similar derivatives.
When ##STR111## is a five-membered ring containing double bond(s), there can be mentioned the following compounds. ##STR112##
When ##STR113## is a six-membered ring containing double bond(s), there can be mentioned the following compounds. ##STR114##
Examples of the optically active cyclic carboxylic acid V were shown above, but the carboxylic acid V is not restricted to these examples.
The above-mentioned optically active cyclic compounds include novel compounds represented by the following formula; ##STR115## [In the above formula, R 2 represents an alkyl group of 1 to 10 carbon atoms, an alkenyl group of 2 to 10 carbon atoms or an alkynyl group of 2 to 10 carbon atoms, Q 3 represents a single bond, a (thio)ether group, a carbonyl group or a methylenoxy group, and Z represents a hydroxyl group or --COOZ' wherein Z' represents a hydrogen or an alkyl group of 2 to 10 carbon atoms, and ##STR116## represents a five- to eight-membered ring which may contain hetero-atom(s) or double bond(s).]
These compounds are prepared by the following known method; ##STR117##
The compound a, which is a known compound, is subjected to asymmetric reduction according to the known method using baker's yeast (B. S. Doel et al., Aust. J. Chem., 29, 2459 (1976)); the resulting compound b is subjected to alkylation to obtain the compound c, and then to acidic hydrolysis to obtain the compound . The other compounds are prepared by conventional procedures.
The compounds c, d, e, i, m, o and p are novel and useful for an intermediate of the liquid crystal compound.
Furthermore, the optically active cyclic compounds are prepared by the following methods such as enzymatic hydrolysis of the prochiral cyclic 1,2-diester [M. Schneider et al., Angew. Chem. Internat. Ed. Engl., 23, 67 (1984)] and the like. ##STR118##
The compound a, which is a known compound, is subjected to asymmetric reduction. The followed compounds are prepared by conventional procedures.
The compounds t, u, x, y, i and ii are novel and useful for an intermediate of the liquid crystal compound.
By a similar manner as above, the optically active cyclic compounds are prepared from the prochiral substance as shown in the following methods [K. Sakai et al., Chem. Commun., 838 (1987), and 966 (1988)]; ##STR119##
The compound iii, which is a known compound, is subjected to asymmetric reduction. The followed compounds are prepared by conventional procedures.
The compounds iv and viii are novel and useful for an intermediate of the liquid crystal compound.
Specific examples of the optically active dichiral cyclic secondary alcohol III and the optically active cyclic dichiral carboxylic acid V were shown above. Similar cyclic derivatives can be used, also when Q 3 is a single bond, a thioether group, a carbonyl group, a carbonyldioxy group or a methyleneoxy group, Therefore, the secondary alcohol III and the carboxylic acid V are not restricted to these examples.
Next, there are specifically described typical examples of the carboxylic acid II and the alcohol or phenolic hydroxyl group-containing compound IV which are both important materials for the skeletal portion of the optically active compounds of the present invention.
The carboxylic acid II can be classified into two type compounds represented by the following general formulas. ##STR120##
As typical examples of these compounds, there can be mentioned 4-(4'-alkyloxy or alkyl-4-biphenylcarbonyloxy)benzoic acid, 4-(4'-alkyloxy or alkyl-4-biphenyloxycarbonyl)benzoic acid, 4'-(4-alkyloxy or alkylphenylcarbonyloxy)-4-biphenylcarboxylic acids, 4'-(4-alkyloxy or alkylphenyloxycarbonyl)-4-biphenylcarboxylic acids, 4-alkyloxy or alkyl-4-biphenylcarboxylic acids, 4"-alkyloxy(or alkyl)-4-terphenylcarboxylic acids, 4'-(trans-4-alkyloxy or alkylcyclohexylcarbonyloxy)-4-biphenylcarboxylic acids, trans-4-(4'-alkyloxy or alkyl-4-biphenylcarbonyloxy)cyclohexanecarboxylic acids, 2-[4-(4-alkyloxy or alkylphenylcarbonyloxy)phenyl]pyridimidinyl-5-carboxylic acids, 2-(4'-alkyloxy or alkyl-4-biphenyl)pyrimidinyl-5-carboxylic acids, 4'-(5-alkyloxy or alkylpyrimidinyl-2-oxycarbonyl)biphenyl-4-carboxylic acids, 4'-[2-(5-alkyloxy or alkyl)-2-(pyridyl)ethyl]biphenyl-4-carboxylic acids, 4-[4-(trans-5-alkyloxy or alkyl-1,3-dioxane-2-yl)phenylcarbonyloxy]benzoic acids, 4'-[4-(trans-5-alkyloxy or alkyl-1,3-dioxane-2-yl)]biphenyl-4-carboxylic acids, 2-[4-(4-alkyloxy or alkylphenylcarbonyloxy)phenyl]pyrazinyl-5-carboxylic acids, 2-(4'-alkyloxy or alkyl-4-biphenyl)pyrazinyl-5-carboxylic acids, 4'-(5-alkyloxy or alkylpyrazinyl-2-oxycarbonyl)-biphenyl-4-carboxylic acids and 4'-(6-alkyloxy or alkyl-3-pyridazinyl)biphenyl-4-carboxylic acids.
The alcohol IV or the compound having a phenolic hydroxy group can be classified into two type compounds represented by the following general formulas. ##STR121##
As typical examples of these compounds, there can be mentioned 4-hydroxyphenyl esters of, 4'-alkyloxy or alkylbiphenyl-4-carboxylic acids, 4'-alkyloxy or alkyl-4-biphenyl esters of 4-hydroxybenzoic acids, 4'-hydroxy-4-biphenyl esters of 4-alkyloxy or alkylbenzoic acids, 4-alkyloxy or alkylphenyl esters of 4'-hydroxybiphenyl-4-carboxylic acids, 4'-hydroxy-4-biphenyl esters of trans-4-alkyloxy or alkylcyclohexanecarboxylic acids, trans-4-hydroxycyclohexyl esters of 4'-alkyloxy or alkyl-4-biphenylcarboxylic acids, 4-(5-hydroxy-2-pyrimidinyl)phenyl esters of 4-alkyloxy or alkylbenzoic acids, 2-(4'-alkyloxy or alkyl-4-biphenyl)pyrimidine-5-ols, 5-alkyloxy or alkyl-2-pyridinyl esters of 4'-hydroxy-4-biphenylcarboxylic acids, 4'-[2-(5-alkyloxy or alkyl-2-pyridyl)ethyl]biphenyl-4-ols, 4-hydroxyphenyl esters of 4-[4-(trans-5-alkyloxy or alkyl)-1,3-dioxane-2-yl]benzoic acids and 5-alkyloxy or 5 alkyl 2-pyrazinyl esters of 4'-hydroxy-4-biphenylcarboxylic acids.
The optically active compounds I of the present invention have a structure in which each asymmetric carbon atom bonds to oxygen or carbonyl, and therefore the compounds generally show high spontaneous polarization. In addition, most of the compounds I show a chiral smectic C (Sc*) phase which is a liquid crystal phase suitable for display methods utilizing the ferroelectric properties of liquid crystals, and the temperature range of the chiral smectic C phase is low and wide.
The optically active compounds of the present invention are very stable to heat, light, water and air. Accordingly, in putting the compounds to practical use as or in liquid crystal materials, there can be eliminated inconveniences such as arrangements of an apparatus for prevention of overheating, a glass frit seal for prevention of moisture absorption or permeation, etc.
The optically active compounds I of the present invention have excellent compatibility with conventionally known liquid crystal compounds such as those of Schiff's base type, biphenyl type, phenylcyclohexane type, heterocyclic type and the like. Therefore, the compounds can be made into liquid crystal compositions having excellent properties, by incorporating them into said liquid crystal compounds.
As the liquid crystal compounds into which the optically active compounds I of the present invention can be incorporated, there can be mentioned, for example, ferroelectric liquid crystal compounds as well as liquid crystal compounds showing a smectic C phase. The ferroelectric liquid crystal compounds include, for example, biphenyl type liquid crystals described in JP-A-118744/1984 and 13729/1985, ester type liquid crystals described in JP-A-128357/1984, 51147/1985, 22051/1986 and 249953/1986, and pyrimidine type liquid crsytals described in JP-A-260564/1985, 24756/1986, 85368/1986 and 215373/1986. The liquid crystal compounds showing a smectic C phase include, for example, ester type liquid crystal compounds described in JP-A-228036/1987, and cyclohexane type liquid crystals and heterocyclic type liquid crystals described in the materials of the 16th Freiburg Liquid Crystal Form (Mar. 21, 1986) and the materials of the First International Symposium on Ferroelectric Liquid Crystals (Sep. 21, 1987).
The optically active compounds of the present invention can also be incorporated into the nematic or cholesteric liquid crystals described in "Flussige Kristalle in Tabellen" I & II, VEB-Verlag, Leipzig, and further can be mixed with commercially available nematic liquid crystal compounds. When the optically active compounds of the present invention are incorporated into nematic liquid crystals, the twisting direction of the cholesteric pitch and the pitch length of the nematic liquid crystal compositions obtained can be freely controlled via the amount added.
When the optically active compound of the present invention is mixed with other liquid crystals as mentioned above, the mixing ratio can be selected depending upon the application purpose of the resulting liquid crystal composition. For example, when it is desired to prepare a ferroelectric liquid crystal composition, the optically active composition of the present invention can be used in an amount of 5-50% by weight based on the total weight of the composition; when a smectic liquid crystal composition is prepared, the compound of the present invention can be used in an amount of 0.1-5% by weight. It is also possible to formulate a liquid crystal composition using only the optically active compounds of the present invention.
As liquid crystal optical modulators, there can be mentioned various display apparatuses using a plurality of liquid crystal devices, for example, display apparatuses used in word processor, lap top type personal computer, work station, etc., image display apparatuses used in TV set, video telephone, etc. and terminal display panels of optical communication apparatuses.
Various types of liquid crystal display devices are known. The liquid crystal compositions of the present invention can be used in any liquid crystal display device as long as the compositions can exhibit the capabilities. The liquid crystal compositions of the present invention can be effectively used in, for example, the liquid crystal devices disclosed in U.S. Pat. No. 4,367,924, JP-B-63-22287, U.S. Pat. No. 4,563,059, etc.
Generally, these liquid crystal devices are basically constituted by a pair of substrates, two polarizing plates provided on the substrates, a pair of transparent electrodes, a pair of molecule polarizing layers, a liquid crystal composition sealed between the substrates by a sealing agent, and a reflecting plate.
The present invention is described more specifically by way of Examples and Application Examples.
The optically active compounds prepared in Examples were measured for phase, phase transition temperature and spontaneous polarization. The results are listed in Table 1 together with the elemental analysis.
Incidentally, phase and phase transition temperature were measured using a polarizing microscope and a differential scanning calorimeter (DSC).
Spontaneous polarization was measured by the Sowyer-Tower method. The values of spontaneous polarization were obtained at a temperature lower by 10° C. than the upper limit temperature of chiral smectic C phase.
The phases such as liquid crystal phase are shown by the following abbreviations.
______________________________________Iso: isotropic phase Ch: cholesteric phaseSA: smectic A phase K: crystalline phaseSc*: chiral smectic C phaseS.sub.1, S.sub.2 : smectic phases which are difficult to______________________________________identify
EXAMPLE 1
Preparation of 4'-octyloxy-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclopentane-1-carboxylic acid (a compound of the general formula I" wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 and Q 3 are both --O--, Q 2 is ##STR122## X is a single bond, and ##STR123## i) Preparation of cis-(1R,2S)-2-methoxycyclopentane-1-carboxylic acid
This optically active cyclic dichiral carboxylic acid can be prepared according to the following scheme. ##STR124## That is, ethyl 2-oxocyclopentane-1-carboxylate was subjected to asymmetric reduction according to the known method using baker's yeast [B. S. Doel et al., Aust. J. Chem., 29, 2459 (1976)]; the resulting ethyl cis-(1R,2S)-2-hydroxycyclopentane-1-carboxylate was subjected to methylation and then to acidic hydrolysis to obtain the title compound as a colorless oil. The IR and 1 H-NMR spectra of the compound are shown below.
IR ν max neat cm -1 : 2700-2400, 1710 1 H-NMR (90 MHz, CDCl 3 ) δ: 1.4-2.25(6H, m, CH 2 ), 2.6-3.05(1H, m,>CHCOO), 3.35(3H, s, OCH 3 ), 3.85-4.15(1H, m, >CHOCH 3 ), 7.7-8.6(1H, broad s, CO 2 H)
The 1 H-NMR spectra of the ethyl ester of the title compound (as a colorless oil) are shown below.
1 H-NMR (90 MHz, CDCl 3 ) δ: 1.26(3H, t, J=7.5 Hz, OCH 2 CH 3 ), 1.3-2.3(6H, m, CH 2 ), 2.6-3.1(1H, m, >CHCO 2 Et), 3.28(3H, s OCH 3 ), 3.8-4.4(3H, m, >CH--OCH 3 and CO 2 CH 2 CH 3 )
ii) Esterification
472.5 mg of the cis-(1R,2S)-2-methoxycyclopentane-1-carboxylic acid obtained in i) above was reacted with oxalyl chloride to obtain 382.5 mg of an acid chloride (IR ν max neat cm -1 : 1800). A solution of this acid chloride dissolved in 5.0 ml of dry toluene was added, with stirring, to a solution of 0.68 g of 4'-octyloxy-4-biphenol and 0.6 ml of pyridine dissolved in 10 ml of dry tetrahydrofuran. The mixture was stirred for 4 days at room temperature. The reaction mixture was concentrated under reduced pressure, and the residue was mixed with benzene. The insoluble materials were removed by filtration and the filtrate was concentrated under reduced pressure. The residue was subjected to column chromatography using silica gel (150 g) and carbon tetrachloride-ether (10:1). 0.44 g of the title compound was obtained from the relevant fraction as waxy crystals. The IR and 1 H-NMR spectra of the compound are shown below.
IR ν max neat cm -1 : 1755, 150, 1245, 1210, 1165 1 H-NMR (90 MHz, CDCl 3 ) δ: 0.89(3H, t, J=6 Hz, --CH 2 CH 3 ), 1.0-2.5(18H, m, CH 2 ), 2.9-3.4 (1H, m, >CH-COO), 3.39(3H, s, OCH 3 ), 3.99(2H, t, J=6 Hz, OCH 2 ), 3.9-4.25(1H, m, >CH--OCH 3 ), 6.75-7.6(8H, m, aromatic H)
EXAMPLE 2
Preparation of 4-(4'-octyloxy-4-biphenyloxycarbonyl)phenyl ester of cis-(1R,2S)-2-methoxycyclopentane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 and Q 3 are both --O--, Q 2 is ##STR125## X is a single bond, Y is ##STR126##
Using 382.5 mg of cis-(1R,2S)-2-methoxycyclopentane-1-carboxylic acid chloride and 0.95 g of 4-(4'-octyloxy-4-biphenyloxycarbonyl)phenol and in the same procedure as in Example 1, there was obtained 0.65 g of the title compound as colorless powder (recrystallized from ethanol).
EXAMPLE 3
Preparation of 4'-(4-octyloxyphenyloxycarbonyl)-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclopentane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 and Q 3 are both --O--, Q 2 is ##STR127## X is ##STR128## Y is a single bond, and all of ##STR129##
Using 382.5 mg of cis-(1R,2S)-2-methoxycyclopentane-1-carboxylic acid chloride and 0.95 g of 4-octyloxyphenyl 4'-hydroxy-4-biphenylcarboxylate and in the same procedure as in Example 1, there was obtained 0.51 g of the title compound as colorless needles (recrystallized from ethanol).
EXAMPLE 4
Preparation of 4'-(4-octyloxyphenylcarbonyloxy)-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclopentane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 and Q 3 are both --O--, Q 2 is ##STR130## X is ##STR131## Y is a single bond and all of ##STR132##
Using 382.5 mg of cis-(1R, 2S)-2-methoxycyclopentane-1-carboxylic acid chloride and 0.95 g of 4'-(4-octyphenylcarbonyloxy)-4-biphenol and in the same procedure as in Example 1, there was obtained 0.39 g of the title compound as colorless needles (recrystallized from ethyl acetate-ethanol).
EXAMPLE 5
Preparation of 4'-(4-n-octyloxyphenyloxycarbonyl)-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 and Q 3 are both --O-- Q 2 is ##STR133## X is ##STR134## Y is a single bond, and all of ##STR135## i) Preparation of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid
This optically active cyclic dichiral carboxylic acid can be prepared according to the following scheme. ##STR136## That is, ethyl 2-oxocyclohexane-1-carboxylate was subjected to asymmetric reduction according to the known method using baker's yeast [B. S. Doel et al., Aust. J. Chem., 29, 2459 (1979)], and the resulting ethyl cis-(1R,2S)-2-hydroxycyclohexane-1-carboxylate was subjected to methylation and then to acidic hydrolysis to obtain the title compound. The NMR spectra of the ethyl ester of the title compound which is a colorless oil are shown below.
1 H-NMR (90 MHz, CDCl 3 ) δ: 0.8-2.2(8H, m, CH 2 ), 1.25(3H, t, J=7 Hz, CO 2 CH 2 CH 3 ), 2.2-2.55 (1H, m, >CHCO 2 Et), 3.29(3H, s, OCH 3 ), 3.55-3.9(1H, m, >CHOCH 3 ), 3.9-4.35(2H, m CO 2 CH 2 CH 3 )
ii) Esterification
4.0 g of the cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid obtained in i) above was reacted with oxalyl chloride to obtain 2.2 g of an acid chloride (IR ν max neat cm -1 : 1800 1 H-NMR (90 MHz, CDCl 3 ) δ: 0.85-2.55(8H, m, CH 2 ), 2.6-3.05 ##STR137## 3.34(3H, s, OCH 3 ), 3.8-4.3(1H, m, >CH--OCH 3 )). 0.5 g of this acid chloride was added, with stirring, to a solution of 1.05 g of 4-octyloxyphenyl 4-hydroxy-4-biphenylcarboxylate and 0.6 g of pyridine dissolved in 10 ml of dry tetrahydrofuran. The mixture was subjected to a reaction overnight. The reaction mixture was concentrated under reduced pressure. The residue was subjected to separation and purification by column chromatography using silica gel and carbon tetrachloride-ether (30:1) and then recrystallized from ethanol to obtain 0.3 g of the title compound. The IR and 1 H-NMR spectra of the compound are shown below.
IR ν max neat cm -1 : 2800-3000, 1740, 1605 1 H-NMR (90 MHz, CDCl 3 ) δ: 0.89(3H, t) 1.1-2.0 (20H, m), 2.6-2.9(1H, m), 3.40(3H, s), 3.9-4.1 (3H, m), 6.8-8.3(12H, m)
EXAMPLE 6
Preparation of 4-(4'-n-octyloxy-4-biphenyloxycarbonyl)phenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 and Q 3 are both --O--, Q 2 is ##STR138## X is a single bond, Y ##STR139##
Using 0.50 g of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid chloride and 1.05 g of 4-(4'-octyloxy-4-biphenyloxycarbonyl)phenol and in the same procedure as in Example 5; there was obtained 0.38 g of the title compound (recrystallized from ethanol).
EXAMPLE 7
Preparation of 4'-octyloxy-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (a compound of the general formula I" wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 Q 3 are both --O--, Q 2 is ##STR140## X is a single bond, and all of ##STR141##
Using 0.7 g of cis(1R,2S)-2-methoxycyclohexane-1-carboxylic acid chloride and 1.05 g of 4'-octyloxy-4-biphenol and in the same procedure as in Example 5, there was obtained 0.62 g of the title compound.
EXAMPLE 8
Preparation of 4'-(4-octyloxyphenylcarbonyloxy)-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 and Q 3 are both --O--, Q 2 is ##STR142## X is ##STR143## Y is a single bond and all of ##STR144##
Using 0.50 g of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid chloride and 1.05 g of 4'-hydroxy-4-biphenyl-4-octyloxybenzoate and in the same procedure as in Example 5, there was obtained 0.77 g of the title compound.
EXAMPLE 9
i) Preparation of trans-(1S,2S)-2-methoxycyclopentane-1-carboxylic acid
The ethyl cis-(1R,2S)-2-hydroxycyclopentane-1-carboxylate prepared in Example 1 i) was subjected to inversion of configuration at the 1-position in ethanol in the presence of a base (K 2 CO 3 ) to convert to ethyl trans-(1S,2S)-2-hydroxycyclopentane-l-carboxylate. This ester was subjected to methyl etherification and then to acidic hydrolysis to obtain the title compound. ##STR145## ii) Esterification
The same procedure as in Example 1 ii) was repeated except that trans-(1S,2S)-2-methoxycyclopentane-1-carboxylic acid chloride was used in place of cis-(1R,2S)-2-methoxycyclopentane-1-carboxylic acid chloride and subjected to a condensation reaction with 4-octyloxyphenyl 4'-hydroxy-4-biphenylcarboxylate, whereby the title compound was obtained.
EXAMPLES 10 and 11
The trans-(1S,2S)-2-methoxycyclopentane-1-carboxylic acid obtained in Example 9 i) was converted to a corresponding acid chloride according to an ordinary method, and the acid chloride was subjected to a condensation reaction with a corresponding compound containing a phenolic hydroxyl group, to obtain compounds of Examples 10 and 11, respectively.
EXAMPLE 12
Preparation of 4-(4-octyloxyphenyloxycarbonyl)phenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (a compound of the general formula I" wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 and Q 3 are both --O--, Q 2 is ##STR146## X is ##STR147## and all of ##STR148##
Using 0.68 g of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid chloride and 1.03 g of 4-(4-octyloxyphenyloxycarbonyl)phenol and in the same procedure as in Example 5, there was obtained 1.30 g of the title compound.
EXAMPLE 13
Preparation of 4'-octyloxycarbonyl-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (a compound of the general formula I wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 and Q2 are both ##STR149## Q 3 is --O--, ##STR150## X is a single bond and all of ##STR151##
Using 0.80 g of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid chloride and 1.14 g of 4'-octyloxycarbonyl-4-biphenol and in the same procedure as in Example 5, there was obtained 0.80 g of the title compound.
EXAMPLE 14
Preparation of 4'-(4-octylphenoxycarbonyl)-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (compound of the general formula I' wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 is a single bond, Q 2 is ##STR152## Q 3 is --O--, ##STR153## X is ##STR154## Y is a single bond, and all of ##STR155##
Using 0.57 g of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid chloride and 1.00 g of 4'-(4-n-octylphenyloxycarbonyl)-4-biphenol and in the same procedure as in Example 5, there was obtained 1.04 g of the title compound.
EXAMPLE 15
Preparation of 4-(4'-octyloxy-4-biphenylcarbonyloxy)phenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 and Q 3 are --O--, Q 2 is ##STR156## X is a single bond, Y is ##STR157## and all of ##STR158##
Using 0.57 g of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid chloride and 1.05 g of 4-(4'-octyloxy-4-biphenylcarbonyloxy)phenol and in the same procedure as in Example 5, there was obtained 1.05 g of the title compound.
EXAMPLE 16
Preparation of 4'-(4-n-propyloxyphenyloxycarbonyl)-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 3 H 7 , R 2 is CH 3 , Q 1 and Q 3 are both --O--, Q 2 is ##STR159## X is ##STR160## Y is single bond, and all of ##STR161##
Using 0.69 g of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid chloride and 1.05 of 4'-(4-n-propyloxyphenyloxycarbonyl)-4-biphenol and in the same procedure as in Example 5, there was obtained 1.05 g of the title compound.
EXAMPLE 17
Preparation of 4'-decyloxy-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (a compound of the general formula I" wherein R 1 is n-C 10 H 21 , R 2 is CH 3 , Q 1 and Q 3 are both --O--, Q 2 is ##STR162## X is a single bond, all of ##STR163##
using 0.69 g of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid chloride and 0.98 g of 4'-decyloxy-4-biphenol and in the same procedure as in Example 5, there was obtained 0.72 g of the title compound.
EXAMPLE 18
Preparation of 4'-dodecyloxy-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 12 H 25 , R 2 is CH 3 , Q 1 and Q 3 are both --O--, Q 2 is ##STR164## X is a single bond, and all of ##STR165##
Using 0.69 g of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid chloride and 1.06 g of 4'-dodecyloxy-4-biphenol and in the same procedure as in Example 5, there was obtained 0.4 g of the title compound.
EXAMPLE 19
Preparation of 4'(4-octyloxybenzyloxy)-4-biphenyl ester of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 8 H 17 , R 2 is CH 3 , Q 1 and Q 3 are both --O--, Q 2 is ##STR166## X is --CH 2 --O--, Y is a single bond, and all of ##STR167##
Using 0.57 g of cis-(1R,2S)-2-methoxycyclohexane-1-carboxylic acid chloride and 1.01 g of 4'-(4-octyloxybenzyloxy)-4-biphenol and in the same procedure as in Example 5, there was obtained 0.32 g of the title compound.
EXAMPLE 20
Preparation of 4'-(4-n-octyloxyphenylcarbonyloxy)-4-biphenyl ester of cis-(1R,2S)-2-butoxycyclopentane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 8 H 17 , R 2 is-Bu(n), Q 1 and Q 3 are both --O--, Q 2 is ##STR168## X is ##STR169## Y is a single bond, and all of ##STR170## 1) Preparation of cis-(1R,2S)-2-butoxycyclopentane-1-carboxylic acid
This optically active cyclic dichiral carboxylic acid can be prepared according to the following scheme. ##STR171##
The ethyl cis-(1R,2S)-2-hydroxycyclopentane-1-carboxylate obtained in Example 1 i) was subjected to butylation and then to acidic hydrolysis to obtain the title compound. The NMR spectra of the ethyl ester of the title compound are shown below:
1 H-NMR (90 MHz, CDCl 3 ) δ: 0.7-1.05(3H, m, CH 3 ), 1.05-2.5(10H, m, CH 2 ), 1.26(3H, t, J=7.15 Hz, OCH 2 CH 3 ), 2.6-3.0(1H, m, CHCO 2 Et), 3.1-3.6 (2H, m, OCH 2 CH 2 --), 3.85-4.3(1H, m, >CHOBu), 4.14 ##STR172## ii) Esterification
1.0 g of the cis-(1R,2S)-2-butoxycyclopentane-1-carboxylic acid obtained in i) above was reacted with oxalyl chloride to obtain 0.70 g of an acid chloride (IR ν max neat cm -1 : 1800). 0.35 g of this acid chloride was added, with stirring at room temperature, to a solution of 0.71 g of 4'-(4-n-octyloxyphenylcarbonyloxy)-4-biphenyl ester and 0.4 g of pyridine dissolved in 10 ml of dry tetrahydrofuran. The mixture was subjected to a reaction overnight. The reaction mixture was concentrated under reduced pressure. The residue was subjected to separation and purification by column chromatography using carbon tetrachloride-ether (30:1) and silica gel and then recrystallized from ethanol to obtain 0.63 g of the title compound.
EXAMPLE 21
Preparation of 4-(4'-octyloxy-4-biphenyloxycarbonylphenyl ester of cis-(1R,2S)-2-butoxycyclopentane-1-carboxylic acid (a compound of the general formula I' wherein R 1 is n-C 8 H 17 , R 2 is Bu(n), Q 1 and Q 3 are both --O--, Q 2 is ##STR173## X is a single bond, Y is ##STR174## and all of ##STR175##
Using 0.35 g of cis-(1R,2S)-2-butoxycyclopentane-1-carboxylic acid chloride and 0.71 g of 4-(4'-octyloxy-4-biphenyloxycarbonyl)phenol and in the same procedure as in Example 1, there was obtained 0.78 g of the title compound.
EXAMPLE 22
i) Cis-(1R,2S)-2-methoxy-1-methylcyclopentanecarboxylic acid
The ethyl cis-(1R,2S)-2-hydroxycyclopentanecarboxylate prepared in Example 1 i) was subjected to methylation, methyl etherification and hydrolysis in this order according to the method by Fra'ter et al. [Tetrahedron, 40, 1269 (1984)] and the method by Mori and Ebara [Tetrahedron, 42, 4413 (1986)] to obtain the title compound as a colorless oil (the following scheme). ##STR176##
The IR spectrum of the compound is shown below.
IR ν max neat cm -1 : 1700-2300, 1700
ii) Esterification
The compound of Example 22 shown in Table 1 was obtained in the same procedure as in Example 1 ii).
EXAMPLE 23-25
The compounds of Examples 23-25 shown in Table 1 were obtained by subjecting the cis-(1R,2S)-2-methoxy-1-methylcyclopentanecarboxylic acid obtained in Example 22 i), to a condensation reaction with an appropriate skeletal compound in accordance with the above methods, for example, the method of Example 1 ii).
EXAMPLE 26
Preparation of 4'-octyloxy-4-biphenyl ester of 4-[trans-(1R,2S)-2-methoxymethyl-1-cyclopentyloxy]benzoic acid
i) Preparation of cis-(1S,2S)-2-methoxymethylcyclopentanol
This optically active cyclic dichiral alcohol can be prepared according to the following scheme. ##STR177##
That is, the ethyl cis-(1R,2S)-2-hydroxycyclopentanecarboxylate obtained in Example 1 was subjected to tetrahydropyranylation, reduction by lithium aluminum hydride, methylation and detetrahydropyranylation by ion exchange resin in this order, to obtain the title compound. The IR and 1 H-NMR spectra of the compound are shown below.
IR ν max neat cm -1 : 3200-3700, 2800-3000, 1740 1 H-NMR (90 MHz, CDCl 3 ) δ: 1.4-1.9 (6H, m), 2.3-2.5(1H, broad), 3.36(s, 3H), 3.52(1H, s), 3.6(1H, s), 4.2-4.4(m, 2H)
ii) Etherification
0.49 g of the optically active alcohol obtained in i) above, 1.05 g of 4'-octyloxy-4-biphenyl 4-hydroxybenzoate and 0.98 g of triphenylphosphine were dissolved in 10 ml of dry tetrahydrofuran. To the solution was added 0.65 g of diethyl azodicarboxylate with stirring at room temperature. The reaction mixture was stirred for 1 hour at room temperature. Then, the solvent was removed by distillation. The residue was subjected to column chromatograph using silica gel and carbon tetrachlorideether (30:1) to obtain 0.60 g of the title compound.
The IR and 1 H-NMR spectra are shown below.
IR ν max neat cm -1 : 800-3000, 1735, 1605 1 H-NMR (90 MHz, CDCl 3 ) δ: 0.9(t, 3H), 1.2-1.5(m, 12H), 1.6-2.0(m, 6H), 2.2-2.5 (m, 1H), 3.34(t, 5H), 4.0(d, 2H), 4.6-4.8 (m, 1H), 6.9-8.2(m, 12H)
EXAMPLE 27
Preparation of 4-[trans-(1R,2S)-2-methoxymethyl-1-cyclopentoxy]phenyl ester of 4'-octyloxy-4-biphenylcarboxylic acid
Using 0.49 g of cis-(1S,2S)-2-methoxymethylcyclopentanol and 1.05 g of 4-hydroxyphenyl 4'-octyloxy-4-biphenylcarboxylate and in the same procedure as in Example 26, there was obtained 0.70 g of the title compound.
EXAMPLE 28
Preparation of 4'-[trans-(1R,2S)-2-methoxymethyl-1-cyclopentyloxy]-4-biphenyl ester of 4-octyloxybenzoic acid
Using 0.49 g of cis(1S,2S)-2-methoxymethylcyclopentanol and 1.05 g of 4'-hydroxybiphenyl 4-octyloxybenzoate and in the same procedure as in Example 26, there was obtained 0.61 g of the title compound.
EXAMPLE 29
Preparation of 4-octyloxyphenyl ester of 4'-[trans(1R,2S)-2-methoxymethyl-1-cyclopentyloxy]-4-biphenylcarboxylic acid
Using 0.49 g of cis-(1S,2S)-2-methoxymethylcyclopentanol and 1.05 g of 4-octyloxyphenyl 4'-hydroxybiphenyl-4-carboxylate and in the same procedure as in Example 26, there was obtained 0.76 g of the title compound.
EXAMPLE 30
Preparation of trans (1R,2S)-2-methoxymethyl-1-cyclopentyl ester of 4'-octyloxy-4-biphenylcarboxylic acid
Using 0.59 g of cis-(1S,2S)-2-methoxymethyl-1-cyclopentanol and 4'-octyloxy-4-biphenylcarboxylic acid and in the same procedure as in Example 26, there was obtained 0.35 g of the title compound,
EXAMPLE 31
Preparation of 4'-octyloxy-4-biphenyl ether of trans-(1R,2S)-2-methoxymethyl-1-cyclopentanol
Using 0.68 g of cis(1S,2S)-2-methoxymethyl-1-cyclopentanol and 4'-octyloxy-4-biphenol and in the same procedure as in Example 26, there was obtained 0.78 g of the totel compound.
EXAMPLE 32
Preparation of cis-(1S,2S)-2-methoxymethyl-1-cyclopentyl ester of 4-(4'-octyloxy-4-biphenyloxycarbonyl)benzoic acid
i) Esterification
20 ml of thionyl chloride was added to 1.11 g of 4-(4'-octyloxy-4-biphenyloxycarbonyl)benzoic acid. The mixture was refluxed for 3 hours. The reaction mixture was concentration under reduced pressure. To the residue was added 20 ml of thionyl chloride, and the mixture was refluxed for 4 hours. The reaction mixture was concentrated under reduced pressure. To the residue was added toluene, and the mixture was subjected to azoetropic distillation to remove excessive thionyl chloride and toluene. To the residue was added 25 ml of dry tetrahydrofuran to dissolve the residue. To the resulting solution were added 0.39 g of cis(1S,2S)-2-methoxymethyl-1-cyclopentanol and 0.40 g of pyridine. The mixture was stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure. The residue was subjected to column chromatography using silica gel and carbon tetrachloride-ether (30:1) to obtain 0.10 g of the title compound.
EXAMPLE 33
The compound of this Example shown in Table 1 was obtained in the same manner as in Example 32.
EXAMPLES 34-45
The compounds of these Examples shown in Table 1 were obtained by subjecting cis-(1R,2S)-2-methoxycyclopentanecarboxylic acid chloride to a condensation reaction with an appropriate skeletal compound in the same procedure as in Example 1.
EXAMPLE 46
i) Preparation of cis-(1S,2S)-1-hydroxymethyl-2-methoxychclopentane
The compound described in Example 1 i), i.e. ethyl cis-(1R,2S)-2-hydroxycyclopentanecarboxylate was reduced with lithium aluminum hydride to obtain the title compound (the following reaction formula). ##STR178## ii) Condensation
The compound of Example 46 shown in Table 1 was obtained in the same procedure as in Example 26 ii).
EXAMPLE 47
Preparation of 4'-octyloxy-4-biphenyl ester of cis-(1R,2S)-2-methoxycarbonylchclohex-4-enecarboxylic acid
3 ml of oxalyl chloride was added, with ice cooling, to 0.25 g of the cis-(1R,2S)-2-methoxycarbonylcyclohex-4-enecarboxylic acid prepared according to the known method [M. Ohno et al., Tetrahedron Lett., 24, 2557 (1984)]. The mixture was stirred for 2 hours. Excessive oxalyl chloride was removed by distillation. To the remaining crude acid cloride were added 5 ml of dry tetrahydrofuran and 0.30 g of 4'-octyloxy-4-biphenol. To the mixture was dropwise added 0.11 g of triethylamine with ice cooling. The mixture was stirred for 1 hour. The reaction mixture was concentrated under reduced pressure. The residue was mixed with carbon tetrachloride. The resulting insoluble materials were removed by filtration. The filtrate was concentrated under reduced pressure. The residue was subjected to separation and purification by column chromatography using silica gel and carbon tetrachloride-ethyl acetate (20:1) and then to recrystallization from ethanol to obtain 0.3 g of the title compound as colorless plates. The IR and 1 H-NMR spectra of the compound are shown below.
IR ν max KBr cm -1 : 1760, 1730 1 H-NMR (90 MHz, CDCl 3 ) δ: 0.89(3H, t, --CH 2 CH 3 ) 1.12-2.00(12H, m, CH 2 ), 2.18-2.95(4H, m, CH 2 --C═C--CH 2 ), 3.10-3.42(2H, m, --OOC--CH--CH--COO---), 3.72(3H, s, OCH 3 ), 3.98(2H, t, J=6 Hz, OCH 2 ), 5.73(2H, m, CH═CH), 6.85-7.60(8H, m, aromatic H)
EXAMPLE 48
Preparation of 4'-(4-octyloxyphenyloxycarbonyl)-4-biphenyl ester of cis-(1R,2S)-2-methoxycarbonylcyclohex-4-enecarboxylic acid
Using 0.22 g of cis-(1R,2S)-2-methoxycarbonylcyclohex-4-enecarboxylic acid and 0.50 g of 4'-(4-octyloxyphenyloxycarbonyl)-4-biphenol and in the same procedure as in Example 47, there was obtained 0.42 g of the title compound.
EXAMPLE 49
Preparation of 4'-(4-octyloxyphenyloxycarbonyl)-4-biphenyl ester of cis(1R,2S)-2-methoxycarbonylcyclohexanecarboxylic acid
In 10 ml of chloroform was dissolved 0.20 g of the 4'-(4-octyloxyphenyloxycarbonyl)-4-biphenyl ester of cis-(1R,2S)-2-methoxycarbonylcyclohex-4-enecarboxylic acid, obtained in Example 48. Thereto was added 30 mg of 5% palladium carbon. The mixture was subjected to hydrogenation at room temperature at atmospheric pressure. After the completion of the reaction, the catalyst was removed by filtration. The filtrate was concentrated under reduced pressure. The residue was recrystallized from ethanol to obtain 0.18 g of the title compound. The IR and 1 H-NMR spectra of the compound are shown below.
IR ν max KBr cm -1 : 1760, 1725 1 H-NMR (90 MHz, CDCl 3 ) δ: 0.89(3H, t, --CH 2 CH 3 ), 1.15-2.47(20H, m, CH 2 ), 2.93-3.20(2H, m, OOC--CH--CH--COO--), 3.72(3H, s, OCH 3 ), 3.96(2H, t, J=6 Hz, OCH 2 ), 6.82-8.30(12H, m, aromatic H)
EXAMPLE 50
Preparation of 4'-octyloxy-4-biphenyl ester of cis-(1R,2S)-2-methoxycarbonylcyclohexanecarboxylic acid
0.18 g of the 4'-octyloxy-4-biphenyl ester of cis-(1R,2S)-2-methoxycarbonylcyclohex-4-enecarboxylic acid, obtained in Example 47 was subjected to the same procedure as in Example 49 to obtain 0.15 g of the title compound.
EXAMPLE 51
Preparation of cis-(3R,4S)-tetrahydro-3-methoxycarbonyl-4-thienyl ester of 4-(4'-octyloxy-4-biphenylcarbonyloxy)benzoic acid
i) Preparation of methyl cis-(3R,4S)-tetrahydro-4-trimethylsilyloxythiophene-3-carboxylate
This optically active cyclic dichiral compound can be prepared according to the following scheme. ##STR179##
Methyl tetrahydro-4-oxothiophene-3-carboxylate was subjected to asymmetric reduction using baker's yeast according to the known method [R. W. Hoffmann et al., Tetrahedron Lett, 23, 3479 (1982)], and the resulting methyl cis-(3R,4S)-tetrahydro-4-hydroxythiophene-3-carboxylate was subjected to trimethylsilylation by 1,1,1,3,3,3-hexamethyldisilazane according to a conventional method, to obtain the title compound. The IR and 1 H-NMR spectra of the compound are shown below.
IR ν max neat cm -1 : 1740 1 H-NMR (90 MHz, CDCl 3 ) δ: 0.11 (9H, s, --Si(CH 3 ) 3 ), 2.70-3.40 ##STR180## 3.70(3H, s, OCH 3 ), 4.83(1H, m, >CH--OSi) ii) Esterification
0.50 g of 4-(4'-octyloxy-4-biphenylcarbonyloxy)benzoic acid was mixed with 10 ml of thionyl chloride, and the mixture was refluxed for 4 hours. Excessive thionyl chloride was removed by distillation. To the remaining crude acid chloride were added 20 ml of dry acetonitrile, 15 mg of zinc chloride and 0.26 g of the methyl cis-(3R,4S)-tetrahydro-4-trimethylsilyloxythiophene-3-carboxylate, obtained in i) above. The mixture was refluxed for 1 hour. After the completion of the reaction, the reaction mixture was concentrated. The residue was subjected to separation and purification by column chromatography using silica gel and dichloromethane-ethyl acetate (10:1) and then to recrystallization from dichloromethane-methanol (1:10) to obtain 0.36 g of the title compound as colorless powdery crystals. The IR and 1 H-NMR spectra are shown below.
IR ν max KBr cm -1 : 1740, 1720 1 H-NMR (90 MHz, CDCl 3 ) δ: 0.90(3H, t, --CH 2 CH 3 ), 1.10-2.00(12H, m, CH 2 ), 3.03-3.56 ##STR181## 3.68(3H, s, OCH 2 ), 4.02(2H, t, J=6 Hz, OCH 2 ), 5.97(1H, m, >CH--OSi), 6.88-8.30(12H, m, aromatic H)
EXAMPLE 52
Preparation of cis-(3R,4S)-tetrahydro-3-methoxycarbonyl-4-thienyl ester of 4'-octyloxy-4-biphenylcarboxylic acid
Using 0.36 g of methyl cis-(3R,4S)-tetrahydro-4-trimethylsilyloxythiophene-3-carboxylate and 0.50 g of 4'-octyloxy-4-biphenylcarboxylic acid and in the same procedure as in Example 51, there was obtained 0.42 g of the title compound as colorless powdery crystals [recrystallized from dichloromethane-methanol (1:10)]
EXAMPLE 53
Preparation of cis-(3R,4S)-tetrahydro-3-methoxycarbonyl-4-thienyl ester of 4-(4'-octyloxy-4-biphenyloxycarbonyl)benzoic acid
Using 0.26 g of methyl cis-(3R,4S)-tetrahydro-4-trimethylsilyloxythiophene-3-carboxylate and 0.50 g of 4-(4'-octyloxy-4-biphenyloxycarbonyl)benzoic acid and in the same procedure as in Example 51, there was obtained 0.14 g of the title compound as colorless powdery crystals [recrystallized from dichloromethane-methanol (1:10)].
EXAMPLE 54
Preparation of cis-(2R,3S)-tetrahydro-2-methoxycarbonyl-3-thienyl ester of 4-(4'-octyloxy-4-biphenylcarbonyloxy)benzoic acid
i) Preparation of methyl cis-(2R,3S)-tetrahydro-3-trimethylsilyloxythiophene-2-carboxylate
This optically active cyclic dichiral compound can be prepared according to the following scheme. ##STR182##
Methyl tetrahydro-3-oxothiophene-2-carboxylate was subjected to asymmetric reduction using baker's yeast according to the known method [R. W. Hoffmann et al., Tetrahedron Lett., 23, 3479 (1982)], and the resulting methyl cis-(2R,3S)-tetrahydro-3-hydroxythiophene-2-carboxylate was subjected to trimethylsilylation by 1,1,1,3,3,3-hexamethyldisilazane according to a conventional method to obtain the title compound. The IR and 1 H-NMR spectra of the compound are shown below.
IR ν max neat cm -1 : 1740 1 H-NMR (90 MHz , CDCl 3 ) δ: 0.12(9H, s, --Si(CH 3 ) 3 ), 2.78-3.30(4H, m, --CH 2 --CH 2 --S), 3.72(3H, s, --OCH 3 ), 3.89 ##STR183## 4.80 (1H, m, >CH--OSi) ii) Esterification
10 ml of thionyl chloride was added to 0.70 g of 4-(4'-octyloxy-4-biphenylcarbonyloxy)benzoic acid. The mixture was refluxed for 4 hours. Excessive thionyl chloride was removed by distillation. To the remaining crude acid chloride were added 15 ml of dry acetonitrile, 27 mg of zinc chloride and 0.40 g of the methyl cis-(2R,3S)-tetrahydro-3-trimethylsilylthiophene-2-carboxylate. The mixture was refluxed for 1 hour. After the completion of the reaction, the reaction mixture was concentrated. The residue was subjected to separation and purification by column chromatography using silica gel and n-hexane-ethyl acetate (10:1) and then to recrystallization from ethanol to obtain 0.15 g of the title compound as colorless powder. The 1 H-NMR spectrum of the compound is shown below.
1 H-NMR (90 MHz, CDCl 3 ) δ: 0.90 (3H, t, --CH 2 CH 3 ), 1.15-1.60(10H, b, --CH 2 --), 1.60-1.98(2H, m, --OCH 2 CH 2 CH 2 --), 2.21-2.87 ##STR184## 2.91-3.40 (2H, m, --CH 2 --CH 2 --S--), 3.60(3H, s, OCH 3 ), 4.02(2H t, --OCH 2 --), 4.32(1H, d, >CH--S), 5.78(1H, d, t, >CH--O--), 6.94-8.26(12H, m, aromatic H)
EXAMPLE 55
Preparation of 4'-octyloxy-4-biphenyl ester of cis-(3R,4S)-tetrahydro-4-methoxyfuran-3-carboxylic acid
i) Preparation of ethyl cis-(3R,4S)-tetrahydro-4-methoxy-furan-3-carboxylate
This optically active cyclic dichiral ethyl carboxylate can be prepared according to the following scheme. ##STR185## Ethyl 4-oxotetrahydrofuran-3-carboxylate was subjected to asymmetric reduction using baker's yeast and the resulting ethyl cis-(3R,4S)-4-hydroxy-tetrahydrofuran-3-carboxylate was subjected to methylation to obtain the title compound.
The IR and 1 H-NMR spectra of the compound are shown below.
IR ν max neat cm -1 : 1740 1 H-NMR (90 MHz, CDCl 3 ) δ: 1.30(3H, t, --OCH 2 CH 3 ), 3.30(3H, s, --OCH 3 ), 3.43-3.57 ##STR186## 4.17(2H, q, --OCH 2 CH 3 ), 3.70-4.45 ii) Esterification
200 mg of the ethyl cis-(3R,4S)-tetrahydro-4-methoxyfuran-3-carboxylate obtained in i) above was added to a mixture of 2 ml of dioxane and 2 ml of 2N hydrochloric acid. The resulting mixture was stirred for 5 hours at 80° C. to effect acidic hydrolysis. 180 mg of the resulting crude carboxylic acid (IR ν max neat cm -1 : 1705) was reacted with 2 ml of oxalyl chloride to obtain 200 mg of a corresponding acid chloride (IR ν max neat cm -1 : 1790) . The acid chloride was added to a solution of 596 mg of 4-octyloxy-4-biphenol and 202 mg of triethylamine dissolved in 10 ml of dry tetrahydrofuran, with stirring at room temperature. The mixture was stirred overnight and the reaction mixture was concentrated under reduced pressure. The residue was subjected to column chromatography (developing solvent: chloroform) to obtain 190 mg of the title compound. The IR and 1 H-NMR spectra of the compound are shown below.
IR ν max KBr cm -1 : 1760, 1610, 1500, 1170 1 H-NMR (90 MHz, CDCl 3 ) δ: 0.90(3H, t, --CH 2 CH 3 ), 1.10-2.00(12H, m, --CH 2 --), 3.33-3.60 ##STR187## 3.47(3H, s, --OCH 3 ), 3.83-4.47 ##STR188## 4.00 ##STR189## 6.85-7.60(8H, m, aromatic H)
EXAMPLE 56 ##STR190##
Using 0.56 g of cis-(1R,2S)-2-methoxycyclopentan-1-carboxylic chloride and 0.93 g of the sleletal compound, 4'-(5-hexenyl)oxy-4-biphenol, and in the procedure same as that of Example 1, there was obtained 0.70 g of the title compound as an oil. 1 H-NMR spectra data of the present compound is shown as below.
1 H-NMR (CDCl 3 ) δ: 1.35 to 2.40(14H, m, --CH 2 --), 3.10 ##STR191## 3.39(1H, S, --OCH 3 ), 3.98(2H, t, J=6 Hz, --0--CH 2 --), 4.10(1H, m, --CH--OCH 3 ), 5.0(2H, t, J=8.5 Hz, CH 2 =C<), 5.60 to 5.78 (1H, m, >C=CH--), 6.80 to 7.60 ##STR192##
EXAMPLE 57 ##STR193##
Using 0.50 g of cis-(1R,2S)-2-methoxycyclopentan-1-carboxylic chloride and 0.88 g of the skeletal compound, 4-(2-octylthio-5-pyrimidinyl) phenol, and in the procedure same as that of Example 1, there was obtained 0.76 g of the title compound as colorless plates (recrystallized from ethyl acetate-hexane), 1 H-NMR spectra data of the present compound is shown as below.
1 H-NMR (CDCl 3 ) δ: 0.88(3H, t, --CH 2 --CH 3 ), 1.12 to 2.40(18H, m, CH 2 ), 3.19(2H, t, J=7 Hz, S--CH 2 ), 3.0 to 3.2 (1H, m, CH--COO), 3.39(3H, S, OCH 3 ), 4.14(1H, m, CH--OCH 3 ), 7.21(2H, d, J=9 Hz, aromatic H), 7.52(2H, d, J=9 Hz, aromatic H), 8.69(2H, s, aromatic H)
EXAMPLE 58 ##STR194##
Using 0.53 g of cis-(1R,2S)-2-methoxycyclopentan-1-carboxylic chloride and 0.80 g of the skeletal compound, 4-(5-hexynyl)oxy-4-biphenol, and in the manner same as that of Example 1, there was obtained 0.92 g of the title compound as colorless plates (recrystallized from hot ethanol). 1 H-NMR spectra data is shown as below.
1 H-NMR (CDCl 3 ) δ: 1.60 to 2.30(12H, m, --CH 2 --), 2.35(1H, m, HC.tbd.C--), 3.10 ##STR195## 3.39(3H, S, --O--CH 3 ), 4.00(2H, t, J=6 Hz, --O--CH 2 --), 4.10(1H, m, --CH--OCH 3 ), 6.88 to 7.52 ##STR196##
EXAMPLE 59 ##STR197##
Using 0.50 g of cis-(1R,2S)-2-methoxycyclopentane-1-carboxychloride and 0.87 g of 4-(2-heptenyl)-4-biphenol and in the manner same as that of Example 1, there was obtained 0.64 g of the title compound as colorless needles (recrystallized from ethanol). 1 H-NMR spectra data of the present compound is shown as below.
1 H-NMR (CDCl 3 , 90 MHz) δ: 0.7 to 1.05(3H, m, CH 3 ), 1.05 to 2.5 (12H, m, CH 2 ), 2.9 to 3.35(1H, m, --OCH<), 3.39(3H, S, OCH 3 ), 4.0 to 4.26 ##STR198## 4.50(2H, d, g=4.7 Hz, allyl CH 2 ), 5.5 to 6.1(2H, m, vinyl H), 6.8 to 7.65(8H, m, aromatic H).
EXAMPLE 60 ##STR199##
Using 0.50 g of cis-(1R,2S)-2-methoxycyclopentane-1-carboxylic acid chloride and 0.96 g of 4-(2-octenoyloxy)-4-biphenyl, and in the same procedure as in Example 1, there was obtained 0.92 g of the title compound as colorless needles (recrystallized from ethanol). 1 H-NMR spectra data of the present compound is shown below.
1 H-NMR (CDCl 3 , 90 MHz) δ: 0.75-1.05(3H, m, CH 3 ), 1.05-2.45 (14H, m, CH 2 ), 2.95-3.45(1H, m, OCH<), 3.40(3H, S, OCH 3 ), 3.9-4.3 ##STR200## 6.03(1H, d, g=15.5 Hz, vinyl H), 6.8-7.7(9H, m, aromatic H and vinyl H)
TABLE 1__________________________________________________________________________Example No. Compound__________________________________________________________________________ ##STR201##2 ##STR202##3 ##STR203##4 ##STR204##5 ##STR205##6 ##STR206##7 ##STR207##8 ##STR208##9 ##STR209##10 ##STR210##11 ##STR211##12 ##STR212##13 ##STR213##14 ##STR214##15 ##STR215##16 ##STR216##17 ##STR217##18 ##STR218##19 ##STR219##20 ##STR220##21 ##STR221##22 ##STR222##23 ##STR223##24 ##STR224##25 ##STR225##26 ##STR226##27 ##STR227##28 ##STR228##29 ##STR229##30 ##STR230##31 ##STR231##32 ##STR232##33 ##STR233##34 ##STR234##35 ##STR235##36 ##STR236##37 ##STR237##38 ##STR238##39 ##STR239##40 ##STR240##41 ##STR241##42 ##STR242##43 ##STR243##44 ##STR244##45 ##STR245##46 ##STR246##47 ##STR247##48 ##STR248##49 ##STR249##50 ##STR250##51 ##STR251##52 ##STR252##53 ##STR253##54 ##STR254##55 ##STR255##56 ##STR256##57 ##STR257##58 ##STR258##59 ##STR259##60 ##STR260##__________________________________________________________________________ SpontaneousPhase transition polarization Elementaltemperature (°C.) (nC/cm.sup.2) analysis__________________________________________________________________________ ##STR261## 180 C.sub.27 H.sub.36 O.sub.4 (424. 580) Calculated: C, 76.38; H, 8.55 Found: C, 76.67; H, 8.72 ##STR262## 270 C.sub.34 H.sub.40 O.sub.6 (544. 688) Calculated: C, 74.97; H, 74.0 Found: C, 75.14; H, 7.50 ##STR263## 180 C.sub.34 H.sub.40 O.sub.6 (544. 688) Calculated: C, 74.97; H, 7.40 Found: C, 74.96; H, 7.45 ##STR264## C.sub.34 H.sub.40 O.sub.6 (544. 688) Calculated: C, 74.97; H, 7.40 Found: C, 74.99; H, 7.36 ##STR265## 120 C.sub.35 H.sub.42 O.sub.6 (558. 71) Calculated: C, 75.24, H, 7.58 Found: C, 75.27; H, 7.58 ##STR266## 133 C.sub.35 H.sub.42 O.sub.6 (558. 71) Calculated: C, 75.24; H, 7.58 Found: C, 75.43; H, 7.66 ##STR267## C.sub.28 H.sub.38 O.sub.4 Calculated: C, 76.28; H, 8.73 Found: C, 76.57; H, 8.75 ##STR268## 160 (87° C., 82.7° C.) C.sub.35 H.sub.42 O.sub.6 Calculated: C, 75.24; H, 7.58 Found: C, 75.07; H, 7.62 ##STR269## 14 C.sub.34 H.sub.40 O.sub.6 (544. 688) Calculated: C, 74.97; H, 7.40 Found: C, 75.21; H, 7.39 ##STR270## 12 (105° C.) C.sub.34 H.sub.40 O.sub.6 (544. 688) Calculated: C, 74.97; H, 7.40 Found: C, 75.04; H, 7.50 ##STR271## C.sub.27 H.sub.36 O.sub.4 (424. 580) Calculated: C, 76.38; H, 8.55 Found: C, 76.28; H, 8.60 ##STR272## -- C.sub.29 H.sub.38 O.sub.6 Calculated: C, 72.27; H, 7.94 Found: C, 72.16; H, 7.96 ##STR273## -- C.sub.29 H.sub.38 O.sub.5 Calculated: C, 74.65; H, 8.21 Found: C, 74.37; H, 8.26 ##STR274## 83 (81° C.) C.sub.35 H.sub.43 O.sub.5 Calculated: C, 77.32; H, 7.97 Found: C, 77.55; H, 7.85 ##STR275## ˜0 C.sub.35 H.sub.42 O.sub.6 Calculated: C, 75.24; H, 7.58 Found: C, 75.30; H, 7.44 ##STR276## -- C.sub.30 H.sub.32 O.sub.6 Calculated: C, 73.75; H, 6.60 Found: C, 73.98; H, 6.59 ##STR277## -- C.sub.30 H.sub.42 O.sub.4 Calculated: C, 77.21; H, 9.07 Found: C, 76.91; H, 9.10 ##STR278## -- C.sub.32 H.sub.46 O.sub.4 Calculated: C, 77.69; H, 9.37 Found: C, 77.90; H, 9.45 ##STR279## 93 C.sub.35 H.sub.44 O.sub.5 Calculated: C, 77.17; H, 8.14 Found: C, 77.90; H, 8.12 ##STR280## -- C.sub.37 H.sub.46 O.sub.6 Calculated: C, 75.74; H, 7.90 Found: C, 75.47; H, 7.89 ##STR281## C.sub.37 H.sub.46 O.sub.6 Calculated: C, 75.74; H, 7.90 Found: C, 75.64; H, 7.89 ##STR282## C.sub.35 H.sub.42 O.sub.6 (558. 715) Calculated: C, 75.24; H, 7.58 Found: C, 75.21; H, 7.57 ##STR283## -- C.sub.35 H.sub.42 O.sub.6 (558. 715) Calculated: C, 75.24; H, 7.58 Found: C, 75.42; H, 7.61 ##STR284## -- C.sub.35 H.sub.42 O.sub.6 (558. 715) Calculated: C, 75.24; H, 7.58 Found: C, 75.27; H, 7.57 ##STR285## -- C.sub.28 H.sub.38 O.sub.4 (438. 607) Calculated: C, 76.68; H, 8.73 Found: C, 76.81; H, 8.86 ##STR286## -- C.sub.34 H.sub.42 O.sub.5 Calculated: C, 76.95; H, 7.98 Found: C, 77.21; H, 8.00 ##STR287## 6 C.sub.34 H.sub.42 O.sub.5 Calculated: C, 76.95; H, 7.98 Found: C, 77.21; H, 8.00 ##STR288## -- C.sub.34 H.sub.42 O.sub.5 Calculated : C, 76.95; H, 7.98 Found: C, 77.06; H, 7.97 ##STR289## C.sub.34 H.sub.42 O.sub.5 Calculated: C, 76.95; H, 7l.98 Found: C, 77.01; H, 7.93 ##STR290## -- C.sub.28 H.sub.38 O.sub.4 Calculated: C, 76.68; H, 8.73 Found: C, 76.93; H, 8.80 ##STR291## -- C.sub.27 H.sub. 38 O.sub.3 Calculated : C, 78.98; H, 9.33 Found: C, 79.08; H, 9.35 ##STR292## -- C.sub.35 H.sub.42 O.sub.6 Calculated: C, 75.24; H, 7.58 Found: C, 73.72; H, 6.95 ##STR293## ˜0 C.sub.35 H.sub.42 O.sub.6 Calculated: C, 75.24; H, 7.58 Found: C, 75.17; H, 7.57 ##STR294## ˜0 C.sub.34 H.sub.42 O.sub.5 (530. 705) Calculated: C, 76.95; H, 7.98 Found: C, 76.78; H, 7.93 ##STR295## 200 C.sub.34 H.sub.42 O.sub.5 (530. 705) Calculated: C, 76.95; H, 7.98 Found: C, 76.88; H, 7.97 ##STR296## 156 C.sub.34 H.sub.40 O.sub.5 (528. 689) Calculated: C, 77.24; H, 7.63 Found: C, 77.32; H, 7.63 ##STR297## ˜0 C.sub.40 H.sub.52 O.sub.6 (628. 849) Calculated: C, 76.40; H, 8.33 Found: C, 76.59; H, 8.45 ##STR298## 180 (40° C.) C.sub.28 H.sub.36 O.sub.5 (452. 59) Calculated: C, 74.31; H, 8.02 Found: C, 74.48; H, 8.06 ##STR299## -- C.sub.31 H.sub.44 O.sub.4 (480. 68) Calculated: C, 77.46; H, 9.23 Found: C, 77.44; H, 9.28 ##STR300## -- C.sub.29 H.sub.40 O.sub.4 (452. 63) Calculated: C, 76.95; H, 8.91 Found: C, 77.01; H, 8.98 ##STR301## C.sub.28 H.sub.38 O.sub.4 (438. 60) Calculated: C, 76.68; H, 8.73 Found: C, 76.67; H, 8.66 ##STR302## -- C.sub.26 H.sub.34 O.sub.4 (410. 55) Calculated: C, 76.06; H, 8.35 Found: C, 76.04; H, 8.35 ##STR303## -- C.sub.25 H.sub.32 O.sub.4 (396. 52) Calculated: C, 75.73; H, 8.13 Found: C, 75.72; H, 8.17 ##STR304## -- C.sub.24 H.sub.30 O.sub.4 (382. 50) Calculated: C, 75.36; H, 7.91 Found: C, 75.28; H, 7.83 ##STR305## -- C.sub.25 H.sub.34 N.sub.2 O.sub.5 (426. 55) Calculated: C, 70.40; H, 8.03 Found: C, 70.30; H, 8.09 ##STR306## ˜0 C.sub.34 H.sub.42 O.sub.5 (530. 705) Calculated: C, 76.95; H, 7.98 Found: C, 76.90; H, 8.04 ##STR307## -- C.sub.29 H.sub.36 O.sub.5 (464. 602) Calculated: C, 74.97; H, 7.81 Found: C, 75.16; H, 7.80 ##STR308## -- C.sub.36 H.sub.40 O.sub.7 (584. 709) Calculated: C, 73.95; H, 8.90 Found: C, 73.99; H, 6.93 ##STR309## C.sub.36 H.sub.42 O.sub.7 (586. 725) Calculated: C, 73.70; H, 7.22 Found: C, 73.60; H, 7.13 ##STR310## -- C.sub.29 H.sub.38 O.sub.5 (466. 618) Calculated: C, 74.65; H, 8.21 Found: C, 74.59; H, 7.96 ##STR311## C.sub.34 H.sub.38 O.sub.7 S (590. 738) Calculated: C, 69.13; H, 6.48 Found: C, 68.97; H, 6.38 ##STR312## -- C.sub.27 H.sub.34 O.sub.5 S (470. 630) Calculated: C, 68.91; H, 7.28 Found: C, 68.95; H, 7.15 ##STR313## -- C.sub.34 H.sub.38 O.sub.7 S (590. 738) Calculated: C, 69.13; H, 6.48 Found: C, 68.89; H, 6.36 ##STR314## -- C.sub.34 H.sub.38 O.sub.7 S (590. 738) Calculated: C, 69.13; H, 6.48 Found: C, 69.16; H, 6.36 ##STR315## -- ##STR316## 298 C.sub.27 H.sub.34 O.sub.4 (422. 565) Calculated: C, 69.55; H, 73.0 Found: C, 69.50; H, 7.34 ##STR317## -- C.sub.25 H.sub.24 N.sub.2 O.sub.3 S (442. 615) Calculated: C, 67.84; H, 7.74: N, 6.33 Found: C, 67.89; H, 7.81; N, 6.28 ##STR318## C.sub.25 H.sub.28 O.sub.4 (392. 493) Calculated: C, 76.50; H, 7.19 Found: C, 76.67; H, 7.26 ##STR319## -- C.sub.26 H.sub.32 O.sub.4 (408. 538) Calculated: C, 76.44; H, 7.90 Found: C, 76.53; H, 7.94 ##STR320## -- C.sub.27 H.sub.32 O.sub.5 (436. 548) Calculated: C, 74.29; H, 7.39 Found: C, 74.31; H, 7.46__________________________________________________________________________
Application Example 1
The optically active compounds of the present invention shown in Table 1 were incorporated into the known ferroelectric liquid crystal compounds A to C (hereinafter referred to as mother liquid crystals) shown in Table 2, in given amounts, to prepare liquid crystal compositions shown in Table 3 each containing an optically active compound of the present invention.
These compositions and the mother liquid crystals A-C were measured for spontaneous polarization. The results are shown in Table 3.
In Table 3, the values of spontaneous polarization are those at a temperature lower by 10° C. than the upper limit temperature of chiral smectic C phase.
TABLE 2______________________________________Motherliquidcrystal Chemical structure______________________________________ ##STR321## ##STR322##B ##STR323##C ##STR324## ##STR325##______________________________________
TABLE 3______________________________________ Optically active compoundMother I of this invention Spontaneousliquid Example Amount used polarizationcrystal No. (wt. %) (nC/cm.sup.2)______________________________________A -- -- 4A 2 10 30A 3 10 26A 8 20 34B -- -- <1B 1 20 32B 2 10 26B 5 10 13B 21 10 11B 38 20 25C -- -- <1C 1 30 51C 6 10 15C 14 20 15______________________________________
Each liquid crystal composition shown in Table 3 was sealed in a cell constituted by (a) two glass substrates each with a transparent electrode, obtained by spin coating of a polyimide and subsequent rubbing and (b) a spacer consisting of a polyethylene terephthalate film 6 μm in thickness, whereby liquid crystal devices were prepared. A rectangular wave (40 Vp-p) was applied to the liquid crystal devices at room temperature, and their optical responses were observed by a polarizing microscope. The devices containing the compositions using the optically active compounds of the present invention gave an optical contrast and showed a very good optical response, while the devices containing the mother liquid crystal B or C alone showed no clear optical response.
Application Example 2
The optically active compounds of the present invention shown in Table 4 were incorporated into the mother liquid crystal A, and the resulting compositions were measured for spontaneous polarization. The results are shown in Table 4. In Table 4, the values of spontaneous polarization are those at a temperature 10° C. lower than the upper limit of Sc* phase.
TABLE 4______________________________________ Optically active compoundMother I of this invention Spontaneousliquid Example Amount used polarizationcrystal No. (wt. %) (nC/cm.sup.2)______________________________________A 51 10 15A 51 20 28A 51 30 41A 52 10 13A 47 30 44A 48 20 25A -- -- <1______________________________________ Mother liquid crystal A: ##STR326## ##STR327##
The composition shown in the uppermost column of Table 4 was sealed in a cell constituted by (a) two glass substrates each with a transparent electrode, obtained by spin coating of a polyimide and subsequent rubbing and (b) a spacer consisting of a polyethylene terephthalate film of 6 μm in thickness, whereby a liquid crystal display device shown in FIG. 1 was prepared. A rectangular wave (40 Vp-p, 10 Hz) was applied to the device at room temperature and observation was made using a polarizing microscope. An optical response was observed. Meanwhile, a device containing the mother liquid crystal shown in the lowermost column of Table 4 showed no optical response even when the applied voltage was increased to 50 Vp-p.
As is clear from Examples and Application Examples, the present invention provides liquid crystal compounds and liquid crystal compositions having a large spontaneous polarization and showing a chiral smectic C phase. The liquid crystal compounds of the present invention can be effectively used to provide a liquid crystal composition of significantly increased opontaneous polarization. Accordingly, the optically active compounds of the present invention and the liquid crystal compositions containing these compounds are useful as a liquid crystal to be employed in optical modulators such as liquid crystal display apparatuses and can provide such apparatuses having excellent capabilities in response, etc.
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The invention relates to optically active compounds represented by the general formula ##STR1## wherein R 1 , R 2 , Q 1 , Q 2 , Q 3 , ##STR2## and M are defined as in the specification, methods and intermediates for their preparation, liquid crystal compositions comprising at least one optically active compound of formula I and their use in electrooptical display, switching and modulation devices.
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[0001] This application is a continuation in part of co-pending U.S. application Ser. No. 12/659,583 which is incorporated herein in its entirety by reference.
FIELD OF THE INVENTION
[0002] The invention relates to a protection element for the thermal insulation of piping, the element being also designed to act as a supporting device for a technical equipment that has to be routed along the piping. In particular, the technical equipment ideally follows the piping in order to detect any leaks from the piping.
[0003] The invention has been described more particularly in the context of the use of such protection elements in the field of aeronautics, for piping particularly carrying air at a high temperature and/or under high pressure. However, the invention applies to all areas involving protection elements or shells for piping.
[0004] In aircraft, dozens of meters of piping are arranged to collect air at high temperatures (260 to 540° C.) or under pressure (5 to 15 bar) from certain areas, such as at the engines, and to distribute that air to treatment systems that particularly make it possible to supply conditioned and/or pressurized air to specific spaces such as the cabin, in the passenger area, or provide hot air to the wings of the aircraft in order to defrost their leading edges.
[0005] The piping passes through unpressurized areas of the aircraft that are subjected to transport conditions, and is therefore exposed to the temperature and pressure conditions of the surrounding environment, particularly with temperatures of down to −50° C. and pressures as low as 0.2 bar. That is why it is necessary to insulate the piping thermally in order to carry the pressurized air at high temperatures without excessive thermal losses.
[0006] Further, it is mandatory, according to standards related to piping, that the thermal insulation is such that the surface temperature of the piping does not exceed 204° C., in order to avoid the risk of auto-ignition of fluids that may inopportunely come into contact with the outside of the pipes, as these pipes are going through areas carrying fluids such as aircraft fuel.
[0007] The piping is made of metal and is thermally insulated in a known manner by wrapping a thermally insulating material such as foam or mineral wool, and rigid protection elements placed above the insulating material. The protection elements, or at least their external skin, are generally made of metal or composite materials or of silicone or even of titanium.
[0008] The protection elements are formed of two half shells taking the pipe surrounded by the insulating material as a sandwich. The half shells are secured to the pipe by welding at their free ends, which have metal connecting sections with a Z-shaped cross-section one side of which is connected to the external skin of a half shell by gluing or welding, while the other side is designed to be welded to the pipe.
[0009] When the half shells are bounded together by gluing, this operation requires to use a curable adhesive, so as to get a strong and sealed seam, able to withstand mechanical and thermal loads. Therefore the protected piping shall be cured through an oven or an autoclave after being wrapped by the protective shell.
[0010] The piping is formed of sections joined end to end and welded to each other, and some of these are connected to closing and opening and/or regulation systems such as valves or angular compensators. The risk of leaking pipes and their connections are, for example related to a crack in the pipe, poor seal between sections, or loss of seal at the valve systems.
[0011] Leak detection is however a necessity, because these pipes run, as has been said earlier, in zones containing fluids that can self-ignite in contact with air at a high temperature.
[0012] Also, leaks can lead to a loss of function by the end system to be supplied (defrosting, air conditioning etc.)
[0013] In order to detect any leaks from the piping, the half shells of thermal insulation have orifices or aeration holes from which hot air can escape in the event of a leak, while a detection device such as sensing line is placed along the piping, with sensors opposite the aeration holes that are capable of detecting any hot air that may escape.
[0014] A sensing line is installed with supports similar to rings that are added around the thermal insulation of the pipes, which hold a cable at a certain distance from the pipe, carrying regularly spaced sensors that are located opposite the aeration holes.
[0015] These detection devices can only be put in place after the piping has been installed. Because of the intertwining of pipes in a small space, the work of putting in place and fastening a number of rings is not practical and remains fastidious, the more so since it is subsequently necessary to correctly position the cable with the sensors and the sensors opposite the aeration holes. Besides, an incorrectly fastened ring can lead to cable movement and thus a shift in the position of one or more sensors, which destroys the chance of efficient or even effective detection.
SUMMARY OF THE INVENTION
[0016] The invention is aimed at providing a protecting element for the thermal insulation of a piping, so as to form a shell of thermal insulation. This protective element providing an additional support function for a technical equipment and leading to a quick and easy installation of this equipment while ensuring its suitable positioning, said installation remaining reliable over time.
[0017] Another object of the invention is to provide a protective element that is lighter than those protective elements known from the prior art, more particularly suited for aeronautics applications.
[0018] A further object of the invention is to provide a protective element that can be secured safely and reliably to an insulated piping without use of welding or of a curing operation in an oven or in autoclave.
[0019] Accordingly, the invention concerns a protective element for protecting the thermal insulation of a pipe, said protective element comprising two half shells assembled to wrap the insulated pipe, including a half shell comprising a rigid platform protruding from the external surface of this half shell, the platform being suitable for positioning and fixing a technical equipment, wherein the shells are made of a fiber reinforced composite material, the rigid platform comprising a metallic insert integrated in the composite material.
[0020] That platform is thus integrated into the thickness of the wall. It does not constitute an independent element, but forms an integral part of the body by being a constitutive and inseparable member of the body. It forms a substantially flat surface. It constitutes means for positioning and/or supporting a device external to the protection element and distinct from the other protection element that may be added in a manner opposed to the element and opposite the cavity in a way as to form a full shell.
[0021] The platform thus provides a support for subsequent fastening. The platform is also used to make the half shell more rigid, thus avoiding deformation of the half shell over time.
[0022] The platform is raised above the remainder of the body and therefore above the pipe, placing the technical equipment to be associated at a certain separating distance from the pipe. In particular, for application in aeronautics with sensing lines, the lines are automatically set at the required distance from the shell and are set with certain regularity. This protrusion with regard to the external surface of the half shell facing the external environment is provided on the general side of the wall in order to make it more easily accessible as a means for positioning and attachment.
[0023] The protective element according to the invention is light, being made of a fiber reinforced composite material. Nevertheless, the metallic insert allows an equipment to be fastened on these shells by means of screwing or riveting, these kinds of fixture being not compatible with such a composite material.
[0024] Therefore, in an advantageous embodiment, the platform comprises at least one hole through the metallic insert, constituting a fastening means.
[0025] According to a particular preferred embodiment, said hole is tapped.
[0026] Advantageously, the protective element includes a shell wherein the wall of the shell comprises an escape hole close to the platform.
[0027] Advantageously, said escape hole is covered with a removable pad.
[0028] The removable pad makes it possible to use protection elements with or without a hole. If one or more escape holes are useful, particularly in the application of the invention in aeronautics for detecting any leak of fluid from the pipe, it is sufficient to pierce or detach the protective pad before adding the protection element against the pipe.
[0029] According to an advantageous embodiment of the protective element of the invention one of the half shells comprises a rabbet on one of its edges, the corresponding edge of the second half shell being adjusted to be guided by the rabbet and abut against the bottom of said rabbet, the joined assembly being covered by a strip of adhesive. This embodiment allows a precise assembly of the two half shells. The combination of this assembly with the adhesive produces a seal seam between the half shells.
[0030] Advantageously, the strip of adhesive is made of a fluorocarbonated elastomer coated with a permanent siliconated adhesive. Such an adhesive can withstand thermal and mechanical loads, when combined with the rabbet assembly, therefore avoiding the curing of the protected pipe in an oven or an autoclave.
[0031] The invention also relates to a thermally insulated piping comprising a plurality of protective elements according to any of the preceding embodiments, assembled end to end, wherein a sensing line, running alongside the piping, is secured to the platforms of the protective elements. Thus, the protective elements of the invention are used for fastening technical elements designed to follow the path of the piping wrapped with said elements.
[0032] According to a particular embodiment of this piping, using protective elements assembled through a rabbet, the adhesive strip extends alongside the joined assembly of the plurality of protective elements, therefore providing sealing alongside the assembly.
BRIEF DESCRIPTION OF THE DRAWINGS
[0033] This invention is now described with examples that are merely illustrative and do not in any way limit the scope of the invention, and by reference to the attached drawings, wherein:
[0034] FIG. 1 represents a perspective view of a protection element according to the invention.
[0035] FIG. 2 is a view of a longitudinal section of a pipe associated with protection elements according to the invention and complementary elements to form protective shells for the pipe.
[0036] FIG. 3 represents a perspective and top view of the protection element of FIG. 1 .
[0037] FIG. 4 represents a perspective and sectional view of a platform of the protection element according to the invention.
[0038] FIG. 5 shows schematically by an exploded view a section of the assembly of two shells made of a composite material, assembled through a rabbet sealed with an adhesive strip.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0039] FIG. 1 illustrates a protection element 1 according to the invention for the thermal insulation of pipes.
[0040] This protection element, with an open concavity 10 A, forms a half shell. It is made of a composite material comprising a plastic binder such as an epoxy resin reinforced by fibers with thermal insulation properties such as glass fibers.
[0041] Such a half shell is designed to cover pipes by being assembled opposite a half shell with similar mechanical and insulating properties and generally an equivalent shape, to form a protective shell.
[0042] FIG. 2 represents a sectional view of a pipe 2 sandwiched between one half shell 1 of the invention and the complementary half shell 3 , together making up a protective shell 4 around the pipe. Such a shell is for instance used for the thermal protection of the pipes used in aircraft, which convey air at a high temperature (up to 540° C.). The pipes are wrapped in thermal insulation 5 such as foam or insulating wool and covered by the protection shell 4 that forms an external skin, the temperature of which does not exceed 204° C. in accordance with the standards applicable in the area of aeronautics.
[0043] The protection element or half shell 1 may be straight or bent to adapt to the shape of the pipe to cover.
[0044] As illustrated in FIGS. 1 and 3 , the protection element 1 has a body 10 comprising a wall 11 with a shape that is substantially concave or semi-cylindrical to cooperate with the substantially cylindrical shape of the pipes, and free ends 12 .
[0045] Advantageously, the wall 11 has a shoulder 13 at each end 12 of the body that is designed for making the protection element integral with the pipe.
[0046] The wall 11 has free lateral edges 14 designed to constitute support edges for the opposite edges of the complementary half shell 3 to assemble.
[0047] Optionally, and in relation with the purpose of the half shell, the half shell has holes 8 to allow, as will be described later, the fluid flowing in the pipes to escape if the pipes have a leak.
[0048] As can be seen in FIG. 2 , the protection element 1 is assembled on the pipe by placing the concavity 10 A of the body against the insulation 5 , and by setting the ends 12 against the pipe 2 . Fastening is carried out by gluing means 6 adapted to the connection of the metal material of the pipe to the composite materials of the ends 12 , more particularly of the shoulder 13 .
[0049] Note that the fastening of the ends 12 of the protection element is carried out advantageously directly at the body 10 by the adapted conformation of the shoulders 13 .
[0050] The complementary half shell 3 is added and fastened to the pipe in the same way as the protection element 1 .
[0051] As can be seen in FIG. 2 , the pipe 2 comprises several shells 4 , joined end to end with each other, so as to follow the lines or curves of the pipe. Each protection element 1 of a protection shell is associated with the same side of the pipe.
[0052] According to the invention, the protection element 1 acts as the means for supporting and positioning technical equipment 7 to be associated with the pipe ( FIG. 2 ).
[0053] The technical equipment 7 may for example be a sensing line for detecting leaks of air or other gases from the pipe. The line may itself be a sensor or be replaced by a series of sensors 70 distributed discretely, and must imperatively follow the pipe, at a specific distance from the pipe and in such a way that the sensors are placed in the immediate vicinity of at least one escape hole 8 provided in the protection element. In the event of a leak, the air escapes from the holes 8 and is detected by the sensors.
[0054] According to the invention, the protection element has a configuration that makes it directly support the sensing line. The wall 11 of the protection element 1 comprises at least one projecting shape or rigid platform 16 that constitutes a means for positioning and/or supporting the technical equipment 7 to be associated with the said element.
[0055] The platform constitutes a boss in relation to the external side 11 A of the wall, which is the side opposite the open concavity 10 A. It is formed by molding when the body of the element is manufactured.
[0056] The platform 16 is sufficiently rigid and integrates in the wall of the body, as can be seen in FIGS. 2 and 4 , at least one metal insert 9 , to provide a support and fastening zone. The insert is made integral by insertion in the composite material of the body 10 during the manufacturing by molding of the protection element.
[0057] The platform 16 advantageously has at least one hole 17 that can be seen in FIGS. 3 and 4 , which is designed to cooperate with a fastening piece 90 ( FIG. 2 ) such as a screw or a rivet for fastening the technical element 7 . Depending on the type of fastening used for the equipment to associate, the hole may be smooth or threaded.
[0058] The sensing line is thereby fastened for example in the manner shown in FIG. 2 , the sensing line being a cable associated at a distance from the remainder of the body 10 of the protection element, and thus at a distance from the pipe. The line may be replaced by a series of sensors 70 distributed discretely. The sensors are then positioned appropriately, directly opposite the escape holes 8 .
[0059] The protection element in the invention is therefore used to provide, in addition to its thermal insulation function, the function of supporting for positioning and/or fastening equipment, thanks to the presence of a rigid platform forming a surface that is appropriate for fastening.
[0060] FIG. 5 shows a section of a protective element according to a preferred embodiment of the invention. Although said section is here represented as straight and without a platform, it shall be understood that such a protective element advantageously comprises any and all of the features described above. The two half shells 501 , 502 are made by laying up pre-impregnated fiber plies in a mold, and curing such lay up in this mold. Alternatively these half shells are made by laying up dry fibers in the mold and further injecting liquid resin in the layup.
[0061] One of these half shells, here the lower shell 503 , comprises a rabbet 510 . The opposite half shell 501 , here the upper shell, is fitted over this rabbet 510 and brought to abutment with the bottom face 511 of said rabbet. Therefore both half shells are precisely positioned relative to each other.
[0062] An adhesive strip 520 , preferably made of a fluorocarbonated polymer coated with a siliconated adhesive is stuck over the seam between the two shells. When a plurality of such protective elements is assembled end to end, so as to cover a whole piping, the adhesive is stuck over the seams so as to insure proper sealing of the assembly. The adhesive strip is compliant enough so as to perfectly cover the seam. The use of a high temperature resistant pressure sensitive permanent adhesive avoids a subsequent curing operation and greatly simplifies the implementation of such a protective element.
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A thermally insulating protection element for piping, including a hollow body with an open concavity and having a wall. The wall includes at least one rigid positioning and/or support platform designed to accommodate the fastening of technical equipment to be associated with the protection element. The element is designed to not only insulate piping, but also to constitute a direct device for supporting and fastening technical equipment such as a sensing line.
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BACKGROUND OF THE INVENTION
(1) Field of the Invention
The present invention relates generally to fabric handling systems and, more particularly, to an apparatus for batching and inspecting a continuous, large fabric roll.
(2) Description of the Prior Art
Historically, circular knitting machines have employed take-up rolls for receiving knitted fabric which are capable of holding between about 50 to 250 lb. rolls. Subsequent fabric processing, including bleaching and dyeing require larger continuous quantities of fabric for efficient handling. In order to achieve longer continuous quantities of fabric, fabric from small fabric rolls were stitched together to form a continuous cloth. Problems associated with stitching smaller fabric sections together include varying product quality and properties, like inconsistent courses per inch (CPI), stretch and shrinkage, stretch and distortion of fabric wales, lower productivity due to machine downtime for removing and loading new fabric rolls, and an increased number of seams causing additional waste at cutting.
One solution to this problem is disclosed in co-pending U.S. patent application Ser. No. 08/911,296, filed Aug. 8, 1997, which is hereby incorporated by reference in its entirety. It teaches a circular knitting machine with a tension-controlled large roll take-up assembly which can form very large continuous fabric rolls for improved quality in subsequent processing, including bleaching, finishing, and cutting operations while, at the same time, permits the operator to attend to most machine functions without the need for a ladder or catwalk. However, the fabric roll produced by this machine may be each 450 lbs., or more. As such, more mechanical assistance than the smaller 50-lbs. fabric rolls may be required.
Thus, there is a need for a fabric handling system for letting off a continuous, large fabric roll while, at the same time, permits the operator to automatically batch the fabric roll and inspect the fabric web.
SUMMARY OF THE INVENTION
The present invention is directed to a fabric roll letoff for unrolling and inspecting a fabric roll. The apparatus includes a continuous belt for supporting the fabric roll. A drive system that rotates the belt to letoff the fabric web. The drive system includes a drive roller; an idle roller; and a tension roller. Thus, the continuous belt receives the fabric roll and rotates the fabric roll to unroll the fabric web at a constant velocity for subsequent processing. In the preferred embodiment, a pair of loading arms is connected to the belt drive support structure for receiving the fabric roll and for positioning the fabric roll onto the belt drive. Also, in the preferred embodiment, a guide frame is positioned downstream from the belt drive for directing the fabric web through an inspection area.
Accordingly, one aspect of the present invention is to provide a fabric roll letoff for unrolling and inspecting a fabric roll. The apparatus includes: a belt drive extending between at least one pair of rollers wherein the belt drive rotates about the rollers for unloading the fabric web from the fabric roll; and a guide frame positioned downstream from the belt drive for directing the fabric web through an inspection area.
Another aspect of the present invention is to provide a fabric roll letoff for unwinding a fabric roll. The apparatus includes: a continuous belt for supporting the fabric roll; a drive system for rotating the belt including a drive roller; a idle roller; and a tension roller, wherein the continuous belt receives the fabric roll and rotates the fabric roll to unroll the fabric web at a constant velocity.
Still another aspect of the present invention is to provide a fabric roll letoff for unrolling and inspecting a fabric roll. The apparatus includes: a continuous belt for supporting the fabric roll; a drive system for rotating the belt including a drive roller; a idle roller; and a tension roller, wherein the continuous belt receives the fabric roll and rotates the fabric roll to unroll the fabric web at a constant velocity; a guide frame positioned downstream from the belt drive for directing the fabric web through an inspection area; and a pair of loading arms connected to the belt drive support structure for receiving the fabric roll, the loading arms having a first end positioned away from the belt drive for receiving the fabric roll, and a second end for positioning the fabric roll onto the belt drive.
These and other aspects of the present invention will become apparent to those skilled in the art after a reading of the following description of the preferred embodiment when considered with the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevational view illustrating a fabric roll letoff constructed according to the present invention;
FIG. 2 is a front perspective view illustrating a fabric roll mounted on the fabric roll letoff;
FIG. 3 is an enlarged side view illustrating the arrangement of the belt drive of the fabric roll letoff; and
FIG. 4 is a side elevational view illustrating a fabric roll located on the outer edges of the unloader arms prior to being loaded onto the belt drive.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the following description, like reference characters designate like or corresponding parts throughout the several views. Also in the following description, it is to be understood that such terms as "forward," "rearward," "left," "right," "upwardly," downwardly," and the like are words of convenience and are not to be construed as limiting terms.
Referring now to the drawings in general and FIG. 1 in particular, it will be understood that the illustrations are for the purpose of describing the preferred embodiment of the invention and are not intended to limit the invention thereto. As best seen in FIG. 1, a large fabric roll letoff, generally designated 10, is shown constructed according to the present invention. The large fabric roll letoff generally includes a guide frame 12, a belt drive 14, and loader device 16.
The belt drive 14 functions to rotate the fabric roll to unwind the fabric web and includes a drive roller 36, an idle roller 40 and a tension roller 42. The drive roller 36 is connected to a motor 46, which rotates the roller resulting in driving the belt while, at the same time, is capable of stopping the large fabric roll in less than one revolution for safety. In one embodiment, the motor is a 10 horse power unit model number AF4S10T61Q1, manufactured by the Lincoln Company. The motor 46 and drive roller 36 are capable of rotating the belt to provide unrolling of the fabric roll 11 at a surface speed from between about 0 yards per minute (ypm) and up to about 350 ypm. The idle roller 40 provides spacing for the belt as it rotates to unload the fabric roll to prevent the two sides of the belt from rubbing against one another.
The tension roller 42 maintains a constant, predetermined tension on the belt 34. The tension roller 42 includes an arm 50 that extends and contracts depending on the changes of the diameter of the fabric roll due to unwinding. By way of an example, the arm 50 will be extended a lesser distance when the diameter of the fabric roll 11 is large, and a greater distance when the diameter is smaller to maintain the constant tension. In one embodiment, the arm 50 is pneumatically actuated to extend out maintaining substantially constant tension on the belt and, thereby, between the belt and the changing diameter of the fabric roll.
The drive roller 36, idle roller 40, and tension roller 42 are preferably cylindrical-shaped for contacting the belt 34. Rollers 36, 40, and 42 further include a groove cut into the cylinders for housing a notch extending from the belt. The groove functions to maintain the belt on the cylinders and prevent the belt from slipping off the edge. This is particularly important when the fabric roll is off-center and pushes the belt to one side during the batching process. Additionally, the drive roller 36, idle roller 40 and tension roller 42 have a width approximately equal to or somewhat wider than the belt width.
The belt 34 extends about the rollers of the belt drive, as illustrated in FIGS. 1, 3 and 4. In one embodiment, the belt is of a seamless construction for strength and for protecting the surface of the fabric web and may be constructed of PVC plastic. Preferably, the belt 34 has a width larger than the width of the fabric roll 11 to better support the roll. In the preferred embodiment, a notch extends from the inside of the belt to mate with the grooves of the rollers to maintain the belt on the rollers.
The loader device 16 provides for loading the fabric roll 11 onto the belt drive 14. The loader device 16 include a pair of arms 54 positioned a fixed distance apart, preferably slightly wider than the width of the fabric roll, as illustrated in FIG. 2. Each arm 54 includes a ridge 60 located on the upper side to help facilitate loading of the fabric roll 11 and guide the fabric roll from the first position as illustrated in FIG. 4 to the second loaded position as illustrated in FIG. 1. A central shaft 13 extends through the fabric roll 11 and extends beyond the ends of the fabric roll to fit within the ridges 60 to prevent the fabric roll from dismounting.
An actuator 56 is positioned at a first end of the arms 54 for raising and lowering the first end. Preferably, the actuator is pneumatically controlled, although one skilled in the art will recognize other styles will function properly. A load cell 66 is connected to the loading arms first end for weighing the fabric roll once placed on the loader arms 54. This positioning of the load cell 66 reduces the need for a separate step of weighing the rolls at a separate location also the additional material handling of the fabric roll prior to batching.
Unwinding cradle 44 is positioned at the end of the loader arms 54 to maintain the roll on the belt during the batching process. The unwinding cradle 44 supports the weight of the roll during the batching process. Clamps 64 are mounted on the unwinding cradle 44 for maintaining the fabric roll on the belt drive in a second position as illustrated in FIG. 3. Clamps 64 are selectively positionable between an open orientation for loading and unloading the fabric roll into the unwinding cradle 44, and a locked position for maintaining the fabric roll in a fixed position while rotating on the belt drive. Preferably, the clamps are pneumatically controlled and open when the loader arms 16 are in a lowered position and close when a roll is placed onto the unwinding cradle.
Fabric protector shields 62 are placed over the loader arms 54 once the fabric roll 11 is locked into the second position, as illustrated in FIG. 3. The fabric protector shields 62 have a generally inverted U-shaped cross section to fit over the loader arms to protect the fabric roll from being damaged during the unwinding process. The fabric protector shields 62 are removable for loading and unloading the fabric roll.
The guide frame 12 provides a path for guiding the fabric web after it is unrolled from the fabric roll 11. In one embodiment, the guide frame 12 provides for the fabric web to be guided overhead and away from the belt drive area. Braces 20 may be used for supporting the guide frame structure.
An inspection station is located downstream of the belt drive and includes a camera 22 and backlight 24, as illustrated in FIG. 1. The fabric web passes between the camera 22 and backlight 24 to provide for an inspection for defects and other inconsistencies in the fabric web. Camera 22 is equipped for sensing defects measuring as small as about a one-quarter inch hole or needle cut at a rate of about 320 ypm. The backlight 24 may include a high-frequency light source for illuminating the fabric web to enhance the accuracy and performance of the camera 22. Further details of this arrangement are disclosed in co-pending U.S. patent application Ser. No. 09/259,461, filed Mar. 1, 1999, which is hereby incorporated by reference in its entirety.
A tension drive 26 is positioned downstream of the belt drive 14 for maintaining tension on the fabric web after it is unrolled from the fabric roll. The tension drive includes rollers 30 for further pulling the fabric web away from the belt drive and downstream to further processing. Rollers 30 are preferably of a width greater than the fabric web width and include friction material to pull the fabric web as it passes over the rollers. The rollers 30 are driven in a first direction for moving fabric web away from the belt drive and a second direction which is opposite and moves fabric web towards the belt drive. Anti-backlash arms 32 may be positioned adjacent to the rollers to prevent the fabric web from becoming tangled on the rollers during direction changes.
In use, a fabric roll 11 is placed at the first end of the loader device 16 in a first position, as illustrated in FIG. 4. At this position, the fabric roll shaft 13 is positioned on the ridges 60 of the loader arms 54 with the fabric roll extending between the arms. The fabric roll 11 can be weighed by load cell 66. In one embodiment, the large fabric roll letoff device is capable of handling fabric roll in excess of about 450 lbs. The actuator 56 may then raise the first end of the arms 54 to help move the fabric roll from the first position to the second position on the unwinding cradle 44 positioning the roll over the belt drive 14. Once positioned on the belt drive, the fabric roll is locked in place by the clamps 64 and fabric protector shields 62 are placed over the loader arms to center the fabric roll on the belt drive and also protect the edges of the fabric roll from becoming damaged by rubbing against the loader arms during the batching process.
The fabric web is fed through the guide frame and tension drives 26 downstream of the belt drive 14. The belt drive is then initiated resulting in the belt rotating along the drive roller 36, idle roller 40 and tension roller 42. The fabric roll 11, which is placed on the belt drive 14, rotates thereby unwinding the fabric web off the roll. As the diameter or the roll 11 decreases, the tension roller 42 extends outward via the arm 50 to maintain the constant tension on the belt as illustrated in FIG. 1. The belt rotates at a constant velocity resulting in the surface speed of the fabric roll to vary depending upon the diameter of the roll. Once the fabric web is completely removed from the roll, a sensor 72 positioned in proximity to the belt drive 15, as illustrated in FIG. 2, will shutoff the belt drive and tension drive. The operator may then unload the empty fabric roll shaft 13 from the belt drive and repeat the process.
The fabric web removed from the fabric roll 11 passes through an inspection station and further through tension rollers 30 located downstream of the belt drive. The fabric web passes between illuminated backlight 24 and camera 22 to inspect for defects within the fabric web. Upon finding a defect, the position of the defect will be registered in the control system 80 and the fabric web will move a fixed distance downstream of the inspection station at which point the tension rollers 30 will play the section of the fabric web for removal or marking by the operator. By way of example, FIG. 1 illustrates a section of fabric web 90 being played down from the overhead guide frame 12 to the operator area where the defect can be removed from the fabric web and then re-sewn by sewing machine 70. The fabric web will then be pulled back by the tension rollers 30 and the process reinitiated.
Certain modifications and improvements will occur to those skilled in the art upon a reading of the foregoing description. It should be understood that all such modifications and improvements have been deleted herein for the sake of conciseness and readability but are properly within the scope of the following claims.
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A fabric roll letoff for unrolling and inspecting a fabric roll. The apparatus includes: a continuous belt for supporting the fabric roll. A drive system for rotates the belt to letoff the fabric web. The drive system includes a drive roller; a idle roller; and a tension roller. The continuous belt rotates the fabric roll to unroll the fabric web at a constant velocity for subsequent processing. In the preferred embodiment, a pair of unloader arms is connected to the belt drive for receiving the fabric roll and for positioning the fabric roll onto the belt drive. Also, in the preferred embodiment, a guide frame is positioned downstream from the belt drive for directing the fabric web through an inspection area.
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RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. provisional application Ser. No. 60/713,023 filed on Aug. 31, 2005 which is incorporated herein by reference in its entirety.
FIELD OF THE INVENTION
[0002] The present invention relates to a system for eliminating the possibility of a static discharge during the refill of high pressure fuel storage tanks in hydrogen fuel cell powered vehicles.
BACKGROUND OF THE INVENTION
[0003] When hydrogen is used as a fuel in motor vehicles, a hydrogen fuel depot infrastructure for refueling must also be developed. Typically, present practice is that fuel is stored in on board tanks maintained at a maximum pressure in the range of about 5000 psi for hydrogen, and higher pressures in the range of about 10,000 psi or more are likely to be utilized in the future as the use of hydrogen becomes more widespread. During driving, a static charge may build up on the vehicle chassis. When the vehicle stops, the charge is usually dissipated to ground through the vehicle's tires; however, the rate of dissipation of the charge through the vehicle tires varies depending on the resistance of the tires and the resistance of the surface on which the vehicle is parked or stopped. If, at a refueling station or depot, the vehicle static charge energy is above a minimum threshold energy level that can cause the spark ignition of hydrogen gas, then it is unsafe to refuel the vehicle through the refill conduit connecting the fuel depot gas outlet and the vehicle tank inlet. If hydrogen were to leak at the depot refill nozzle or at the vehicle receptacle, a spark may occur when the refill nozzle is connected to the vehicle receptacle, which could potentially ignite the hydrogen. A conventional solution mitigates the static discharge problem, by manually connecting a grounding cable to the vehicle before refueling to avoid the potential for a spark to occur.
OBJECTS OF THE INVENTION
[0004] It is an object of the present invention to isolate any charge potential that could be present on the vehicle chassis from the refueling receptacle, and thus reduce the possibility of a static discharge during the refill of high pressure storage tanks in hydrogen fuel cell powered vehicles at a retail outlet fueling depot.
SUMMARY OF THE INVENTION
[0005] The invention is described more fully in the following description of the preferred embodiment considered in view of the drawings in which:
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0006] FIG. 1A is a diagram showing typical static potential between the vehicle, the fuel depot and ground at a refueling station. FIG. 1B is a schematic diagram showing the electrical resistance and capacitance of the vehicle, earth and refueling pump circuit equivalent to the representation of FIG. 1A . FIG. 1C is an electrical schematic diagram representing the circuit of FIG. 1B .
[0007] FIG. 2 shows a cross section side view demonstrating the principles of the insulating properties of the invention showing a vehicle fuel refilling receptacle with reference to the vehicle tank inlet on a hydrogen powered vehicle.
[0008] FIG. 2A , FIG. 2B , FIG. 2C , FIG. 2D and FIG. 2E depict cross section side views of embodiments of the invention.
[0009] FIG. 3 is a cross section side view of an alternative configuration of a vehicle fuel receptacle applying the insulating principles of the invention.
[0010] FIG. 3A and FIG. 3B are cross section side views of further embodiments of the alternate configuration of the invention shown in FIG. 3 .
DETAILED DESCRIPTION OF THE INVENTION
[0011] The invention electrically isolates the refueling receptacle from the vehicle chassis. The electrically isolated receptacle is engageable with a refueling nozzle from the station depot side. The vehicle receptacle includes electrically insulating media to prevent electrical contact from the refueling nozzle to the vehicle chassis and gas tank. With reference to the description herein, the nozzle is an external fuel dispensing device that is connected to the receptacle; in describing the invention, “nozzle” refers to the station nozzle and the application should be so read contextually in the event of any ambiguity.
[0012] FIG. 1A depicts a typical static potential between the vehicle, the fuel depot and ground at a refueling station. In FIG. 1A , the rear of the vehicle is shown as 1 having right rear tire 2 and left rear tire 3 . Hydrogen gas fuel tank 4 is interconnected through fuel conduit 6 to gas tank inlet 5 . Ground [earth] is shown at 20 . Refuel depot pump 10 is installed on base 11 and includes conduit 12 and nozzle 15 for interconnection with the fuel tank inlet 5 . Electrical charges in the ambient vehicle/fuel depot environment are respectively shown as positive, +, and negative, −. FIG. 1B shows the electrical circuit equivalent wherein C A indicates capacitance between fuel cell vehicle 1 and earth 20 and C Z indicates capacitance between fuel cell vehicle 1 and refueling pump 10 and earth 20 . R 1 indicates resistance between refueling pump 10 and ground or earth. As shown in FIG. 1A and FIG. 1B , a static charge builds up on the vehicle chassis during driving. When the vehicle stops, the rate of dissipation of the charge through the vehicle tires varies depending on the resistance of the tires and the resistance of the surface on which the vehicle is parked or stopped. If, at a refueling station or depot, the vehicle static charge potential stored in the capacitor elements, C A and C Z of the circuit is above a minimum threshold energy level exceeding the limit of R 1 , a spark may occur that can cause the ignition of hydrogen gas. See FIG. 1C .
EXAMPLE A
[0013] FIG. 2 is a longitudinal side cross section view of an embodiment of the invention showing the exterior side of the vehicle receptacle (that joins with the station nozzle) 100 and the vehicle receptacle assembly 200 through which the fuel conduit is joined to the vehicle's hydrogen storage tanks in accordance with the invention. In the drawings of the FIG. 2 and FIG. 3 series shown, a frontal lateral cross section of the cylindrical elements involved is evident from the side views depicted and their respective explanations. Fuel depot receptacle connector 100 is conventional and includes interlocking means (not shown) to securely engage the pump nozzle with the fuel inlet of the vehicle tank. The interior side of the vehicle receptacle 200 leads from the receptacle through a conduit 250 to the vehicle fuel storage tank (not shown). The vehicle receptacle 200 is electrically isolated from both the vehicle body 400 and the fuel tank system 250 . The receptacle comprises vehicle body interior section 201 and mating vehicle body exterior section having integral interior extending element 202 i sandwiching the section of the vehicle body 400 upon which the receptacle is mounted. Receptacle mating elements, element 201 , and element 202 , are affixed to the vehicle body by a plurality of fasteners insulated from contact with the vehicle body. As shown in the cross section, fastener 203 is insulated by grommets 204 and 205 ; fastener 206 is insulated by grommets 207 and 208 . A gasket or laminate layer of insulating material 220 at least coextensive with the facing receptacle elements is also secured by the fasteners and insulates the receptacle surface from the vehicle body. Insulating o-ring or gasket 210 prevents contact of any extending stem portion, alternatively of either of the station nozzle or the vehicle receptacle exterior section, and/or both, with the interior portion of the vehicle tank receptacle 201 . In this manner, the flow path of fuel in the station conduit from the nozzle 100 to the conduit for the vehicle tank system 250 is electrically insulated from the vehicle body and vehicle tank system.
[0014] In Example A, a vehicle fuel receptacle is isolated from a vehicle body and tank system while allowing a secure conduit for high pressure fuel gas flow from the nozzle to the tank. An exterior vehicle tank inlet receptacle is engageable with the refueling nozzle; the receptacle has a vehicle body interior flange and a mating vehicle body exterior flange with a cylindrical extending section concentric with the interior flange leading to the fuel tank. The receptacle flanges are disposed to and fasten the section of the vehicle body upon which the receptacle is mounted; an insulating gasket is essentially coextensive with the exterior flange and the vehicle body. Concentrically extending sections of the flanges and gasket are secured with respect to the vehicle body by electrically non-conducting fasteners, or equivalently, by electrically conductive fasteners insulated from the flanges and vehicle body by insulating grommets. An o-ring may be disposed within the interior extending section of the interior flange adjacent the end of the concentric section of the exterior flange that extends within the interior flange. In an example, an insulating sleeve is disposed around the outer surface of the extending interior section of the exterior flange; the sleeve may extend beyond the end of the extending interior section of the exterior flange and fold inwardly at the end thereof to enhance insulating qualities.
[0015] In embodiments, a recessed o-ring is disposed within the interior extending section of the interior flange between the sleeve and the extending section of the interior flange or a pair of recessed o-rings, a first o-ring disposed within the interior extending section of the interior flange, and a second o-ring disposed within the interior extending section of the exterior flange, may be disposed within the flange sections such that the o-rings sandwich the sleeve. Based on design factors, one o-ring may be formed from a metal and the second o-ring may be formed from an electrically insulating material. The sleeve for the extending section of the exterior flange may be a cylindrical metallic collar having interior and outer surfaces covered with an electrical insulator and the insulator may comprises a surface coating of a polymeric material. O-rings may be longitudinally offset from, or aligned with, one another. The gaskets and insulator materials are preferably a nylon as described below.
[0016] The object of the invention is to isolate and minimize any electrical charge that could be present on the vehicle chassis and prevent the creation of a spark when the station nozzle is connected to the vehicle receptacle. Because the station nozzle is electrically grounded, if the receptacle on the vehicle is directly connected to the vehicle chassis, and the chassis still holds a static electrical charge, a spark can occur across the air gap as the nozzle approaches the receptacle while connecting the two during the refueling process. This spark could potentially ignite a hydrogen/air mixture that could be present due to a leak or other factors in the nozzle or receptacle areas. Normally the vehicle is grounded via a grounding cable or thru the vehicle tires before the nozzle is connected to the receptacle. However, the user may forget to or purposely avoid connecting the grounding cable prior to connecting the nozzle, or the fueling pad surface may have too high a resistance to adequately ground through the tires. When the receptacle is electrically isolated from the vehicle chassis, then there is little or no possibility for the electrical charge on the vehicle chassis to gap across to the nozzle and create a spark that may potentially ignite the hydrogen. The invention thus creates a safer refueling environment for the user and can be utilized as a secondary layer of protection in case the primary protection, dissipation of static electrical charge via grounding to earth, fails. In the discussion of the embodiments, reference numerals for elements of the vehicle receptacle and the fuel station connector to the receptacle that are initially identified in prior drawings may be omitted, both to avoid redundancy and for purposes of clarity in explaining the invention; however, their presence is evident in context.
[0017] FIG. 2A shows an embodiment in which a high strength engineering plastic material with good durability and electrical isolation properties, such as a nylon electrical insulating material, is molded into a shape 222 that fits around and/or is bonded to the outer surface of the conductive inner sleeve section 202 of the outer part of the receptacle. As used herein, “nylon” refers to the synthetic polymer engineering material, nylon, and other suitable, or equivalent, high strength engineering plastic materials with electrical isolation properties, such high performance polyamides and other polymeric electrical insulating materials having properties of toughness, durability and wear resistance, with mechanical performance characteristics over a wide temperature range suitable for use in high pressure fuel delivery systems for automotive applications.
[0018] An embodiment is shown in FIG. 2B , wherein a nylon engineering plastic material, is molded into a shape 223 that fits around and/or is bonded to the outer surface of the inner sleeve section 202 of the outer part of the vehicle receptacle. Shape 223 provides an insulating mechanism sealed on the inner surface and which is secondarily sealed in the assembly by an o-ring 224 interposed between the extending segment of the receptacle section 202 and the nylon insulating shape 223 . Assembly o-ring 210 is also shown.
[0019] FIG. 2C shows an embodiment wherein the nylon electrically insulating engineering plastic material 225 is molded around a tubular metal collar 226 to form an insulating sleeve, which is then bonded to the inner male receptacle section 202 i of the outer part 202 of the vehicle receptacle. The collar includes a folded over extending end section proximate the terminal end of receptacle section 202 i. Primary sealing occurs on the inner surface by bonding of the inner surface of the collar 226 to section 202 i; secondary sealing results from pressures exerted by insulating o-ring 210 in part 201 and metallic o-ring 227 recessed in section 202 i. The polymeric insulating o-rings and gaskets shown include elements formed from nylon and other high strength engineering plastic materials having properties of toughness, durability, wear resistance, and mechanical performance over a wide temperature range, suitable for use in high pressure fuel delivery systems in automotive applications.
[0020] FIG. 2D shows an embodiment wherein the electrically insulating nylon material 225 is molded around a metal collar 226 to form an insulating sleeve, which slides over and correspondingly engages the inner male receptacle sleeve section 202 i of the outer part of the vehicle receptacle, extending beyond the terminal end thereof. Gas sealing occurs on the sandwich disposition of the insulator, namely collar 226 surrounded by plastic 225 between insulating o-ring 210 recessed in section 201 supplemental o-ring 228 recessed in section 202 i.
[0021] FIG. 2E shows an embodiment wherein the electrically insulating engineering plastic material 225 is molded around a metal collar 226 to form an insulating sleeve, which slides over and engages with the inner male receptacle sleeve section 202 of the outer part of the vehicle receptacle. Gas sealing occurs as a result of circular forces generated by the sandwich disposition of the insulator, namely collar 226 surrounded by insulating plastic coating 225 , between o-ring 231 recessed in section 202 i and o-ring 232 recessed in section 201 .
EXAMPLE B
[0022] FIG. 3 is a side cross section view of another embodiment of the invention using a series of collinearly aligned gaskets and receptacle elements insulating the vehicle fuel receptacle from the vehicle body. In FIG. 3 the exterior side of the receptacle that joins with the station nozzle 100 and the interior side of the receptacle 300 which is joined to the vehicle's hydrogen storage tank system in accordance with the invention are shown. Fuel nozzle receptacle 100 is conventional and includes interlocking means (not shown) to securely engage the pump nozzle with the fuel inlet of the vehicle tank. The interior side of the vehicle receptacle 300 leads from the nozzle through a conduit 350 to the vehicle fuel storage tank (not shown). The vehicle nozzle 100 is electrically isolated from both the vehicle body 400 and the fuel tank conduit system 350 . The receptacle comprises collinearly aligned elements 301 a, which includes a flange section 302 for securing the receptacle to the vehicle exterior body panel 400 . Separating flange 302 from the vehicle body 400 is an insulating gasket 310 . The flange 302 and gasket insulator 310 are fastened to the vehicle body by one or more fasteners such as 303 , insulated from the vehicle body and receptacle by grommets 304 and 305 , and 306 , insulated from the vehicle body and receptacle by grommets 307 and 308 . Exterior receptacle component 302 includes elements 301 a and 301 b separated from each other and insulated from each other by electrically insulating gasket 320 maintained in a fixed alignment by fasteners such as fastener 311 , insulated from section 301 a and section 301 b, and fastener 314 , insulated from section 301 a and section 301 b by grommets 315 and 316 . In this manner, insulator 310 (held in place by the insulated fasteners) electrically isolates the vehicle body 400 from section 301 a of the receptacle and insulator 320 (held in place by the insulated fasteners) electrically isolates the vehicle receptacle nozzle 100 from the vehicle tank system 250 . Fuel thus flows from the nozzle into the vehicle tank through an electrically isolated pathway 350 from the fuel pump to the vehicle tank.
[0023] In this example, the receptacle comprises a vehicle body flange having an exterior flange section disposed with respect to the vehicle body and an interior section extending from the exterior section toward the vehicle body interior. An insulating gasket is disposed between the exterior flange and the vehicle body in a sandwich relationship and a terminal is plate affixed to the interior extending end section of the vehicle body flange insulated by a gasket disposed between the end section of the vehicle body flange and the terminal plate. As in the above example, the flange, gaskets and plate are collinearly concentrically aligned such that an unobstructed fuel conduit is provided for high pressure hydrogen gas (or compressed natural gas). The exterior flange is insulated from the vehicle body by a flange in the gasket providing a central collar section extending over the inward extending section of the exterior flange from the vehicle body exterior. Fasteners securing the assembly, electrically insulate the receptacle from the vehicle body. In the embodiment shown, the plate gasket comprises a metal washer coated with an electrically insulating material and the plate gasket may be disposed between the aligned or offset o-rings. A reverse flange may be intrinsically formed at the interior facing end of the extending section of the exterior flange to receive a fastener for securing the plate with the insulator therebetween.
[0024] In FIG. 3A , a nylon wrapping collar or sleeve 331 is molded around a disk 332 , which may be formed as a steel washer, that serves as structural support for high stresses in the filling system, and the gas sealing occurs by o-ring 333 recessed in the inner section 301 b of the receptacle and o-ring 334 recessed in the outer section 301 a of the receptacle.
[0025] In FIG. 3B , an assembly is shown in which bolt 351 insulated by nylon grommet 353 and bolt 352 insulated by nylon grommet 351 and 354 secures cap 301 b securely in position with the extending part 301 a of the interior flange. Between cap 301 and flange element 301 b, an insulating washer 356 is provided. The washer comprises a high strength engineering nylon molded around a central steel disk that serves as structural support for high stresses. Central metal element 356 is coated or molded with insulating material 356 c. O-rings 356 and 357 recessed respectively in the facing ends of sections 301 a and 301 b provide the gas sealing.
[0026] The mechanism of the invention thus isolates electrical charge that is possibly present on the vehicle chassis that could create a spark when the station nozzle is connected to the vehicle receptacle. The possibility is reduced that a spark could potentially ignite a hydrogen/air mixture that might occur due to a leak in the nozzle or receptacle areas. When the receptacle is electrically isolated from the vehicle chassis, the possibility for the electrical charge on the vehicle chassis to gap across to the nozzle and create a spark resulting in the potential ignition of hydrogen is reduced. The invention thus creates a safer refueling environment for the user and can be utilized as a secondary layer of protection in the event that the primary protection—dissipation of static electrical charge via grounding to earth—fails.
[0027] Having described the invention in detail, those skilled in the art will appreciate that, given the present description, modifications may be made to the invention without departing from the spirit of the inventive concept herein described. Therefore, it is not intended that the scope of the invention be limited to the specific and preferred embodiments illustrated and described. Rather, it is intended that the scope of the invention be determined by the appended claims.
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Apparatus for electrically isolating interconnecting station nozzle and vehicle receptacle components during the refueling of high pressure gas into a vehicle tank comprising an electrically isolated vehicle tank inlet receptacle engageable with a refueling nozzle wherein the receptacle includes an assembly of mutually engageable electrically insulating media in conjunction with the vehicle receptacle mount to prevent electrical contact from the refueling nozzle to the vehicle chassis and gas tank in the refueling gas flow conduit system.
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CLAIM OF PRIORITY
Priority is claimed on a Provisional application Ser. No. 60/096,432 deposited in the United States Patent and Trademark Office Aug. 13, 1998 by Express Mail, Label No. EL140120622US.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to the field of high frequency integrated circuits.
2. Description of the Related Art
High frequency microwave-range integrated circuits (ICs) based on gallium arsenide (GaAs) are known. Lower frequency-range integrated circuits which include components fabricated on silicon (Si) are also known. It would be highly desirable to extend the high frequency performance capacity of GaAs-based ICs to Si-based ICs, using materials and equipment which are adaptations of those whose use is well established in silicon processing.
Silicon technology has been the foundation of the microelectronics industry, but in attempts to extend the more mature silicon technology to the integration of high frequency microwave components such as coplanar transmission lines and inductors, the inherent limitation of the resistivity of silicon, which is maximal in pure silicon, has been a barrier to fabricating Si-based devices which are technically noncompetitive with GaAs in the microwave range. For example, loss at about 10 GHz on silicon is approximately 20 times that on GaAs; GaAs-based microwave structures have the low loss tangent that would be desirable to achieve in manufacturable Si-based structures. Manufacturability requires processes and results that are stable, predictable, reproducible and cost effective. High frequency devices based on GaAs are relatively more expensive to fabricate than are lower frequency devices based on Si, but lower frequency devices based on Si can be fabricated by processes that produce stable, predictable and reproducible results.
U.S. Pat. No. 5,528,209 issued Jun. 18, 1996 to Mcdonald et al. describes a silicon-based high frequency monolithic structure in which the high frequency transmission lines are fabricated by electroplating gold. Gold plating may give rise to problems such as cost, added process steps to create barriers to electromigration of gold into copper and handling and disposal of the gold electroplating baths and rinses. The present invention does not include gold processing. Rather, wet electroprocessing is avoided by using sputter deposition and sputter cleaning and ashing. The '209 patent describes via fabrication by reactive ion etching (RIE). In the present invention, via (through-hole) photolithography, including wet or reactive ion etching (RIE) is avoided in fabricating internal vias by using laser ablation, a process which provides superior control of the critical via dimension of slope angle. The '209 patent uses benzocyclobutene (BCB) resin, which was found not to laser well for the purposes of the present invention. The polyimide (PI) used in the present invention has the advantages of lasering well, low dielectric constant, low moisture absorbency, ability to be applied and cured in a layer up to at least 15 microns thick, and ability to withstand the temperature required to solder or wire bond the completed device without cracking. A paper presented at the 1995 IEEE conference, “High Performance Microwave Elements for SiGe MMICs” by Michael Case et al. describes a Si-based microwave device using BCB, a resinous composition used in the prepreg art, as the dielectric material. BCB was found to be unsuitable for the processing of the present invention, particularly with respect to laser processing.
An article by Anthony Cataldo and Ron Wilson beginning on page 1 in the Electronic Engineering Times dated Jan. 26, 1988 describes some of the IBM activity in the area of SiGe-based RF ICs.
“Low-Loss Microwave Transmission Lines and Inductors Implemented in a Manufacturable Si/SiGe HBT Process” by David C. Laney, Lawrence E. Larson, John Malinowski, David Harame, Seshu Subanna, Rich Volant, Michael Case and Paul Chan was orally presented in September, 1998 at the BCTM meeting in Minnesota. In it are described experimental results of measurements made for square planar inductors and microstrip transmission lines for standard Si VLSI structures having CuAl metallization and thick polyimide dielectric. The work indicates the manufacturability in Si VLSI technology of these lines and inductors and predicts their use in high performance, low cost Si-based 5-10 GHz MMICs in the future.
U.S. Pat. No. 4,830,706 issued May 16, 1989 to Ronald S. Horwath et al. describes one method, not involving laser, in which slope-walled vias with rounded corners are fabricated by finally curing a resinous insulating material in which, after a preliminary partial cure, the via walls had been conventionally straight and corners square. The patent describes problems associated with straight-walled vias and benefits of slope-walled vias and rounding at the intersection of via wall and planar surface.
None of the references anticipates the process and article of manufacture of the present invention.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the invention to provide a silicon-based integrated circuit structure having the high frequency performance characteristic of GaAs-based structures.
It is a further object of the invention to provide a high frequency silicon-based integrated circuit structure having the performance characteristics of high frequency GaAs-based structures, in which the processing steps and equipment employed are compatible with the processing steps and equipment employed in existing silicon technology processing, and for which the overall cost of manufacture is market competitive.
These and other objects are accomplished in the present invention, wherein a silicon-based high frequency integrated circuit structure includes a dielectric resin separating the signal lines. The substrate is typical of that used in Si-based back-end-of-line (BEOL) IC fabrication, metal deposition in the fabrication of elements such as inductors, transmission lines and capacitors is efficiently performed by vacuum deposition of non-precious metals, and via fabrication is performed by laser ablation rather than by wet processing or RIE in thick polyimide dielectric of a type used also in non-microwave applications Use of the laser enables the fabrication of predictably and reproducibly smooth and even slope-walled vias on which continuous metallization can be deposited despite the thickness of the dielectric.
The number of processing steps in the present invention is reduced compared to the art, and the number of wet processing steps is minimized. The resulting silicon-based modular structure can incorporate numerous integrated high quality passive microwave lines and components and a ground plane fabricated in BEOL metallurgy. Structures can be built with or without a ground plane, depending upon the application. It is high frequency performance competitive with GaAs-based structures and is cost competitive with silicon-based structures. It is useful in applications and markets such as, for example, tuned matching networks, reactive loading, power splitters, transistors, inductors, transmission lines, resonators, couplers, analog, mixed signal, RF, communications, impedance transformers, monolithic microwave integrated circuit (MMIC) interconnects and like microwave elements.
Advantages include the provision in transmission line structures of low loss compared to BEOL Si-based structures; self-resonant frequency beyond GaAs while showing significant Q factor improvement compared to BEOL; Si enabling process for RADAR (20 GHz) applications which otherwise cannot have integrated passive elements; and provision of high level of integration (BiCMOS) for GaAs. The modularity of the structure of the present invention permits the addition of high frequency microwave receive/transmit capability to be mounted to existing products on Si, SiGe, GaAs and other semiconductor substrates.
In one embodiment of the present invention, a SiGe wafer is processed normally through solid conductive terminal via formation. Polyimide (PI) 5811, a product of E.I.Dupont et Nemours and Co. of Delaware, in an amount sufficient to result in a cured layer of nominally 15 microns, is spun on and cured on the wafer at about 400 degrees C. Laser ablation is performed on the cured PI down to each terminal stud via to create a rounded slope-walled via of about 62 degrees. Between the SiGe and the polyimide is TV dielectric, which comprises a silicon oxide/nitride sandwich layer. Ashing the ablated via in an oxygen-containing plasma by RIE, optionally followed by sputter etching, assures the removal from the slope-walled via of any debris left behind by the laser. A via at its narrowest width is about 10 microns in diameter. Next a top metallization layer about 2 microns to about 2.5 microns thick of AlCu is sputter deposited over the PI, including along the sloped walls and the bottom of the terminal stud via, for electrical communication between transmission lines. The AlCu metallurgy can be about 0.2% to about 5.0% by weight of Cu. After photolithography a top metal etch shapes the transmission lines. A second layer of resist is spun onto the structure and cured to a thickness of about 3 microns and “ball vias” are fabricated to provide electrical communication with the transmission lines at predetermined locations. Whereas the layer of thick polyimide need not be photoactive because the topography is shaped by laser rather than by photolithography, the second layer of polyimide can be photoactive since it is thin enough to be patterned photolithographically rather than by laser. PbSn solder is applied at the ball via, reflowed and cooled to form a ball of solder for subsequent controlled collapse chip connection (C 4 ) to a customer-defined package. Wire bonding is an alternate to C 4 bonding.
In order to facilitate further understanding of the present invention, reference is made to the A following detailed description taken in conjunction with the drawings:
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A, 1 B, 1 C, 1 D and 1 E together comprise a series drawings illustrating, in cross section, major stages in the preparation of the structure of the present invention.
FIG. 2 is a cross-sectional view of a completed structure of the present invention including multiple terminal stud vias and ball vias.
FIG. 3A is the equation used to calculate the predicted values of impedance for transmission lines of each of three widths when the dielectric material on which the lines are disposed is 13 microns thick and has an effective dielectric constant of 2.8. The result of this calculation is shown in FIG. 3B along with the average measured impedance for each width.
FIG. 4 shows the variation in effective dielectric constant as a function of frequency for each of the three measured line widths.
FIG. 5 shows the variation in loss in dB per mm as a function of frequency for each of the three measured line widths.
FIG. 6 shows the variation in loss in dB per wavelength as a function of frequency for each of the three measured line widths.
FIG. 7 shows the variation in Q (quality) factor as a function of frequency for each of the three measured line widths.
FIG. 8A is the equation used to calculate maximum impedance shown in FIG. 8B as a function of frequency for each of the three measured line widths.
FIG. 9 shows the impedance of a line width of 27 microns as a function of frequency.
FIG. 10 shows the variation in effective dielectric constant of a line width of 27 microns as a function of frequency.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Fabrication and Structure
FIG. 1A shows a SiGe wafer substrate ( 10 ) on which a ground plane ( 17 ) has been prepared, including terminal stud ( 18 ). A thick layer of dielectric material ( 11 ), preferably either polyimide 5811 or 5878, both products of E.I. Dupont et Nemours and Co. of Delaware is disposed on the surface of wafer substrate ( 10 ) which includes terminal stud ( 18 ). The dielectric has been applied and cured, i.e. has been heated at about 400 degrees C. in order to evaporate solvent and thermally cross link the resinous PI dielectric. The final thickness of the cured thick polyimide dielectric ( 11 ), is about 12 microns to about 15 microns depending on the functional requirement of the ultimate device, is nearly an order of magnitude greater than that conventionally used in silicon-based IC technology. In such a thick layer of PI, wet photolithographic development of precision vias of such narrow width would be impractical or impossible to manufacture. The thick dielectric layer ( 11 ) is necessary to prevent signal loss between the microwave transmission lines formed in metallization layer ( 20 ) shown in FIG. 1 C and the wafer substrate ( 10 ) and to assure high quality (Q) inductors at high RF frequencies.
Preferably, the liquid resinous PI dielectric is spun on in one layer and cured to achieve the desired thickness; the slower the spin speed the thicker the layer. Alternatively, the dielectric can be built up to the desired thickness by more than one coat with intermediate curing steps. If the alternative technique is used, the additional step of oxygen ashing followed by applying an adhesion promoter, such as hexamethyl disulfoxide (HMDS) or A1100, an organofunctional silane primer which is a product of Union Carbide, is performed after each cure and prior to the next resin layer application. A Drytek Quad RIE tool from Lam Research of CA was used for ashing, using the following parameters: 200 W power, 50 sccm flow, and 300 mT pressure for a time of 30 seconds/wafer. In the curing process, the temperature is ramped up at about 5 degrees C./minute in a nitrogen atmosphere in an IR oven to a final cure temperature of up to about 400 degrees C. In a 2-step cure process, the first coat is cured up to about 220 degrees C. and the second coat up to about 385 degrees C.
In FIG. 1B is shown a cured PI dielectric layer ( 11 ) that has been laser ablated, oxygen-ashed and sputter cleaned, creating a clean via opening ( 12 ) which extends to terminal stud ( 18 ) and which, due to the laser ablation, has walls ( 13 ) which are sloped, preferably about 62 degrees, to receive a continuous metallization layer ( 20 ), shown in FIG. 1 C. Each via opening ( 12 ) includes rounded edges ( 21 ), also shown in FIG. 1C, where the wall of the slope-walled stud via ( 12 ) intersects with the planar surface of the cured thick PI ( 11 ). Laser ablation through this thickness of PI produces precision vias which can be a narrow as about 10 microns to about 25 microns at the narrowest width. Although the laser ablated walls ( 13 ) of the vias are preferably angled at about 62 degrees, it should be noted that ablated walls which are angled plus or minus about 15% of 62 degrees between about 52 degrees and about 71 degrees also enable, to a somewhat lesser extent, the fabrication of narrow width precision vias having continuous metallization and rounded edges ( 21 ).
The laser removes sufficient PI to form slope-walled via ( 12 ) without damaging the underlying metal of the terminal stud ( 18 ). The laser ablation tool used is a Tamarack model 290, manufactured by Tamarack Scientific Co. of Anaheim, Calif. An excimer laser, medium of xenon chloride, is generated at a wavelength of 308 nm, 300 Hz, 400 pulses/mm2 and 200 mJ/cm2. Any remaining debris from the ablation can be removed by oxygen ashing, a 400 pulse/mm2 process which removes less dielectric from the exposed surface of the cured PI dielectric layer ( 11 ) which surrounds slope-walled via ( 12 ) and results in minimal undercut and substantially uniform thickness of the PI ( 11 ). In a Drytek Quad RIE tool, a product of Lam Research of California, ashing is performed at a power of 200 Watts, a flow rate of 50 sccm and a pressure of 300 mT. A sputter preclean just prior to sputtering the continuous metallization layer ( 20 ) removes any further residue within the slope-walled via ( 12 ).
A blanket sputter deposition of AlCu is then performed to produce the desired thickness for the metallization layer ( 20 ), normally about 1 to about 5 microns, such as about 2.5 microns. The metallization layer ( 20 ) is then ready to be defined by photolithography and etched into high frequency transmission lines or fabricated into other microwave elements. A solution by volume of 1 part nitric acid: 3 parts deionized water: 16 parts phosphoric acid, the acids being in “off the shelf” concentrations, plus a few drops per gallon of a nonionic surfactant, such as Igepal from Ashland Chemical, is used to etch the AlCu lines. The etchant gives adequate control over fine line width and spacing between lines, which affect loss and impedance, respectively, in the high frequency structure. Improved resolution over wet etch was demonstrated for 4% AlCu and for 0.5% AlCu using a chlorine-based dry RIE. A sputter deposition of antireflective TiN (not shown) on the exposed surface of the metallization layer ( 20 ) helps to effect a uniform lithographic process. About 320 Angstroms to about 600 Angstroms of TiN is sufficient. Any residue remaining after the formation of the transmission lines is removed with hot hydrogen peroxide.
At this point a second dielectric layer of polyimide 5811, shown as ( 14 ) in FIG. 1D, is applied to the surface and cured at about 400 degrees C. to result in a thickness of about 3 to about 4 microns, and ball via ( 15 ), shown in FIG. 1E, is exposed and developed therein down to the transmission line fabricated in metallization layer ( 20 ). In this step laser processing could be used as an alternative to wet photolithography. PbSn solder is applied to ball via ( 15 ), where it is reflowed and cooled into a ball shape ( 19 ). Wire bonding is an alternate procedure to C 4 bonding. The structure is now ready for mounting by means of controlled collapse chip connection (C 4 ) at solder ball ( 19 ) onto a customer-defined package.
The FIG. 2 cross-section representation of a structure of the present invention indicates that normally there will be a more complex pattern fabricated on a substrate than shown and discussed for FIGS. 1A-1E above for merely one example of each feature.
Measurements
Various measurements were made in order to determine performance characteristics of transmission lines of various lengths and widths disposed over a thick layer of polyimide. Unless otherwise indicated, all measurements were performed on a signal conductor comprised of 2.5 micron thick 4%Cu CuAl disposed over a cured layer of polyimide 5811 having a nominal thickness of about 13 microns and an effective dielectric constant (Eeff) equal to 2.8, which was in turn disposed over a Si substrate coated with a ground plane of about 1.5 microns of about AlCu 4%. Measurements were conducted on 370 micron and on 3362 micron lengths of signal conductor, each having widths of 15 microns and of 27 microns, and on lengths of 171 microns and 1668 microns, each having a width of 8.5 microns.
Two-port S-parameter data were collected and the results compared to the expected values. MatLab, a software program which is a product of MatLab of Massachusetts, was used to calculate the transmission line data for Zo, Eeff and dB (loss) from the measured S-parameter data, not including contributions from contact pads and probes. The data was transferred to a personal computer by means of a general purpose interface board (GPIB). HP Tester 8570, a product of Hewlett-Packard of Oregon, as well as Cascade 100 micron pitch probes, SOLT calibration and Alessi wafer station were used to collect data. The data analysis procedure comprised a method suggested by Professor H. J. Orchard of the University of California at Los Angeles (UCLA), and set forth in FIGS. 13A-13D.
The expected values for impedance (Zo) were calculated using the equation set forth in FIG. 3 A and are plotted as a function of line width in FIG. 3 B. The three points located slightly above the plot of expected values are measured values. The measured values are within about 10% of the expected values. High impedance is favored by narrower lines.
The variation of Eeff as a function of frequency is shown in FIG. 4 for each measured line width. The values of Eeff are rather consistent for all tested line widths at frequencies greater than about 8.5 GHz.
The variation of loss (dB) per mm as a function of frequency for each measured line width is shown in FIG. 5, and for dB per wavelength as a function of frequency is shown in FIG. 6 . Loss is generally lower with wider lines at microwave frequencies, but the difference becomes less significant for a given line width at the highest range. The narrower lines show greater consistency in dB across the range of frequencies tested.
The variation in Q value as a function of frequency for each measured line width is shown in FIG. 7 . Higher Q is favored by the smaller line widths under about 10 GHz, but for all measured frequencies above that value the consistency of Q breaks down for all line widths.
The Zmax (maximum impedance) as a function of frequency for each measured line width, as calculated by the equation set forth in FIG. 8A, is shown in FIG. 8 B. The 15 micron and 27 micron width lines have higher Zmax than the 38.5 micron, but the Zmax values for the 27 micron width line are more consistent than the 15 micron width line at all measured frequencies. The values for the impedance Zo as a function of frequency for a line width of 27 microns are constant at frequencies above about 5.5 GHz , as shown in FIG. 9 . The values for the Eeff as a function of a line width of 27 microns are constant at frequencies above about 7.5 GHz, as shown in FIG. 10 .
Thick dielectric, while providing lower loss, requires wider signal line width in order to maintain impedance.
The dimensions of the structure of the present invention are a compromise driven by the electrical properties required at the operating frequency of the final product. For example, if the final product is intended for operation at 10 GHz, the dielectric material being 13 microns thick with an Eeff of 2.8, a line width of 30 microns would be a reasonable compromise. Measurement results indicate that the modular structure of the present invention is suitable and manufacturable, i.e. stable, predictable and reproducible, for use in its intended purpose.
Although the invention has been described in conjunction with one or more specific embodiments, modifications will be apparent to those skilled in the art in light of the foregoing information. Accordingly, it is intended that the present invention embrace all such modifications as are encompassed by the spirit and broad scope herein.
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Disclosed is a manufacturable silicon-based modular integrated circuit structure having performance characteristics comparable to high frequency GaAs-based integrated circuit structures, comprising materials and made in process steps which are compatible with existing low cost silicon-based integrated circuit processing.
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This application is continuation-in-part of application Ser. No. 08/151,707, filed Nov. 12, 1993, now abandoned, which is a continuation-in-part of application Ser. No. 07/832,151, filed Feb. 6, 1992, now U.S. Pat. No. 5,353,820.
FIELD OF THE INVENTION
The invention relates to an assembly for dyeing and/or coating selected portions of a yarn during the manufacture of dental floss yarn. In particular it relates to an assembly and a method for dyeing and/or polymer coating selected portions of a yarn as the yarn is traveling at a high speed. The arrangement is particularly suitable for providing a dye and/or polymer coating to selected portions of a dental floss yarn.
BACKGROUND OF THE INVENTION
Tooth decay and dental disease can be caused by bacterial action resulting from the formation of plaque about the teeth and/or the entrapment of food particles between the teeth and interstices therebetween. The removal of plaque and entrapped food particles reduces the incidence of caries, gingivitis, and mouth odors as well as generally improving oral hygiene. Conventional brushing has been found to be inadequate for removing all entrapped food particles and plaque. To supplement brushing, dental flosses and tapes have been recommended. The term "dental floss", as used herein, is defined to include both dental flosses, dental tapes and any similar article.
To improve the effectiveness and convenience of dental flosses, dental flosses combining a thin "floss" portion and a thickened "brush" portion, together with a threader have been developed. The brush portion, when drawn between tooth surfaces, has been found to provide an improved cleaning action which removes materials left by the floss portion, when used alone. The combination provides a substantially superior cleaning action. Such a device is described in U.S. Pat. No. 4,008,727, for example. The complexity of this product requires that each floss segment be individually manufactured and that the product be packaged as bundles of the individual, separate floss articles.
A continuous yarn having brush segments separated by thinner segments is disclosed in U.S. Pat. Nos. 4,008,727 and 4,142,538.
A problem arising in the manufacturing process of continuous floss brushes involves the application of coatings to the yarn. A variety of assemblies and methods are known for providing a yarn with a coating at spaced locations. For example, in one arrangement, a roller receives a coating from a supply, and provides a coating to the yarn as the yarn passes there over in contact with the roller. The roller can be formed with only a partial section of a cylinder, such that only intermittent portions of the yarn contact the roller as the roller rotates. However, such an arrangement has been unsatisfactory in providing an adequate coating to the yarn, particularly in high speed manufacturing assemblies, for example, in which the yarn is traveling at over 100 meters/min., possibly even as high as 160 meters/min.
OBJECTS AND SUMMARY OF THE INVENTION
It is an object of the present invention to provide a yarn coating assembly and method which applies a coating material to a yarn travelling at high speed, at precise and predetermined intervals along the yarn.
It is a further object of the present invention to provide a yarn coating method and assembly which can provide an appropriate amount of a coating material to a yarn while minimizing wastage of the coating material.
It is another object of the invention to provide a method and an assembly for coating selected portions of a yarn under tension such that the selected portions are maintained at a reduced diameter by the coating material after the tension is released.
It is yet another object of the present invention to provide a yarn coating assembly which can coat a plurality of yarns simultaneously, with a continuous supply of coating material provided for intermittent coating of the plurality of yarns.
It is yet another object of the invention to provide a coating applicator for applying a coating material to a yarn, comprising a container for supporting a coating material wherein the level of the coating material in the container is determined by capillary action.
According to the invention there is provided a coating applicator for applying a coating to a yarn, comprising a container wherein the container has at least one open-ended slot, each slot having a base and an open end for receiving a section of yarn, and being dimensioned to support a predetermined amount of a coating material, wherein the container has an upstream and a downstream face, at least the upstream face of the container being inclined inwardly towards the open end, and wherein the open-ended slot is defined by a pair of opposed surfaces extending between the base and the open end, the surfaces being inclined outwardly towards the open end.
The slot may be dimensioned to support the predetermined amount of coating material by capillary action.
The slot may narrow from the upstream face to the downstream face.
Further according to the invention there is provided a yarn coating assembly for applying a coating material to a length of yarn comprising a container means for holding a quantity of the coating material, a drive means for moving the length of yarn past the container means, and displacement means for displacing at least a portion of the yarn toward the container means to bring a section of the yarn into contact with the coating material. The displacement means may comprise a cam on a rotatable wheel, the cam having a cam surface positioned relative to the yarn such that, upon rotation of the wheel, the yarn is urged into contact with the coating material by the cam surface engaging the yarn, and when the cam surface is not in contact with the yarn, the yarn is not in contact with the coating material. The cam may be removably mounted on the wheel to permit replacement with differently sized or differently shaped cams.
The container means may define an open-ended slot having a width sufficient to accommodate the thickness of the yarn and to support a predetermined amount of the coating material. The width of the slot may be dimensioned to support the predetermined amount of the coating material by capillary action, and may narrow from an upstream to a downstream end.
The assembly may include a guide means defining a guide slot located upstream of the container means for aligning the yarn with the slot of the container means. The guide means may have an inclined upstream face. The container means typically defines a plurality of open-ended slots, each dimensioned to receive a section of yarn and to support a predetermined amount of the coating material. The guide means will then typically define a corresponding number of slots.
The assembly may include a storage reservoir having an inlet, and an outlet in liquid communication with the container means. The assembly may also include a pump means for pumping coating material to the storage reservoir, and a pump motor connected to the pump means for driving the pump means.
The assembly may further include a supply controller means for controlling the pump means to replenish the storage reservoir at the same rate as that at which the coating material is removed from the container means by the yarn. The supply controller means may be operable to control the pump motor.
The assembly may also include a main supply reservoir in liquid communication with the inlet of the storage reservoir.
Furthermore, the assembly may include a speed controller means for controlling the rotational speed of the wheel in proportion to the speed at which the length of yarn is moved past the container means by the drive means.
Still further according to the invention there is provided a method of applying a coating material to at least one length of yarn at intermittent locations along the length of yarn, comprising running a length of yarn past a container means for holding a quantity of coating material, and intermittently displacing at least a portion of the length of yarn toward the container means, each displacement bringing a section of the yarn into contact with the coating material to produce intermittently coated sections. The tension of the section of yarn displaced into contact with the coating material may be controlled while said section of yarn is in contact with the coating material.
The speed at which the length of yarn is run past the container means may be determined and the displacement frequency at which the yarn is displaced into contact with the coating material, controlled, the frequency being controlled to change in proportion to the change in speed of the yarn. The coating material in the container means may be replenished at the same rate as that at which it is removed from the container means by the length of yarn.
A coating material in the container means may be replenished in proportion to the speed at which the length of yarn is run past the container means.
A plurality of yarn lengths may be run past the container means simultaneously.
BRIEF DESCRIPTION OF THE DRAWINGS
A more complete appreciation of the invention and many of the attendant advantages thereof will become readily apparent from the following detailed description, particularly considered in conjunction with the drawings in which:
FIG. 1 is a plan view of a yarn coating/dyeing assembly of the present invention;
FIG. 2 is a side view of the assembly of FIG. 1;
FIG. 3 is a schematic side view of the assembly of FIG. 2 showing the location of some of the components of the assembly;
FIG. 4 is a front view of a coating/dye applicator for use in the assembly in accordance with the invention;
FIG. 5 is a plan view of a coating/dye applicator for use in the assembly in accordance with the invention;
FIG. 6 is a side view of a coating/dye applicator for use in the assembly in accordance with the invention;
FIG. 7 is a plan view of another embodiment of a coating/dye applicator in accordance with the invention;
FIG. 8 is a front view of the coating/dye applicator of FIG. 7;
FIG. 9 is a detailed plan view of part of the coating/dye applicator of FIG. 7;
FIG. 10 is a front view of a comb-like guide means for guiding a plurality of yarns into the coating/dye applicator;
FIG. 11 is a side view of the guide means of FIG. 10, and
FIG. 12 is a side view of a deflection roller in partial cross-section.
DETAILED DESCRIPTION OF THE INVENTION
For purposes of this invention the term "coating" will be used to refer to a variety of coating substances, e.g. dyes, polymer solutions, scented and unscented waxes and any other coating substance which may be applied to a yarn irrespective of its degree of penetration into the yarn.
For ease of description, however the terms "dye" and "dyeing" will be used to cover all types of coating materials.
Furthermore, the terms "container" and "container means" will be used to refer to any vessel or medium capable of supporting a liquid. This would, for example, also include a pad capable of soaking up and retaining a liquid.
Referring now to FIGS. 1 and 2, a plan view and side view of the yarn dyeing assembly of the present invention are respectively shown. Thus, for example, in the context of a floss/brush, as discussed above, a coating is applied to maintain the selected portions at a reduced diameter, and also to provide a dyed section to demarcate individual lengths.
As shown in FIG. 1, the yarn dyeing assembly 10 includes a dyeing head or dye applicator 12, which provides dye at intermittent or spaced locations along a continuous length of yarn 13 as the yarn 13 travels in a direction indicated by arrow A. Upstream of the dyeing head 12 is a cam roller 14 which is suitably driven by a drive means indicated generally by reference numeral 20. Further upstream from the cam roller 14, a deflection roller 16 is provided to assist in guiding the yarn 13, and to urge the yarn 13 against the cam roller 14. It is to be understood that the apparatus is preferably utilized for simultaneous dyeing of a plurality of yarns 13, with the plurality of yarns 13 extending in the direction of arrow A, however a single yarn 13 could be dyed if desired.
Referring now to FIG. 2, it will become apparent that the yarns 13 pass over the deflection roller 16, and under the cam roller 14. At least one cam 15 is provided at a peripheral portion of the cam roller 14, such that as the roller 14 rotates, the yarns 13 will be deflected each time the cam 15 passes about the lowermost portion of the path of revolution of the cam 15, with the cam 15 contacting the yarns 13 and deflecting the yarns 13 downwardly. As the yarns 13 are deflected downwardly, they are coated or dyed by the dyeing head 12.
The drive means 20 (FIG. 1) drives the cam roller 14 at a speed dependent upon the yarn travel speed, as well as the desired spacing between dyed portions. This is controlled by means of a magnetic sensor and controller arrangement as is described in greater detail below. The lengths of the dyed portions, in turn, are determined by the configuration of the cam 15. For example, in the floss/brush context, it is desirable to provide selectively dyed portions having a length of approximately 3 inches, with 18 inches of the floss/brush disposed between respective dyed portions. The yarn 13 is driven by feed rollers (schematically indicated on FIG. 2 as 19) which also serve to control the tension of the yarn 13 downstream of the rollers 19. The drive means can include a separate motor, or a shaft extending from a common drive means which operates other components in a floss manufacturing system. For dyeing or coating a floss/brush, the yarn tension during feeding is held at a predetermined level to control absorption of the dye. In the case of an elastic yarn 13, as is envisaged here, the tension typically is such as to maintain the yarn 13 at a reduced diameter. Clearly, however, the tension must be below the tensile strength of the yarn 13 when deflected by the cam roller 14, such that the yarn 13 does not break during the dyeing operation. As is also shown in FIG. 2, a guide means 18 is provided between the cam roller 14 and the dyeing head 12, such that the plurality of yarns 13 are properly positioned with respect to the dyeing head 12 as will become readily apparent hereinafter.
Referring to FIGS. 4, 5 and 6, details of the dyeing head 12 will now be described. FIG. 4 shows a front view of the dyeing head 12, in which a plurality of slots or grooves 22 are provided for a corresponding number of yarns 13 which are to be dyed simultaneously. In the embodiment of FIG. 4, 40 slots are provided, thereby allowing for the simultaneous selective dyeing of 40 yarns. The upper open ends of the slots or grooves 22 are defined by inclined surfaces 23 which support the yarns. The lower closed ends of the slots 22 are defined by a pair of spaced apart, substantially parallel sides, extending from a base. The inclined surfaces 23 insure that any splices or other irregularities in the yarns 13 do not interrupt the process, e.g. by catching in the slots 22 and thereby breaking the yarn 13. In the event of an irregularity the inclined surfaces 23 will urge the yarn 13 upwardly to accommodate the irregularity. A plurality of bolt holes 26 are provided for mounting the dyeing head 12 by means of mounting bolts (not shown). By loosening the mounting bolts, and manipulating an adjustment screw 27 (FIG. 2) the height of the head 12 may be adjusted to increase or decrease the height of the head 12 relative to the yarn 13.
Each slot 22 includes a liquid supply conduit 24 which supplies the dye upwardly into the slots 22, such that the slots 22 are constantly supplied with the dye. In the embodiment shown in FIGS. 4 to 6, the supply conduits 24 are alternatingly staggered, thereby allowing the supply conduits 24 to be formed of a sufficient size constantly to flood the slots 22, while increasing the structural integrity of the dyeing head 12. In this embodiment the supply conduits 24 are formed with a diameter of 0.05 to 0.12 inches, preferably 0.07 to 0.09 inches, depending on the viscosity of the dye or coating material. The slots 22 may be formed of a sufficiently small width 21 (e.g. 0.015 inches), such that the dye is constantly maintained within the entire length of the slots 22 by capillary action. Instead, as in this embodiment, a pump may be controlled to supply the appropriate amount of dye to replenish the slots 22 at the same rate as that at which the dye is removed from the slots 22 by the yarns 13.
As regards the capillary action embodiment, it has been recognized that a dye/coating can be provided for selected portions of yarns by utilizing grooves which maintain the dye by capillary action. Capillary action depends upon two factors including: (1) the cohesion of the liquid molecules; and (2) the adhesion of the molecules to the surface of a solid, in this case the material of the dyeing head.
Thus, the actual width of the grooves can vary as coatings or liquids to be applied to the yarn 13 vary, or if different materials for forming the dyeing head 12 are selected. Brass and stainless steel have, for instance, been found to work well as materials for the head 12. It will be appreciated that the positioning of the conduits 28 may take a variety of configurations. In one embodiment, illustrated in FIGS. 7 to 9, found to work particularly well, the conduits 28 are spaced along a common straight line running slightly to one side of the longitudinal axis of the head 12, closer to its upstream end. This provides for a very uniform coating for all the yarns.
In this embodiment the conduits 28 have a diameter of 0.07 inches and the grooves 29 tapered from 0.018 inches at their upstream ends to 0.011-0.012 inches at their downstream ends. This tapered shape provides for better retention of the coating material.
Referring again to FIG. 6, the supply conduits 24 are in flow communication with a dye storage reservoir 30, such that the supply conduits 24 supply the dye upwardly from the storage reservoir 30 to the slots 22. A ceramic piston pump 31 (FIG. 1) replenishes the reservoir 30 by continuously supplying dye from a main supply reservoir 32 to the reservoir 30 via a primary supply conduit (not shown). The primary supply conduit feeds the dye into the reservoir 30 by means of an inlet (not shown) provided in a lower wall of the reservoir 30. The conduits 24 are thus constantly supplied with dye and act as temporary storage reservoirs for supplying dye to the slots 22. The dye level in the conduits accordingly fluctuates as dye is continuously supplied from the reservoir 30 and is intermittently removed by the yarn 13. As is also shown in the side view of FIG. 6, the upstream and downstream faces 33 of the dyeing head 12 are inclined, resulting in the hexagonal appearance of the open ends of the slots 22 when seen in plan view (FIG. 5). The inclined configuration serves to urge the yarn 13 upwardly in the event of an irregularity in the yarn 13, thus causing the yarn 13 to ride higher on the inclined surfaces 23 as was described above.
Referring to FIGS. 10 and 11, the guide means 18 (disposed adjacent the dyeing head 12 as shown in FIG. 2) includes a comb-like structure, with a plurality of guide slots 34 corresponding to the number of slots provided in the dyeing head 12. The guide slots 34 have a width 35 which typically is larger than the width 21 of the slots 22 or the maximum width of the slots 29, such that the yarns can be guided by the guide slots 34, without rubbing excessively against the guide slots 34, and to accommodate small irregularities in the yarn. The yarns are thus suitably positioned with respect to the slots 22, 29 by the guide slots 34 of the comb-like structure, and by the inclined surfaces 23 of the dyeing head 12. A suitable width 35 of the guide slots 34 is for example 0.03 inches. The height 36 of the guide slots 34 is sufficient such that the yarns 13 are retained in the guide slots 34 irrespective of whether or not they are deflected by the cam 15. Mounting apertures 37 are provided such that the guide means 18 can be mounted directly on the dyeing head 12. As shown in the side view of the guide means 18 (FIG. 11), the guide means 18 is shaped to be mounted closely adjacent to the dyeing head 12. As with the head 12, the guide means 18 has an inclined upstream face 38 to allow the yarn to ride up on the guide means 18 in the event of an oversized irregularity in the yarn 13 being encountered.
Referring now to FIG. 12, a front view of the cam roller 14 is shown in partial cross-section. The roller 14 includes a pair of end plates 40 secured to opposite ends of a roller cylinder having a surface 42. The roller 14 is maintained by a plurality of bolts 44. Three bolts 44 were found to be adequate in practice. The cam 15 in the form of a rod, is secured to the end plates 40, by means of suitable fasteners. In the embodiment illustrated, spigot-like ends of the cam 15 are received in apertures in the plates 40 and retained by means of retention clips 45.
As mentioned above, and referring again to FIGS. 1-3, the drive means 20 is controlled by a magnetic sensor and controller arrangement. Referring to FIG. 1, a sensor (not shown) detects the yarn speed. A second magnetic sensor 54 monitors the rotational speed of the cam drive gear 56. The magnetic signal from the sensor 54 is converted into a 4-20 mA output signal which is, in turn, shaped by a programmable controller 58 (FIGS. 2 and 3) and used to control the rotational speed of the cam roller 14. In addition, the pump 31 is controlled in a manner described below. The 4-20 mA output signal is sent to a stepper motor controller 60 (FIG. 3). This controls the speed of a stepper motor (not shown) which drives the pump 31. A digitally adjustable slope multiplier, adjustable to 0.1% of full scale, allows adjustment of the stepper motor speed.
Furthermore, by adjusting the angle between the stepper motor and the pump 31, the piston stroke and consequently the displacement of the piston may be adjusted. Thus the amount of dye supplied by the pump 31 and the spacing between dyed portions can be controlled in sympathy with and as a function of the yarn speed.
The replenishment of the dye in the slots can instead be related to the depletion of the dye from the slots by the yarns 13 by monitoring the level of the dye in the slots, for example by using an optical sensor. The signals from the sensor are then fed to a microprocessor to control the stepper motor speed.
In order to adjust the length of the dyed portions, the cam 15 may be replaced with a suitably shaped cam. The length of application is fine-tuned by adjusting the height of the head 12 by loosening the mounting bolts and manipulating the adjustment screw 27 (FIG. 2). Clearly, numerous modifications and variations of the present invention are possible in the light of the above teachings. It is therefore to be understood that within the scope of the appended claims, the invention may be practiced otherwise than as specifically described herein.
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An apparatus and method for applying coatings to yarns, particularly yarns to be utilized as dental floss. In a preferred arrangement, an array of parallel spaced yarns are continuously fed while being intermittently deflected by a cam or deflector. As the yarns are deflected, they enter a grooved liquid applicator, with the grooves maintaining a predetermined amount of liquid therein by capillary action. A predetermined amount of liquid is thus applied at intermittent or spaced locations along the length of the yarn. The method and apparatus is particularly suitable for providing dye at spaced locations along a continuous length of floss, thereby demarcating lengths suitable for individual use. Various aspects are also applicable to a variety of yarn coating and/or dyeing applications.
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BACKGROUND OF THE INVENTION
This invention relates to a scroll compressor of a differential pressure oil-supply type, and, more particularly to a scroll compressor including means for maintaining a differential pressure oil-supply in a wide operation range.
A scroll compressor of the aforementioned type is proposed in, for example, U.S. Pat. No. 4,365,941 wherein an intermediate pressure chamber on the back of an orbiting scroll.
A pressure of the intermediate pressure chamber is governed by a pressure of an airtight chamber which is communicated with the intermediate pressure chamber through a communication hole and roughly maintained at an average pressure of the airtight chamber. The pressure of the airtight chamber is governed by a suction pressure according to characteristics of the scroll compressor and that value is determined by a position of the communication hole. In other words, the intermediate pressure is detemined by the suction pressure and the communication hole position independent of discharge pressure.
However, in the above-noted scroll compressor, as oil is supplied to the sliding part by a differential pressure between the discharge pressure and the intermediate pressure, if the differential pressure is small or null, the oil cannot be supplied to the sliding part so that the operation is impossible. Also, when the communication hole is provided at the position where the intermediate pressure is low in order to maintain the differential pressure, a force pressing the orbiting scroll against a stationary scroll produced by the intermediate pressure is insufficient when the pressure differential between the suction pressure and the discharge pressure is so great that sealing between tips of lapping parts and flat plate parts becomes impossible.
It is an object of the pressent invention to provide a scroll compressor which facilitates maintaining an oil-supply pressure within a wide operation range.
In a scroll compressor, when suction pressure is constant and discharge pressure is low, the force pressing the orbiting scroll against the stationary scroll can be small compared to when the discharge pressure is high. According to the present invention, a scroll compressor is provided with a valve which can switch connection of an intermediate pressure chamber to a lower intermediate pressure or to a higher intermediate pressure of a compressor part, and is constructed so that when the discharge pressure is below a certain value, the intermediate pressure chamber is connected to the lower intermediate pressure side of the compressor by the valve to maintain oil-supply pressure and, when the discharge pressure is above the certain value, the intermediate pressure chamber is connected to the higher intermediate pressure side of the compressor part by the valve which maintains the oil-supply pressure.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional view of an embodiment of a scroll compressor of the present invention;
FIG. 2 is an enlarged sectional view of a main part of FIG. 1;
FIG. 3 is a sectional view for explaining an operation of the valve shown in FIGS. 1 and 2;
FIG. 4 is a sectional view of another embodiment of a scroll compressor of the present invention;
FIG. 5 is a sectional view of the main part of a scroll compressor according to further another embodiment the present invention;
FIG. 6 is a perspective view of a valve body of a valve shown in FIG. 5; and
FIG. 7 is a sectional view of FIG. 5 for explaining the operation of the valve.
DETAILED DESCRIPTION
Referring now to the drawings wherein like reference numerals are used throughout the various views to designate like parts and, more particularly, to FIG. 1 according to this figure, a scroll compressor includes a compressor part generally designated by the reference numeral 2 disposed at an upper part in an airtight container 1 and a motor part 3 disposed at a lower part in the airtight container 1, with the compressor part 2 including an orbiting scroll 6 and a stationary scroll 7 which mesh with each other. The orbiting scroll 6 includes a flat end plate 6a and a spiral lapping part 6b vertical to the flat end plate 6a. The stationary scroll 7 includes a flat end plate 7a and a spiral lapping part 7b vertical to the flat end plate 7a and fixed to a frame 5. A lower end of a crank shaft 4, joined with a rotating shaft of a motor 3, is immersed in an oil sink 9 defined at the bottom of the airtight container 1. An oil path 4a whose lower end is opened in a shaft axis and whose upper end is opened at an eccentric position with respect to the rotating shaft axis is provided in the crank shaft 4. A communication hole 10 is provided in the orbiting scroll 6 at a position where an intermediate or back pressure between a suction pressure and a discharge pressure is obtained and an intermediate pressure chamber 8 in which the pressure is at the intermediate value is also provided. An upper end of the crank-shaft 4 is coupled with a boss part 6c extending downwardly from the orbiting scroll 6.
As shown in FIG. 2, a valve 13 connects or disconnects a communication between a suction chamber 11a of the compressor part 2 and the intermediate pressure chamber 8, with the valve including a cylinder 14 formed in the stationary scroll 7, a valve body 15 incorporated in the cylinder 14, a compession spring 16 for pressure setting and a stopper ring 17 for preventing the valve body from coming out. One side of the cyliner 14 communicates with the airtight container 1 and the other side of the cylinder 14 communicates with the intermediate pressure chamber 8 through a communication hole 18 and also communicates with the suction chamber 11a through a communication hole 19. The valve body 15 includes a surface 15a for receiving the internal pressure of the airtight container 1 at one end and a surface 15b for receiving the internal pressure of the intermediate pressure chamber 8 on the back side of the pressure receiving surface 15a. The valve body 15 also has a needle part 15c which can open and close the communication hole 19 at its other end. The compression spring 16 is placed between the pressure receiving surface 15b of the valve body 15 and a side wall of the cylinder 14. The stopper ring 17 is fitted into an annular groove provided along an inside wall of the cylinder 14 and prevents the valve body 15 from coming out.
When the pressure differential between the pressures applied to both pressure receiving surfaces of the valve body 15 of the valve 13 is higher than the spring force of the compression spring 16, the valve body 15 is shifted to the position where the needle part 15c closes the communication hole 19, in other words, it disconnects the connection between the intermediate pressure chamber 8 and the suction chamber 11a. When the pressure differential is lower than the spring force of the compression spring 16, the valve body 15 is shifted by the spring force to the position where its needle part opens the communication hole 19, in other words, it communicates the intermediate pressure chamber 8 to the suction chamber 11a.
Referring to FIG. 1, the orbiting scroll 6 orbits as the boss part 6c is rotated in the intermediate pressure chamber 8 of the frame 5 by the rotation of the crankshaft 4. By the movement of the contact points between the orbiting lapping part 6b and the stationary lapping part 7b, the gas drawn through a suction tube 11 is compressed while flowing through the spiral chamber from the outside to the inside, is discharged into an airtight container 1 through a discharge outlet 7c provided at the center of the stationary scroll 7 and flows through a path 7d provided on an outer periphery of the stationary scroll 7 and a path 5a of an outside periphery of the frame 5. A part of the gas having passed through the paths 4d and 5a flows through outside periphery paths 3a and 3b of the motor 3 and the other part of the gas flows between the frame 5 and the motor 3, and all gas is discharged out of the machine through the discharge tube 12. The volume of the airtight chamber, defined by the lapping parts 6b and 7b and the flat end plates 6a and 7a of the orbiting scroll 6 and stationary scroll 7, is reduced according to the movement from the outside to the center so that the pressure of the gas contained therein is increased according to the movement. The pressure in the intermediate pressure chamber 8, defined by the orbiting scroll 6 and the frame 5, is, as mentioned above, maintained at the intermediate pressure between the suction pressure and the discharge pressure by the communication hole 10. With the pressure differential between the intermediate pressure and the internal pressure of the compression part, the orbiting scroll 6 is pressed against the stationary scroll 7 to maintain the tight contact of the sealing part of a gap between the tips of the lapping parts 6b and 7b and the flat plate parts 7a and 6a. Moreover, as the pressure in the airtight container 1 is the discharge pressure and higher than that in the intermediate pressure chamber 8, freezer oil in the oil sink is pushed up through the oil path 4a in the crank shaft by the differential pressure between those two pressures and supplied to a sliding part.
Referring to FIGS. 2 and 3, an operation of the valve 13 is hereinunder described. Ps denotes the suction pressure; Pb, the intermediate pressure; Pd, the discharge pressure; K, the spring force of the compression spring; SA, the cross sectional area of the cylinder 14; and SB, the cross sectional area of the communication hole 19. Because the relation Ps=Pb=Pd is maintained before start, the valve body 15 of the valve 13 is pressed against the stopper ring 17 by the spring force K as shown in FIG. 3. In other words, the valve body 15 is shifted to the position where it fluidly connects the intermediate pressure chamber 8 to the suction chamber 11a. When the compressor is started at this state, if the discharge pressure Pd is increased to the value which conforms to following formula (1):
Pd×SA>Pb×SA+K (1)
the valve body 15 is shifted to the position shown in FIG. 2 and the communication hole 19 is closed by its needle part 15c. In this state, the inside of the airtight container 1, the suction chamber 11a and the back pressure chamber 8 are separated from each other and the compressor is driven essentially under the same condition as if the valve did not exist.
When the discharge pressure Pd cannot reach a value high enough to conform to the formula (1), in other words the differential pressure between pressures applied to both pressure receiving surfaces of the valve body 15 is lower than the spring force K, the valve body 15 is maintained at the position shown in FIG. 3 and the intermediate pressure chamber 8 is communicated with the suction chamber 11a through communication holes 18 and 19 so that the intermediate pressure Pb is low. The fact that the intermediate pressure Pb is maintained at a value lower than the normal intermediate pressure means that the differential pressure between the discharge pressure and the intermediate pressure is large and the oil-supply pressure (the differential pressure between the discharge pressure and the intermediate pressure) is maintained; therefore, a wide range of operation can be obtained. When the intermediate pressure is maintained relatively low, a pressing force of the orbiting scroll 6 is small. However, as the discharge pressure is also low, the pressing force may be small and this is also a convenient point.
Then the case when the discharge pressure is reduced during operation, for instance by reduction of the load, is hereinunder described. While the needle part 15c of the valve body 15 closes the communication hole 19, if the discharge pressure is decreased to the value which conforms to the following formula (2):
Pd×SA<Pb×(SA-SB)+Ps×SB+K (2)
the valve body 15 is shifted to the direction of opening the communication hole 19 and the intermediate pressure is maintained at a pressure lower than a normal pressure.
FIG. 4 shows another embodiment of the present invention and this embodiment is different from the one shown in FIG. 2 at the point that the position where a communication hole 19a is opened is provided in an airthight chamber 11b of a compressor part 2 in which a pressure is lower than the intermediate pressure.
Also in this embodiment, operation principle is basically the same as the one shown in FIG. 2 and, if Ps is substituted by Ps' (a pressure in the airtight chamber llb) in the formulae (1) and (2), the same performance and effect as described by FIG. 2 can be realized.
Still another embodiment of a scroll compressor of the present invention is hereinunder described with reference to FIG. 5 through FIG. 7. This embodiment is the same as FIG. 1 except for a valve 113 and a part of a compressor part 200.
In FIG. 5, the scroll compressor is provided with a valve generally designated by the reference numeral 113 at the stationary scroll 107. The valve 113 is constituted by a cylinder 114 formed in the stationary scroll 107, a valve body 115 incorporated in the cylinder 114, a spring 116 and a stopper ring 117. A pipe 118 communicating with the intermediate pressure chamber 8, a first port 119 communicating with a lower intermediate pressure side of the compressor part 200 and a second port 120 communicating with a higher intermediate pressure side of the compressor part 200 are connected to the cylinder 114. One end surface 115a of the valve body 115 is formed so as to receive a fluid pressure which is normally the discharge pressure and a seat part 115c which opens and closes the first port 119 protrudes from the other end surface 115b of the valve body 115. An annular groove 115d is provided at a central part of the valve body 115 and a valve hole 115e which is opened at the annular groove 115d and the end surface 115b is provided. The spring 116 is placed between a side wall of the cylinder 114 and the end surface 115b of the valve body 115 and actuates the valve body 115 toward the direction of opening the first port 119. The stopper ring 117 is attached to an inner wall of the cylinder 114 and prevents the valve body 115 from projecting out.
With the valve 113 of the above constitution, when the valve body 115 is shifted to the position where the first port 119 is closed by the seat part 115c, the pipe 118 is fluidly connected to the second port 120 through the annular groove 115d and the valve hole 115e and, when the valve body 115 is shifted to the position where the valve body 115 touches the stopper ring 117 as shown in FIG. 7, the pipe 118 is connected to the first port 119.
Then the operation of the embodiment of FIG. 5 is as follows:
Because the pressures in the compressor are normally balanced when the compressor starts, the valve body 115 of the valve 113 is shifted to the position where it touches the stopper ring 117 by the spring 116 as shown in FIG. 7. At this state, the pipe 118 is connected to the first port 119. In other words, the intermediate pressure chamber 8 is connected to the lower intermediate pressure side of the compressor part 200 when the compressor starts.
After the compressor starts, when the discharge pressure exceeds a certain value, the discharge pressure applied to one end surface 115a of the valve body 115 overcomes the spring force of the spring 116 and the valve body 115 is shifted to the position shown in FIG. 5. Then the first port 119 is closed by the seat part 115c and at the same time the pipe 118 is connected to the second port 120 through the annular groove 115d and the valve hole 115e. In other words, when the discharge pressure exceeds a certain value, the intermediate pressure chamber 8 is connected to the higher intermediate pessure side of the compressor part 200.
As described above, when the discharge pressure is below a certain value, the intermediate pressure is maintained at a relatively low value and, when the discharge pressure exceeds a certain value, the intermediate pressure is maintained at a relativey high value. The fact that the intermediate pressure is maintained at a relatively low value when the discharge pressure is low means that the oil-supply pressure, the pressure differential between the discharge and the intermediate pressure, can be maintained, and the range of operation can be widened in terms of the oil-supply. When the intermediate pressure is maintained at a relatively low value, the pushing-up force for the orbiting scroll 6 is small. However, the discharge pressure is also low in this case and the pushing-up force may be small and this is also a convenient point.
As described above, the intermediate pressure is controlled in accordance with the fluctuation of the discharge pressure by a valve of simpler structure to facilitate maintaining sufficient differential pressure between two pressures required for oil-supply and hence a wider range of operation is possible.
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A scroll compressor including a stationary scroll and an orbiting scroll, with an intermediate pressure chamber being defined on a back side of the orbiting scroll member and being in communication with a pressure chamber through a communication hole to produce a force for pressing the orbiting scroll against the stationary scroll. Oil in an oil sink is supplied to sliding portions by a differential pressure between a pressure in the air tight container and a pressure in the intermediate pressure chamber. A valve is provided for switching the connection of the intermediate pressure chamber to a higher intermediate pressure side or to a lower intermediate pressure side of the compressor. The valve is constructed such that the intermediate pressure chamber is connected to the lower intermediate pressure side of the compressor when a discharge pressure of the compressor is lower than a certain value and connected to the higher intermediate pressure side of the compressor when the discharge pressure is higher than a certain value so that a proper oil supply pressure is maintained over a wide operational range.
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FIELD OF THE INVENTION
[0001] THIS INVENTION relates to agricultural apparatus, namely a ground engaging apparatus. The ground engaging apparatus is particularly suitable for, but not limited to, tillage applications and non-till seed planting.
BACKGROUND OF THE INVENTION
[0002] When planting seeds, in particular for large scale applications such as a commercial farm, a ground engaging apparatus such as a planter apparatus may be towed behind a tractor to cut channels or furrows into the soil which is followed by planting of a seed within the channel. Usually, a plurality of planter units are attached to a support towing bar that aligns the planter units at selected distances apart from each and the support bar is attachable to a tractor via a tow bar.
[0003] The ground engaging unit may comprise a frame having a pivotable parallelogram arrangement that maintains a ground opening tool in the ground while traversing level and uneven ground. A spring located between two pivotable arms of the parallelogram applies a force that maintains the ground opening tool at a pre-selected depth in the soil as the ground engaging unit encounters inclines and depressions. When the ground engaging unit encounters an obstacle such as a rock or stump, the shank is pivoted upward and away from the obstacle by a break-away or breakout mechanism to thereby prevent damage to the ground opening tool. The break-away mechanism comprises a spring that applies a force independent of the parallelogram as a separate break-away unit.
[0004] A ground engaging apparatus described in Australian patent AU 1996 60854 B2 (714157) (Techsearch Incorporated) comprises a single bias means for adjusting both a downward force to maintain the ground opening tool in the soil at a selected depth and a break-away force that maintains the ground opening tool in the soil unless the planter unit encounters an obstacle. This design is limited in that adjusting the downward force on a parallelogram arrangement also adjusts the break-away force, which is undesirable in situation where a user wishes to adjust each force independently of the other. Also, a minor adjustment of the bias means to the downward force of the parallelogram has a significant affect on the break-away force, which may result in excessive break-away force applied to the ground opening tool.
SUMMARY OF THE INVENTION
[0005] It is an object of the invention to provide an alternative or improvement to the abovementioned background art.
[0006] In a first aspect, the invention provides a ground engaging apparatus comprising:
[0007] (i) a frame;
[0008] (ii) a support plate pivotally attached to the frame about a first point;
[0009] (iii) a first bias member attached at a first end to the frame and attached at a second end to the support plate;
[0010] (iv) at least two arms each pivotally attached at respective first ends to the support plate;
[0011] (v) a shank support to which respective second ends of the at least two arms are pivotally attached;
[0012] (vi) a second bias member attached at a first end to the frame and attached at a second end to one arm of the at least two arms;
[0013] (vii) a shank attached to the shank support;
[0014] (viii) a ground opening tool attached to a free end of the shank opposite the shank support; and
[0015] (ix) a ground follower attached to the shank support;
[0016] wherein:
[0017] said first bias member applies a first force to the support plate urging the support plate to rotate about the first point to thereby abut a stop that obstructs rotation thereof until a counter force is applied against the ground follower or ground opening tool that is greater than the first force such that the support plate rotates about the first point in a direction away from the stop; and
[0018] the second bias member applies a second force to the one arm thereby urging the ground follower against a surface and the ground opening tool into the surface.
[0019] Preferably, the apparatus comprises two arms.
[0020] Preferably, the ends of the two arms define pivotable corners of a parallelogram arrangement comprising linkages respectively comprising the two arms, the support plate and the shank support, each of which define a side of the parallelogram and respectively capable of uniform movement.
[0021] Preferably, a point at which the second end of the first bias member attaches the support plate and the respective first ends of the two arms define a first linkage of the parallelogram.
[0022] Preferably, the respective second ends of the two arms and the shank support comprise a second linkage of the parallelogram.
[0023] More preferably, the second linkage further comprises the ground follower and ground opening tool.
[0024] Preferably, the first ends of the respective two arms are capable of being vertically aligned.
[0025] Preferably, the second ends of the respective two arms are capable of being vertically aligned.
[0026] Preferably, the second bias member is attached intermediate the one arm.
[0027] Preferably, the first point is located intermediate the stop and the point at which the second end of the first bias member attaches to the support plate.
[0028] Preferably, the first bias member and second bias member each comprise a coiled spring or hydraulic cylinder.
[0029] More preferably, the first bias member is a coiled spring and the second bias member is a hydraulic cylinder.
[0030] Preferably, the first force of the first bias member and the second force of the second bias member are independently adjustable.
[0031] Preferably, the ground follower is located in front of the shank and below the at least two arms.
[0032] Preferably, the ground follower comprises a wheel.
[0033] Preferably, the frame comprises a towing attachment for attaching to a tow bar.
[0034] Preferably, one or more apparatus are attached to a tow bar via the towing attachment.
[0035] Preferably, the surface is a surface of ground for cultivation.
[0036] In a second aspect, the invention provides a ground engaging assembly comprising a plurality of ground engaging apparatus of the first aspect each attached to a same tow bar.
[0037] Preferably, the ground engaging assembly further comprises a seed dispenser located adjacent to each ground opening tool such that in use one or more seed may be placed within a channel formed in the ground by the ground opening tool.
[0038] More preferably, the seed dispenser is located behind the ground opening tool at an end opposite a cutting end.
[0039] It will be appreciated that the present invention comprises at least two bias members for respectively providing a downward force to maintain the ground opening tool in the ground when traversing level, risen or depressed ground and a breakout force that maintains the ground opening tool in the ground unless an obstruction or obstacle is encountered. The invention preferably has the advantage of adjusting the downward force and breakout force independently of each other. The invention in a preferred embodiment combines the two bias members in a compact and efficient configuration such that both bias members are located in front of a wheel or ground follower as described herein.
[0040] Throughout this specification unless the context requires otherwise, the word “comprise”, and variations such as “comprises” or “comprising”, will be understood to imply the inclusion of the stated integers or group of integers or steps but not the exclusion of any other integer or group of integers.
DESCRIPTION OF THE DRAWINGS
[0041] In order that the invention may be readily understood and put into practical effect, preferred embodiments will now be described by way of example with reference to the accompanying drawings wherein like reference numerals refer to like parts and wherein:
[0042] FIG. 1 shows a side view of a ground engaging apparatus of the invention on level ground and first bias member in phantom;
[0043] FIG. 2 . shows a side view of the ground engaging apparatus traversing level ground without breakout;
[0044] FIG. 3 shows a side view of the ground engaging apparatus traversing a depression in the ground without breakout;
[0045] FIG. 4 shows a side view of the ground engaging apparatus traversing risen ground without breakout;
[0046] FIG. 5 shows a side view of the ground engaging apparatus retracted;
[0047] FIG. 6 shows a side view of the ground engaging apparatus traversing level ground in a breakout configuration;
[0048] FIG. 7 shows a side view of the ground engaging apparatus traversing a depression in a breakout configuration;
[0049] FIG. 8 is a side view of the ground engaging apparatus traversing risen ground in a breakout configuration;
[0050] FIG. 9 is a line diagram of the ground engaging apparatus traversing level ground without breakout;
[0051] FIG. 10 is another representation of a line diagram of the ground engaging apparatus traversing level ground without breakout;
[0052] FIG. 11 is a line diagram of the ground engaging apparatus traversing a depression without breakout;
[0053] FIG. 12 is a line diagram of the ground engaging apparatus traversing risen ground without breakout;
[0054] FIG. 13 is a line diagram of the ground engaging apparatus traversing level ground with breakout;
[0055] FIG. 14 is a line diagram of the ground engaging apparatus traversing a depression with breakout;
[0056] FIG. 15 is a line diagram of the ground engaging apparatus traversing risen ground with breakout; and
[0057] FIG. 16 is another diagram illustrating preferred structures and applied forces of the ground engaging apparatus.
DETAILED DESCRIPTION OF THE INVENTION
[0058] Terms used herein when referring to an item or integer are not intended to suggest or imply any limitation to the structure or function of the item or integer.
[0059] FIG. 1 shows a side view of a ground engaging apparatus 10 comprising a support plate 50 , a shank support 60 and two arms 30 , 40 each pivotally attached at opposites ends to said support plate 50 and shank support 60 thereby forming sides of a parallelogram 35 . Attachment points A, B, C and D of ends of arms 30 , 40 generally define corners of the parallelogram 35 . Accordingly, plate 50 and shank support 60 effectively form part of the parallelogram 35 . A shank 70 , also referred to as a tine, tyne, tine shank or tyne shank, is attached to the shank support 60 and is adjustable relative thereto by loosening and tightening bolts 61 . A ground opening tool 80 that is adapted to disrupt the ground 91 , preferably forming a channel suitable for planting seeds, is attached to the shank 70 at a free end opposite the shank support 60 . A ground follower 90 , shown as a wheel, is attached to shank support 60 and located in front of the ground opening tool 80 at a leading end digging tip 81 of the ground opening tool 80 . The wheel 90 contacts the ground 91 as shown and in use assists with guiding and positioning the ground engaging apparatus 10 , in particular the ground opening tool 80 .
[0060] The support plate 50 is pivotally attached to a frame 100 at attachment point A (also referred to herein as a first point). A first bias member 200 is attached to the support plate 50 at pivotable attachment point E and attached to the frame 100 at point 220 as shown in FIG. 1 . The first bias member 200 applies a downward force, referred to herein as an applied breakout force, against plate 50 that is countered by stop 210 when there is no reaction or counter breakout force applied to the ground opening tool 80 as discussed hereinafter. Point A is preferably located intermediate the stop 210 and point E, where the first bias member 200 attaches to the support plate 50 . Adjusting the distance of the pivot point A to the stop 210 and point E preferably adjusts a force applied by the second bias member 200 about point A. A second bias member 300 is attached at a first end 310 to the housing 100 by member 110 and at a second end 320 to arm 40 as shown in FIG. 1 . The second bias member 300 applies a downward force onto the parallelogram 35 at point 320 , which is preferably intermediate arm 40 . The applied downward force directs the ground opening tool 80 into the ground 91 and is countered by the ground follower 90 .
[0061] One or more ground engaging apparatus 10 may be attached to a towing cross bar via towing attachment 400 thereby forming a ground engaging assembly. It will be appreciated that preferably there are a plurality of ground engaging apparatus 10 attached to a towing cross bar, which is attachable to a tractor, car, truck, horse, mule, ox or other means for pulling the ground engaging apparatus 10 . Preferably, a seed dispenser 82 such as a planting tube 83 is located adjacent to the ground opening tool 80 so that one or more seeds may be deposited within a channel or furrow 92 cut by the ground opening tool 80 when in use. Other substances may be deposited into the channel 92 , for example fertiliser and the like.
[0062] FIGS. 2 to 5 and 10 to 12 show side views and line diagrams of the ground engaging apparatus 10 in various configurations when traversing different ground levels and when retracted. In these configurations, points A and C are substantially vertically aligned and points B and D are substantially vertically aligned as shown and arms 30 , 40 pivot about points A, B, C and D. First bias member 200 maintains a constant applied downward breakout force that is countered by stop 210 . The second bias member 300 applies a downward force against the parallelogram 35 and a change in ground elevation 91 results in extension and retraction of a hydraulic cylinder of the second bias member 300 .
[0063] The parallelogram 35 is defined by points A, B, C and D and sides of the parallelogram comprise arms 30 , 40 , support plate 50 and shank support 60 . As shown in FIGS. 10-15 , points E, A and C form a first single linkage that is capable of uniform movement and points B, D and shank 60 form a second single linkage that is capable of uniform movement.
[0064] FIGS. 2 and 10 show the ground engaging apparatus 10 in a configuration wherein the ground engaging apparatus 10 is on level ground. As shown, the arms 30 , 40 are substantially parallel with the surface of the ground 91 and attachment points A and C are substantially aligned vertically with each other and attachment points B and D are also substantially aligned vertically with each other thereby forming a generally rectangular configuration of the parallelogram 35 . A downward second force 300 a applied by second bias member 300 directs the ground opening tool 80 into the ground 91 and is countered by the ground follower 90 . An applied breakout first force 200 a applies a force preventing the ground opening tool 80 from breakout unless a sufficient reaction breakout force 200 b is encountered as described hereinafter.
[0065] FIGS. 3 and 11 show a ground engaging apparatus 10 in a configuration wherein the ground engaging apparatus 10 is traversing a depression in the ground. In this configuration, arms 30 , 40 are pivoted downward thereby lowering points B and D respectively below points A and C. Points B and D are each attached to shank support 60 such that shank support 60 effectively forms an end of the parallelogram defined by points A, B, C and D. Accordingly, when the arms 30 , 40 are lowered as shown in FIG. 3 , shank support 60 is lowered thereby maintaining the ground opening tool 80 in the ground 91 . The shank 70 remains substantially vertical. The second bias member 300 is shown extended.
[0066] FIGS. 4 and 12 show the ground engaging apparatus 10 in a configuration when traversing risen ground 91 . The second bias member 300 is shown retracted and arms 30 , 40 are angled upward such that points B and D are above respective points A and C as shown.
[0067] FIG. 5 shows the ground engaging apparatus 10 retracted such that the ground opening tool 80 no longer contacts the ground 91 . This is useful, in particular, when a plurality of ground engaging apparatus 10 are attached to a support towing bar and only selected ground opening tools 80 are in use. This may be suitable for example when adjusting spacing between planting rows of a crop. The present invention has the advantage of being compact in horizontal length, preferably when the ground opening tool 80 is retracted. As shown, the shank support 60 is lifted substantially vertically with minimum or no outward horizontal extension of the shank 70 . This provides a compact configuration of the ground engaging apparatus 10 , which is advantageous when compared with other ground engaging apparatus. For example, this configuration is preferred if seed boxes are fitted as the boxes are maintained horizontally level.
[0068] FIGS. 6 to 8 and 13 to 15 show the ground engaging apparatus 10 in a configuration wherein the ground opening tool 80 encounters an obstacle such as a rock, branch, stump or the like. It is desirable that the ground opening tool 80 is moved away from the ground 91 and obstacle or obstruction to prevent or minimise damage to any part of the ground engaging apparatus. This movement of the ground opening tool 80 away from the ground 91 is referred to herein as a “breakout” or “breakaway” as the support plate 50 is rotated about point A thereby moving an end 51 of the support plate 50 away from the stop 210 . The first bias member 200 applies a breakout force 200 a as shown in FIGS. 9 and 10 - 15 that prevents the ground opening tool 80 from breaking away unless the ground opening tool 80 encounters a reaction force 200 b greater than the applied breakout force 200 a applied at point E by the first bias member.
[0069] FIGS. 6 and 13 show the ground engaging apparatus 10 in a breakout configuration when traversing level ground. An applied breakout force 200 a prevents the ground opening tool 80 from breakout unless a sufficient reaction breakout force 200 b is encountered, e.g. hitting an obstacle such as a rock or stump. When an obstacle is encountered, a reaction breakout force 200 b shown in FIG. 13 moves shank 70 as shown thereby shifting arm 30 rearward thereby causing the support plate 50 to rotate counter clockwise about point A. As the wheel 90 and shank 70 are attached to shank support 60 , the breakout force is transferred via a side of the parallelogram 35 defined by points B and D effectively as a single link as shown in FIG. 13 .
[0070] FIGS. 7 and 14 show the ground engaging apparatus 10 in a breakout configuration when traversing a depression and FIGS. 8 and 15 show the ground engaging apparatus 10 in a breakout configuration when traversing risen ground. Similar applied and breakout forces as previously illustrated are shown.
[0071] FIG. 16 shows another diagram representing the structural components of the invention with applied forces indicated. As shown in FIG. 16 , a first bias member applies a dominant breakout force 200 a to resist breakout away from abutment point 210 , which is represented in FIG. 1 as stop 210 . The breakout force 200 a is applied to a vertical link defined by points E, A and C, wherein point A is a fixed pivot point. A second bias means applies a smaller downward force 300 a to the parallelogram 35 , preferably via arm 40 . The second bias member 300 provides independent adjustment of the downward force 300 a without affecting the applied breakout force 200 a. In a preferred embodiment wherein the second bias member 300 comprises a hydraulic cylinder, another benefit is an ability to adjust the second bias member 300 without a need to manually adjust the mechanism.
[0072] First bias member 200 and second biased member 300 may comprise a spring, hydraulic cylinder or other bias member. Preferably, the first bias member 200 is a coiled spring and the second bias member 300 is a hydraulic cylinder as shown. Use of a hydraulic (or pneumatic) cylinder is advantageous in that adjustment of a force applied by the bias member may be performed remotely for one or more bias members by adjusting a fluid pressure. The fluid may be air, oil, water or any other suitable fluid. In a preferred form of the invention, in use a user is capable of driving a tractor that is towing one or more ground engaging apparatus 10 and the force of the first bias member 200 and/or second bias member 300 may be adjusted from the tractor without needing to manually adjusting an applied force for each bias member.
[0073] It will also be appreciated that the ground follower comprises a wheel, sled, cutting disc, roller or other suitable device. In one embodiment, the ground engaging apparatus comprises both a wheel and a cutting disc for slicing through weeds and other plant material in a path of the apparatus.
[0074] The ground opening tool comprises devises and configurations including for example seed shoes, plough shares, seed openers, furrow openers, disc openers, cutting edges and the like. It will also be appreciated that the present invention is preferably used with a seed dispenser such as a seed tube or planter tube that releases one or more seeds in a channel 92 formed by the ground opening tool 80 . Although there is no need to deposit any material in the channel, preferably seeds, fertiliser, wetting agent or other agricultural material is dispensed in the channel. The seeds may be for any crop, including for example, a vegetable or fruit including a cereal crop, wheat, rice, barley, corn, lettuce and the like.
[0075] Although the invention has been shown and described with exemplary embodiments thereof, it should be understood by those skilled in the art that the foregoing and various other changes, omissions and additions may be made therein and thereto without departing from the scope of the invention.
[0076] The disclosure of each patent and other document referred to in this specification is incorporated by reference in its entirety.
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A ground engaging apparatus ( 10 ) has a support plate ( 50 ) pivotally attached to a frame ( 100 ); a pair of arms ( 30, 40 ) interconnecting the support plate ( 50 ) and a shank support ( 60 ), which supports a shank ( 70 ) and ground follower ( 90 ) and first and second biasing rams or springs ( 200, 300 ), to maintain the ground follower ( 90 ); against the ground ( 91 ) but allow controlled break out of a ground opening, or tillage, tool ( 81 ) if an obstruction is engaged.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to gyroscopic reference systems of the type including a plurality of strapped-down force rebalanced gyroscopic rate sensors for measuring craft rotation rates about its primary axes, together with a digital computer for computing from such measures aircraft stabilization and attitude data, for example. More specifically, the invention relates to rate range switching and control apparatus for adapting the full range of the gyroscope analog rate output signal to a range consistent with the range of precision conversion of the analog signal into a corresponding digitally compatible signal, for example, consistent with the precision range of a voltage-to-frequency converter. The invention comprises circuit apparatus for providing a rate tracking gate voltage for protecting the solid state switching devices of the system from destructive voltages.
2. Description of the Prior Art
Strapped-down gyroscopic reference apparatus for aircraft and space vehicles is well known to those skilled in the art of gyroscopic aircraft control systems and many gyro configurations and control systems based thereon have been described extensively in the literature. In general, such systems include a plurality of single-degree-of-freedom or two-degree-of-freedom rate sensors strapped down to the vehicle (usually skewed with respect to the vehicle primary coordinate axes for redundancy purposes) for measuring the angular velocities of the vehicle about its primary coordinate axes which data, along with vehicle acceleration and heading data, is supplied to a digital computer to provide output data for use in stabilization, control, navigation, and guidance of the aircraft. Since the gyros are strapped to the airframe, it will be appreciated that the rate sensors will be of the force or torque rebalance type; that is, the gyro is maintained substantially aligned with its support case by feeding the gyro pick off signal back to the gyro torquer in a manner to maintain the pick off signal essentially null, the torquer current so required being a measure of the rate being sensed by the gyro. A typical two-degree-of-freedom rate sensor of this type is disclosed in the present assignee's U.S. Pat. No. 3,529,477.
It will be appreciated that the ultimate output signal of the sensor must be compatible with the requirements of digital computation. One way of accomplishing this might be to convert the gyro pick off signal, for example, to a duty-cycle-modulated square wave of a suitable frequency and to apply this signal to the torquer and together with suitable clock pulses provide a frequency count proportional to sensor rates. Another way would be to convert the gyro pick off signal to a proportional direct current and then to apply this current through the torquer to a precision resistor being used to produce a corresponding voltage and to apply this voltage as an input to a voltage-to-frequency converter to provide a frequency proportional to the sensed rate. The present invention relates to the latter conversion technique.
During normal operation of commercial aircraft, body rates are relatively low, being of the order of 0° to 30° per second. However, flight safety considerations dictate that the rate gyro be capable of measuring body rates greater than the aircraft design maximum; such rates may be on the order of 150° per second or more for commercial aircraft. Of course, military aircraft are designed to be capable of body rates of several hundred degrees per second and the strapped down rate gyros must be capable of sensing such rates for these applications. Thus, the range of torque feed back currents and the corresponding sensed voltages may be quite large. Also, the conversion precision of a voltage-to-frequency converter is, within reasonable circuit complexity and cost restraints, limited to a relatively narrow input voltage range, substantially smaller than the range of voltage corresponding to the full gyro torquer current range, so that if the full range of voltage resulting from the torquer current were applied to this converter it would saturate at the higher voltage levels.
The present invention overcomes the above conversion range deficiency by a unique switching circuit responsive to the gyro pick off signal for switching the torquer current between different voltage sensors so as to maintain the input voltage to the converter within the converter's precision range. Actuation of the switching means also alerts the digital computer that the range scale factor has been changed.
Depending upon the design of the rate range switching and control system, the solid state switching means may have to switch relatively high currents very rapidly, which factor severely limits the choice of available switches. For example, a switch that can handle the high currents may be restricted in terms of switching voltage; i.e., if the effective turn-on voltage exceeds a predetermined value, the switch will be destroyed. The present invention overcomes this difficulty by rate tracking circuit means which maintains the effective switch voltage substantially constant over the range of gyro rates.
SUMMARY OF THE INVENTION
The present invention provides automatic rate tracking switching and control apparatus for use, for example, in a digital strapped down inertial reference system for aircraft, which apparatus adapts the full range of the analog output signal of the system force rebalance rate sensors to a range consistent with the precision conversion of such a signal to a signal compatible with digital computation techniques; that is, consistent with the precision or linear conversion characteristics of a voltage-to-frequency converter.
The conversion of current flowing through the gyro torquer into digital data is provided by running the torquer current through a precision resistor and using the voltage developed across the resistor as the input to a voltage-to-frequency converter. The converter creates a frequency which is a function of its input voltage, and this frequency is counted and transmitted to the computer. The computer accumulates these numbers as aircraft rate data and integrates this data to determine aircraft attitude. In order to conduct the current required to null the gyro at abnormal or high maneuvering rates without exceeding the input range of the voltage-to-frequency converter, the resistance of the voltage sensor should be relatively small. However, achieving sufficient accuracy during normal cruising conditions requires a high value for the voltage sensing resistor. In order to accommodate these conflicting requirements, two differently valued sensing resistors are used. Normally, switches select the low rate sensor as the path for the torquer current and the input to the converter. However, if the output of the torquer amplifier exceeds a certain voltage, implying high maneuvering rates, then the switches select the high rate sensor.
The present invention overcomes a limitation of certain types of solid state switches employed to switch the rate voltage to the voltage-to-frequency converter. Many solid state switches have a limited range of voltage which they are capable of handling without damage. Therefore, the present invention provides a circuit whereby the rate gyro feed back voltage is tracked and is supplied to the switch elements to maintain their switching voltage ratios within the safe operating limits.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram showing a typical torque rebalanced rate gyroscope and a circuit diagram of the range rate switching system in association with an aircraft strapped-down inertial reference system, illustrating components thereof and their electrical interconnections.
FIG. 2 is a simplified schematic diagram illustrating the basic principles of the novel rate tracking switching circuit of FIG. 1.
FIGS. 3A and 3B together constitute a diagram of a preferred circuit for carrying out the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The tracking gate switch of the present invention is used for rate-range command switching, operating to facilitate the analog-to-digital conversion of the rate gyroscope outputs of an aircraft digital, strapped-down attitude and heading reference apparatus. The rate gyroscopes of such apparatus may be dual-axis, torque feed back flexure gyroscopes of the general kind described in U.S. Pat. Nos. 2,719,291 and 3,529,477, both assigned to Sperry Rand Corporation. These patents describe the structure and operation of typical tuned flexure rate gyroscopes. Such gyroscopes are characterized by having a gyroscopic rotor that is, in effect, freely suspended by flexure support members for spinning about a spin axis by means of an electric-motor-driven shaft journalled in the instrument casing. Universal tilting of the gyroscope rotor about a pair of axes perpendicular to the normal spin axis is permitted by the flexure support.
Such gyroscopic instruments are normally supplied with 90° spaced apart pairs of inductive pick offs for detecting angular displacement of the rotor with respect to its spin axis SA (FIG. 1) about mutually perpendicular inertial axes IA1 and IA2. Cooperating quadrature-spaced pairs of similarly disposed torquing coils are also normally present. In FIG. 1, purely as a matter of convenience, each such pair of torquer coils is schematically represented by respective single torquer coils 7, 8 and each such pair of inductive pick offs is schematically represented by respective single pick off coils 5, 6. Normally, the signal from pick off coil 6, for example, is kept at null by passing it through leads 18 and high gain amplifier 30 into torquer coil 7 to precess the gyroscope rotor 3 opposite to the precession caused by the input rate, thus keeping rotor 3 essentially aligned with the instrument casing 1, which case 1 is affixed to the craft 2. As noted, the rotor 3 is flexibly mounted on shaft 4 and is spun by a motor inside of the instrument casing 1. In a similar manner, the signal from the quadrature pick off coil 5 is nulled through the gyro restoring loop 20 via leads 16, 15 into torquer 8. It will be recognized, therefore, that the current driven into any one torquer coil 7 or 8 is proportional to the rate at which the gyroscope casing 1 is being rotated as the craft itself correspondingly rotates about a respective inertial axis IA1 or IA2. As the craft 2 on which the gyroscope is fixed rolls, for example, the gyroscope rotor 3 is maintained substantially fixed with respect to casing 1 by precessing rotor 3 in roll at the same rate that the craft is rolling. Consequently, craft roll rate, for example, can be precisely measured if the current passing through the corresponding torquer coil 7 or 8 is accurately measured.
In what follows, it will be understood by those skilled in the art that the control systems respectively associated with inertial axes IA1 and IA2 are substantially similar. The gyroscope rotor position-restoring loop 20 uses tilt signals derived with respect to axis IA2 by pick off 5 to supply precession signals via leads 15 to the IA1 axis torquer coil 8. Similarly, the gyroscope rotor restoring loop 21 uses tilt signals derived with respect to axis IA1 by pick off 6 to supply precession signals via leads 18, 17 to the IA2 axis torquer coil 7. Certain corresponding control signals are generated in gyroscope rotor position-restoring loops 20, 21 and appear at the respective junctions 23a, 24a, and 23b, 24b for use as will be further discussed. Since the control loops 20, 21 are of similar structure, only loop 21 need be discussed in detail. Elements coupled to terminals 23a, 24a of restoring loop IA1 are similar to those coupled to terminals 23b, 24b with respect to restoring loop IA2.
As shown in FIG. 1, the invention is represented in the form of the gyroscope rotor position-restoring loop 21 for axis IA2 and couples the output of pick off 6 via leads 18 and amplifier 30 into a lead branching at junction 50. The signal at terminal 50 is coupled to the level detector and rate control circuit 54 whose output appears on lead 55 and at terminal 24b and also at the input 53b of switch control 52. Control 52 determines whether the ganged switch blades 31, 32 respectively contact switch terminals 33, 35 or 34, 36. In practice, these devices will be wholly-electronic solid state switches. The output of level detector and rate control 54 is also coupled via lead 53a to a gain control input of torquer amplifier 30 to compensate for the change in load impedance seen by amplifier 30 when the sensing resistor 38 or 39 is changed.
The second lead branching at terminal 50 conducts the amplified pick off current through one of leads 17, torquer coil 7, and the second of leads 17 to the blade of switch 31. Terminals 33, 34 of switch 31 are respectively coupled to ground at junction 40 through precision calibrated resistors 38, 39. The terminals 33, 34 are also respectively coupled to switch terminals 35, 36 associated with the second switch blade 32 via the respective leads 41, 42. Blades 31, 32 are cooperatively positioned by a mechanical or other link, such as the conventional mechanical link 37 driven by switch control 52 to one extreme position or the other. The voltage on switch blade 32 is proportional to torquer current and is supplied as an input to the conventional voltage-to-frequency converter 51 which provides a frequency output at terminal 23b proportional to torquer current and hence to craft turn rate. It will be appreciated that the mechanical switches 31, 32 are in practice electronic solid-state switches such as semiconductor switches, as will be further discussed.
In the operation of the apparatus as thus far described, it is desired to convert the amplitude of the current flowing through torquer coil 7, for example, into data in a form compatible for use with a digital computer generally represented at 71. To convert the torquer current into a corresponding voltage, it is passed through one of the precisely calibrated sensor resistors 38 or 39. The voltage drop across the selected resistor is used as the input of the voltage-to-frequency converter 51. The converter 51 is a conventional device for generating an output signal whose frequency is proportional to its input voltage amplitude, and this frequency is supplied to a counter 68 whose output is coupled to a center frequency subtractor 58, whose output is in turn supplied to a digital computer 71. The computer accumulates the counts, which are proportional to craft rates about particular axes to provide aircraft rate stabilization signals p, q, and r at terminal 61a, and integrates them in the conventional manner to convert time to measures of craft altitude φ, θ and ψ at terminal 69a for conventional aircraft control and display purposes, such as at terminals 69a and 70a. The counting or sampling times for counter 68 are determined in a conventional manner by clock 75 which supplies timing signals to counter 68 via lead 76a. Similar clock signals at terminal 75a are used for synchronizing purposes yet to be discussed with respect to FIG. 3A. Clock 75 may also perform the timing of the operations of conventional functions in the usual way within computer 71.
In order to be capable of conducting the maximum current that may be required to null the position of gyroscope rotor 3 with respect to casing 1 at high craft turn rates without exceeding the input range for voltage-to-frequency converter 51, the resistance of the sensing resistor, such as resistor 38, should be small. However, a relatively high resistance value is required for the sensing resistor if sufficient accuracy is to be held during normal cruising conditions of the craft. Thus, to resolve this conflict, different resistance values are used according to the invention for sensing resistors 38, 39. For the low rates associated with craft cruising conditions, switches 31, 32 under control of level detector 54, select the high resistance sensing resistor 39 as the path for the current from torquer coil 7 for providing the input voltage to converter 51. However, when the output of power amplifier 30 exceeds a predetermined level, implying high craft-maneuvering rates, level detector 54 changes state and switch control 52 then control switches 31, 32 automatically to select the high rate or low resistance sensor resistor 38. In this manner, the input to the voltage-to-frequency converter is maintained within its linear conversion range without danger of saturation.
Voltage-to-frequency converter 51 is a conventional device capable of converting either positive or negative input voltages to corresponding distinguishable frequencies. For this purpose, the converter is appropriately biased to provide an effective "zero" frequency. In one form of the invention, a "zero" signal frequency of 40 kHz is produced for a zero voltage or zero rate input. Finite input voltages then develop a frequency change above or below the 40 kHz value. For example a +10 volt input may develop a 64 kHz output; on the other hand, a -10 volt signal at the input may develop a 16 kHz output. The frequency subtracter 58 is used in a conventional manner to remove the effect of the bias or center frequency by simply subtracting a count proportional to the center or effective "zero" frequency and to the sample time. If the converter 51 output frequency were counted say, for one second, then the frequency subtracter 58 would subtract, for example, 40,000 from the accumulated count. For the same example, the residual count would be +24,000 if the input was +10 volts, or -24,000 if the input was -10 volts. Obviously, for lower voltages, the count is proportionally reduced.
The foregoing residual count is now to be converted to determine the corresponding rotational increment for the one-second sample. However, which of the rate sensing resistors 38, 39 is selected must be accounted or compensated for in computer 71 in the conversion from counts to the corresponding angular rate value. A count of +24,000 indicates that the input to converter 51 was +10 volts, but this voltage corresponds to either of two different angular rates, depending upon which rate sensing resistor 38 or 39 is in the circuit. On this account, a signal is provided to computer 71 via lead 55 from the level detector rate control 54 defining which sensing resistor was engaged during the corresponding time and, thus, which of two scale factors is to be used in the computation by computer 71. By way of example, if the low rate sensing resistor 38 is selected by switch 31, +10 volts will be developed across resistor 38 at a turn rate of 20° per second, and a scale factor of 3 arc seconds per count will yield 20° per second for 24,000 counts per second. On the other hand, the high rate resistor 39 with +10 volts developed thereacross at a craft turn rate of 160° per second and the corresponding scale factor of 24 arc seconds per count will yield a 160° per second turn rate for 24,000 counts per second. In actual practice, other sampling periods, preferably much smaller, may be used, and the output data is further processed by computer 71 to provide the final aircraft control, display, and guidance functions.
In one form of the invention, the output of voltage-to-frequency converter 51 at terminal 23b may be, for example, supplied to a conventional frequency mixer or subtracter 58, where the center frequency is subtracted from the counter 68 output. The difference-frequency output of subtracter 58 is thus supplied via lead 60 to scale factor control 61 which by means of switch control 59 operated by level detector 54, operates to select the scale factor corresponding to which of the resistors 38, 39 is in the torquer circuit and to whether the count from subtracter 58 represents a low rate or a high rate.
The foregoing elements 59, 61 thus constitute compensator circuit means for rendering the output of counter 68 independent of which of the impedances 38, 39 is switched into the gyro torquer circuit and thus accounting for their different impedance values.
A significant problem encountered in the switching system for selecting one or the other of the rate sensor resistors 38, 39 lies in suitably controlling the torquer current path over the full range of voltages involved. The torquer current required to null the gyro output may be substantial; thus the current to be switched may likewise be large. This severely limits the number of suitable commercially available switches from which a selection may be made. The semiconductor switches that can safely handle the current level each have various other problems, such as a limited range of switching voltage. Of course, mechanical switches are not acceptable because of their very slow switching speeds.
The object of the present invention is to permit the selection and use of available semiconductor switches that have an otherwise undesirable voltage range limitation. For example, one switch acceptable as to current switching capability is a vertical gate MOSFET or VMOS switch manufactured by Siliconix, Inc. of Santa Clara, Calif. However, the gate-to-source voltage required to turn on such a switch is about +10 volts but the maximum value of the gate-to-source voltage is +15 volts. Because the source voltage may be as high as +10 volts, the gate voltage must be +20 volts to turn on this switch. With a +20 volt gate voltage, a source voltage falling below +5 volts will destroy the switch.
FIG. 2 presents an explanatory schematic of the invention showing a circuit for providing the desired tracking gate voltage required in preventing destruction of the semiconductor switch for controlling one of the sensors 38, 39 of FIG. 1 and for controlling but one of the gyro torquer currents. As in FIG. 1, there are present a gyro rotor 3, a torquer coil 7, pick off coil 6, torquer amplifier 30, level detector and rate control 54, and voltage-to-frequency converter 51 for supplying the variable frequency signal at terminal 23b, while resistor 81 corresponds to one of the sensors 38, 39. The output of torquer amplifier 30 is again supplied through junction 50 and through torquer coil 7 via leads 17 to the switching system; the output of amplifier 30 also controls circuit 54. Junction 50 is also coupled via junction 84 through series resistors 79, 78 to the power source terminal 77, the common junction between resistors 78, 79 being coupled through the source-drain circuit of JFET transistor 80. A series current path is supplied through torquer coil 7, the source-drain circuit of VMOS transistor 82, and resistor 81 to ground. The gate electrode of JFET transistor 80 is controlled by level detector circuit 54, as by lead 85, while the gate electrode of JFET transistor 83 is also controlled by circuit 54, as by lead 86. The source-drain circuit of the latter field effect transistor 83 is coupled to the junction between resistor 81 and transistor 82 to provide the sensed input voltage to voltage-to-frequency converter 51.
When the rate controller of circuit 54 supplies a predetermined switching signal via lead 85 to the gate electrode of transistor 80, its source-drain circuit is rendered conducting, and whatever control voltage is at the junction between resistors 78, 79 is coupled to the gate electrode of the VMOS transistor 82, switching the torquer current to resistor 81. The applied control voltage is generated by combining a voltage proportional to the current output of torquer amplifier 30 (the voltage across resistor 79) with a predetermined voltage across resistor 78 derived by a voltage source at terminal 77 arbitrarily selected as substantially the maximum possible gate reference voltage. When the current output of torquer amplifier 30 is at its maximum positive value, the voltage applied to the gate electrode of rate sensor switch transistor 82 may be about +22 volts, for example, while the source electrode voltage level of transistor 82 may be +10 volts, for example, yielding a difference voltage of 12 volts. Now, if the magnitude of the output of torquer amplifier 30 falls, the gate voltage at transistor 82 and the source electrode voltage are correspondingly reduced, so that the voltage between gate and source electrodes still remains relatively constant. For example, if the source electrode voltage is reduced to about 31 10 volts, the gate voltage will correspondingly fall to about -1 volt; accordingly, over the full range of possible source electrode voltages, the voltage rendering transistor 83 conducting is reasonably close to a constant +10 volts, safely within the voltage parameters of VMOS transistor 82. Such is accomplished by the action of the invention in tracking the rate gyroscope feed back current and in supplying a version of it to the switching elements so as to maintain voltages applied thereto within a safe operating range.
One embodiment of practical circuits within the level detector and rate control 54 and the switch control 52 of FIG. 1 appears in FIGS. 3A and 3B. The high and low rate sensing resistors 38, 39 appear at the low middle portion of FIG. 3B. FIG. 3A includes in series connection, an absolute value detector associated with amplifier 108, a level detector associated with amplifier 120 and flip-flop 128, and a rate select driver circuit associated with inverting amplifiers 129, 133 and transistors 144, 149. FIG. 3B depicts the circuits that select the rate sensing resistor of resistors 38, 39 that provides a current path from the low side of rotor torquer coil 7 to ground, the voltage sensed thereby being transmitted to voltage-to-frequency converter 51 of FIG. 1.
Referring first to FIG. 3A, the output of torquer amplifier 30 at terminal 50 is coupled through torquer coil 7 and terminal 115 to sensing resistors 38, 39 of FIG. 3B. Terminal 50 is also coupled through junction 101, diodes 100, 102, and resistors 104, 105 to the differential amplifier 108, the circuit being poled as indicated in the drawing to provide an absolute value detector. The positive and negative inputs of amplifier 108 are coupled to ground via resistors 103 and 109. Suitable low pass filtering is provided by a shunt capacitor-resistor circuit 106, 107. The absolute value detector is a conventional circuit adapted for rectifying both polarities of a bipolar input signal so that a signal of only one predetermined polarity appears across its output resistor 110. Thus, there is generated a positive signal to be sensed by the next following level detector circuit for either polarity of the torquer drive signal; accordingly, a single level detector circuit may be used to generate a high rate mode command for either positive or negative angular input rates.
The conventional level detector circuit associated with amplifier 120 has one input coupled to resistor 110 and a second input coupled through junction 119 and resistor 122 to a fixed positive reference voltage supply (not shown) at terminal 121 and also to ground through junction 119 and resistor 123. The two input are poled as indicated in the figure. The level detector compares the input voltage at resistor 110 from the absolute value detector with the reference voltage supplied at terminal 119. As long as the reference voltage on terminal 119 is greater than the input supplied by resistor 110, the low rate mode command of detector 120 is provided (+12 volts, for example). However, when the input signal from resistor 110 exceeds the voltage supplied to detector 120 from junction 119, detector 120 switches to its high rate mode command level. The high rate mode command (-12 volts) is equal to but opposite in polarity with respect to the low rate mode command (+12 volts).
The output of level detector 120 is coupled through series resistor 124 with respect to the shunting, grounded Zener diode 136 to one input of flip-flop 128, elements 124, 136 conveniently acting to limit the level detector output signals to +5 and zero volts, rather than the respective ±12 volts levels of the example thus far being discussed. A change-enabling pulse, which may be about 0.1 milliseconds long, is applied at a predetermined time at terminal 76b to the C input of flip-flop 128 to transfer the rate mode command selected by the level detector to one of the Q and Q outputs of flip-flop 128. Thus, through the subsequent circuits of FIG. 3A, the rate command switches 31, 32 respond to the selected rate, and computer 71 is at the same time informed via leads 126 and 55 (FIG. 1) so that switch control 59 will be controlled to select the appropriate scale factor via scale factor control 61.
It will be understood that flip-flop 128 of FIG. 3A is used because it is not permissible to change the computer counting rate during the sampling time. In other words, the counts passed to scale factor control 61 by counter 55 and by subtracter 58 must be for a full sampling time interval and not for a fraction thereof; otherwise, the rate output and the output of integrator 69 will have false values. The change-enabling pulse is provided on terminal 76b of converter 51 (FIG. 1) at each time a sampling period ends. Clock 75 may be the same clock as that which synchronizes computer 71. In the present configuration, clock 75 additionally supplies synchronizing pulses via lead 76b that determines the counting or sampling periods of counter 68. Consequently, a change-enabling pulse appears at lead 76b substantially at the end of each successive sampling time to set the output of flip-flop 128 for the next sampling period, flip-flop 128 holding this output steady until the end of that sampling time. For example, when the D input of flip-flop 128 is low, the level detector having requested a high rate command, the Q output of flip-flop 128 will command high rate switch selection by going low with the next change-enabling pulse from clock 75. Simultaneously, the Q output of flip-flop 128 goes high to notify computer 71 through lead 126 that the sample is a high rate sample.
The Q output of flip-flop 128 is coupled through inverting amplifier 129 to one terminal 134 of resistor 132 whose opposite terminal 127 is connected to a positive voltage source (not shown, but providing, say, +15 volts). The output junction 134 of amplifier 129 is also coupled through diode 135 to junction 119 associated with amplifier 120. The Q output of flip-flop 128 is similarly connected through a second inverting amplifier 133 to the intermediate junction 142 of a voltage divider consisting of series connected resistors 141 and 143. The terminal 140 of the voltage divider 141, 143 opposite the output of amplifier 133 is coupled to a positive supply (not shown) delivering, say, +26 volts. The amplifiers 129, 133 act as rate command drivers.
When the output at terminal Q of flip-flop 128 is high, the output of inverter-amplifier 129 is low, in effect grounding the intermediate junction 134 of the voltage divider involving resistor 132 and diode 135. In this high rate command condition, the reference voltage supplied for level detector 120 at junction 119 is reduced, because of the absence of the current path through diode 135 which is back biased to the value established by resistors 122, 123 at about one volt. On the other hand, when a low rate command is to be controlling, there is no output from amplifier 129, and the reference voltage at junction 119 associated with level detector 120 rises, because it now primarily depends upon the presence of diode 135 and of resistors 123, 122, and 132, to a level of about +8 volts. This change in the voltage level at junction 119 provides desirable hysteresis and accommodates a change in the high voltage that is supplied to torquer coil 7, when the rate mode command is changed.
The Q output of flip-flop 128 drives the rate command semiconductor switches located in FIG. 3B via amplifier-inverter 133. For this purpose, the intermediate terminal 142 is coupled to the base of a transistor 144 whose emitter is coupled to the positive voltage supply terminal 140 and whose collector supplies control signals to the low rate (L) command terminal 150. The collector of transistor 144 is coupled through resistor 145 to the base of transistor 149, whose collector is coupled by resistor 153 to a conventional power supply (not shown) connected to terminal 148 and also to the high rate (H) command terminal 151. The emitter of transistor 149 is coupled to a negative source (not shown) at terminal 146 held at about -20 volts, for example. The L and H signals are supplied from terminals 150, 151 to several locations in the switching circuit of FIG. 3B, as will be described, particularly to eight discrete terminals marked L or H therein.
When the Q output of flip-flop 128 is low (for a high rate), the output of amplifier 133 is high, causing transistors 144 and 149 to be non-conducting, thus setting the high rate or H voltage on terminal 151 at about +30 volts and the low rate or L voltage on lead 150 at -20 volts, for example. When the Q terminal is high, the output of amplifier 133 is low, thus causing transistors 144, 149 to conduct and making the L output +26 volts and the H output -20 volts, for example. The H and L values drive the rate sensing resistor selector switches of FIG. 3B as well as the gain changer in the torquer amplifier 30 of FIG. 1 so as to compensate for changes in load impedance seen by torquer amplifier 30 when the active sensing resistor 38 or 39 is changed.
It is observed that the switching circuit of FIG. 3B is controlled by the L and H signals and also receives the output of torquer amplifier 30 of FIG. 1 on terminal 116 and a signal corresponding to current flow through rotor torquer coil 7 at terminal 115. Except for the manner in which the input leads associated with terminals 115, 116 are laid out, the circuit of FIG. 3B has essentially mirror image symmetry qualities with respect to line A-B, the torquer amplifier signal of terminal 116 branching at 199 to couple to one of the respective ends of a pair of similar voltage dividers 200, 201 and 200', 201', the second respective end terminals 202, 202' of the voltage dividers being connected to a positive power supply (not shown) providing about +26 volts, for example. The torquer coil signal at terminal 115 is supplied via lead 231 to a bridge-like circuit 230 at line A-B and including the two sensing resistors 38, 39. The bridge-like circuit 230 includes in series connection lead 231, diode 212, the drain and source electrodes of field effect transistor 213, sensor resistors 38 and 39, the source and drain electrodes of a field effect transistor 213', diode 212', and lead 231. At lead 231, the circuit 230 is coupled to ground through capacitor 232. Between sensor resistors 38, 39, the circuit 230 is directly grounded at terminal 40. Diodes 212, 212' are poled as shown in the drawing and are similar devices, as are the transistors 213, 213', which as previously stated, are preferably VMOS devices.
The two mirror image sides of the switching arrangement are similar and, for that reason, equivalent components to the left and the right of circuit 230 are identified similarly, the reference numerals to the right being primed versions of those on the left. The voltage level at the tap between resistors 200, 201 is coupled in series through field effect transistor 208 to the gate of MOSFET 210. There is also a series current path through MOSFET 210 and diode 211, poled as illustrated, to lead 231. A further series current path flows from the tap of voltage divider 200, 201 through field effect transistor 221 to the gate electrode of MOSFET 213, being also coupled to ground at resistor 223.
The high rate command or H signals of terminal 151 are coupled in three places in the left part of FIG. 1, while the L signals of terminal 150 are used there only at one input. Thus, the L signals are coupled only through diode 203, poled as shown, to the gate electrode of transistor 205 and also through resistor 204 to the series lead between transistors 208 and 205.
The high rate command signals H on terminal 151 are first coupled through diode 206, poled as shown, to the gate of transistor 208 and through resistor 207 to the lead between the tap of voltage divider 200, 201 and transistor 208. Second, the H signals are coupled through diode 222 to the gate of transistor 221 and also through resistor 220 to the tap between voltage divider resistors 200, 201. Third, the H signals are coupled through diode 225, poled as shown, to the gate electrode of an output field-effect transistor 224. The other two electrodes of transistor 224 find themselves in a series output circuit coupled between transistor 213 and sensor resistor 38 to converter 51. The drain electrode of MOSFET 213 is coupled through resistor 226 between diode 225 and the gate of transistor 224. The other end of resistor 226 is also coupled to provide a current path through transistor 210 to resistor 226. The right part of FIG. 3B is similarly constituted, but H, rather than L signals, are supplied through diode 203', and L signals are supplied through diodes 206', 225', and 222' rather than the H signals coupled to diodes 206, 225, and 222. The output of transistor 224' and that of transistor 224 are united at junction 232 for alternative supply to converter 51.
Since the circuits of FIG. 3B for selecting one or the other of the high and low sensing resistors 38, 39 are substantially similar, only the operation of the circuit when the high rate H is commanded need be described. If the H signal at terminal 151 is +30 volts, for example, transistors 208, 221, 224, and 205' are conducting. At the same time, and L signal is -20 volts and drives transistors 205, 208', 221', and 224' into their non-conducting situation.
When transistors 208 and 221 are conducting, they connect the gates of the transistors 210 and 213 to the tap between voltage divider resistors 200, 201. Divider 200, 201 then provides a gate drive voltage about +10 volts higher, for example, than the voltage on lead 231, thus developing a +10 volt difference between gate and source electrodes of VMOS transistors 210 and 213, causing them to conduct. VMOS transistors 210' and 213' are then non-conducting, transistors 208' and 221' being non-conducting, removing the gate drive voltage and transistor 205' being conducting, ensuring a zero gate-to-source voltage difference. Then, the only path that the current flowing through torquer coil 7 has available is through sensor resistor 38, transistor 210, and diode 211 or through transistor 213 and diode 212, depending upon the polarity of the current. The voltage developed across the sensing resistor 38 is supplied by output transistor 224 to converter 51. In this case, output transistor 224' is held non-conducting, so that the second sensor resistor 39 is not connected to the input of converter 51. The operation of the circuit is correspondingly the same for a low rate command except that the states of the conducting and non-conducting switching transistors are each reversed from the described situation.
Accordingly, it is seen that the invention adapts the full rate range of a gyroscopic angular rate sensor to the more limited range of precision of a voltage-to-frequency converter by providing automatic rate range or scale factor switching. To accommodate the full range of angular rates, dual gyro torquer current sensors are employed for maintaining the input to the converter within its linear range. Simultaneously with switching the sensors, the digital computer is advised of the change in scale factor so that it can adjust its operation accordingly. The system provides novel rate tracking semiconductor switching circuit means adapted safely to control the torquer current over the full wide range of associated switching voltage values without destroying the switches and without requiring exotic and expensive switching devices.
While the invention has been described in its preferred embodiments, it is to be understood that the words which have been used are words of description rather than of limitation and that changes may be made without departing from the true scope and spirit of the invention in its broader aspects.
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An automatic rate range switching and control system adapts the full range of an analog output signal of a gyroscopic rate sensor to a range consistent with the precision conversion thereof into a digitally compatible signal. In a digital strapped down inertial reference system, for example, a plurality of strapped down, force-rebalanced rate sensors is used to sense aircraft body rates, wherein each gyro pick off signal is fed back to the gyro torquer in a manner to maintain the pick off signal essentially null, the torquer current signal thus being proportional to the sensed aricraft rate. The full range of the gyro's rate sensing capability may extend from zero to several hundred degrees per second. However, with the present invention, the switching and conversion of the analog rate signal into a digitally compatible signal is necessary only over a limited range. The current switching is accomplished by means of a rate tracing gate voltage rate switch for protecting the switching devices from destructively high switching voltages.
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BACKGROUND OF THE INVENTION
The invention relates to a coating machine for the processing of chocolate and similar masses, having a frame and bearing therein a circularly driven grating belt for the reception of the articles to be coated, which is guided by deflectors and has a tensioning device, and with pieces of the coating machine, especially a shaking device, arranged under the upper run of the grating belt. Such a coating machine serves to cover the articles on the grating belt with chocolate, the chocolate flowing in surplus through the coating machine penetrating the grating belt and coming into contact with many parts of the coating machine. It may be a coating machine which has a covering station in which the liquid chocolate reaches the articles in free fall. The coating machine may also have a bottom covering station and/or a blower to blow off any surplus chocolate. Masses other than chocolate, such as fat-containing masses, coating masses and, caramel masses may also be processed with such a coating machine.
When changing the mass in the coating machine, that is when a dark chocolate has been processed and the following articles are to be coated with a light chocolate or even a white coating mass, the problem to remove the previously processed mass and to clean all parts which have been in contact with this mass, so that the new mass, for example a white coating mass, can be used in the coating machine, arises.
It is known that in order to complete such a change of masses the coating machine including the previously processed mass is heated and emptied by removing the previously processed mass using a recovery pump. Then a cleaning mass such as cocoa butter or some other fatty solution is introduced into the coating machine. The coating machine is then put into action without any articles passing through, so that the cleaning mass is continuously recirculated and passes through the machine station. By this the cleaning mass reaches a large fraction of the parts of the coating machine contaminated with the old mass and cleans these more or less completely by melting off the old mass. But not all parts of the coating machine are reached by the cleaning mass, so that the cleaning action is incomplete. The cleaning mass is removed from the coating machine at the end of the cleaning and used in the normal production of chocolate. Afterwards the coating machine can be filled with the new coating mass.
It is further known to fashion major parts of the coating machine from stainless steel and to follow the emptying of the coating machine of the old mass with a wet-cleaning using pressurized hot water. This wet-cleaning is problematic in several aspects. When applying the stream of hot water onto the grating belt a considerable spraying and distribution action takes place, so that the pieces of the coating machine below the upper run are reached only incompletely. The hot water necessarily introduced into the coating machine during this cleaning procedure causes a contamination which creates favorable conditions for bacteria. To counteract this danger, it is known to conclude the wetcleaning by a blow-drying procedure with hot air. By this, too, the parts of the machine are heated, and the drying process is carried out for a correspondingly long time. But even so, not all parts of the machine are reached by the drying procedure, and there is no possibility to check whether all parts that had come into contact with the water have been dried.
In German patent application P 42 09 966.8 a tempering and coating machine for different masses, especially white and non-white chocolate, is described, in which a production line for articles has two coating machines assigned to it which can alternately be introduced into the production line, where one coating machine is determined to be used for dark coating masses and the other coating machine for light coating masses, and are provided thus, so that in this way a changing of the masses is avoided and the problem of changing the masses has been solved by using two seperate coating machines. This solution is possible only when there is enough room for the coating machines to the left and to the right of the production line, though. in many cases this room is not available, though, especially when several parallel production lines for articles are installed.
For the changing of masses in a coating machine it is also known to cut open the grating belt transversely to its direction of travel and thus to open the loop of the grating belt, so that the aggregates located below the upper run of the grating belt are well accessible for cleaning. Cleaning masses, which may consist of cocoa butter or, again, of hot water, have to be used for this cleaning. In this case, too, the cleaning is correspondingly cumbersome, elaborate, and unsure. Especially since the severed grating belt has to be reassembled.
SUMMARY OF THE INVENTION
The invention has the object to provide a coating machine of the above described type, in which the cleaning of the machine parts with a cleaning mass when changing the coating mass is possible with greater certainty and the pieces of the coating machine below the upper run of the coating machine are more accessible.
According to the invention this is achieved in the coating machine of the above described type in that the tensioning device has an extended tensioning travel enabling a lifting of the grating belt and that an apparatus is provided to support the lifted grating belt, to include supports for carriers on the frame of the coating machine.
The invention is based on the idea to fashion the grating belt in a liftable form and to support it with supports and carriers in the lifted state, so that the pieces of the machine below the upper run of the grating belt, for example a shaking device, a bottom-surge-station, a bottom-wipe-off roller and so on, are immediately accessible for cleaning with a cleaning mass, and cleaning therefore becomes easier, faster and more certain. The tensioning devices known also have a relatively small tensioning travel, as it is necessary when tensioning the grating belt to compensate for temperature influences. This tensioning travel is not enough to enable a lifting of the upper run of the grating belt in the relaxed state of the tensioning device. The tensioning travel has to be increased so that it becomes possible to lift up the closed loop of the grating belt in order to gain access from the side to the machine below the lifted grating belt. In order to secure the lifted state of the grating belt bearings are provided on the frame of the coating machine. To lift the grating belt, carriers, e.g. shafts, are inserted under the upper run of the grating belt after relaxing the tensioning device and the upper run is lifted with these. Preferably this is done at two well seperated places, at the beginning and the end of the coating machine for example. In the lifted state a distance of 20-30 cm is created between the raised run of the grating belt and the surface of the machine on which the grating belt travels, so that the cleaning mass may be directed onto the aggregates to be cleaned with a lance or nozzle in a direct way and without spraying through the grating belt. There is also the advantage of providing these pieces of the machine in a form that can easily be grasped and cleaned, e.g. also on the bottom sides, which up to now, when the grating belt is in its operating position, were not accessible. On the other hand the opening and laborious closing of the grating belt after the cleaning has become unnecessary. The cleaning should be performed with a cleaning mass, especially cocoa butter, and not with water, so that there is no danger of contamination.
Above the upper run of the grating belt a covering station and/or a blower may be arranged in a way that allows lifting, so that a space for the lifting and supporting of the grating belt is created. The covering station can consist of a curtain station, from which the liquid chocolate falls onto the articles on the grating belt and the articles are coated thus. Usually such a coating machine has a blower arranged after the covering station with which air is blown through a lip-like nozzle onto the articles treated under the covering station in order to remove excess chocolate from the articles and to return this excess through the grating belt to the recirculation cycle. It is also already known to fashion the covering station and/or the blower in a raisable way, including the help of motors or similar means, but this raisability is limited to adjustments with respect to the different heights of different articles to be coated on the grating belt. To create the space needed to raise and support the grating belt, so that the aggregates to be cleaned are readily accessible, the covering station and/or the blower must be arranged in a way that allows a comparatively much greater lift.
The blower can be arranged pivotably about a horizontal axis transverse to the direction of travel of the grating belt, so that, when the blower has been turned about said horizontal axis, the space for lifting and supporting of the grating belt is created. In principle such pivotable blowers are known. The pivotability has the object to exclusively change or adjust the angle at which air is blown onto the articles. With the new method of pivoting the blower, however, to create room for the raised grating belt, the blower or parts thereof are turned through an angle of about 90°, so that after the pivoting the necessary space for the grating belt is created.
It is also possible that one or both of the deflectors mounted at the ends is detachable in conjunction with or instead of an extended tensioning travel of the tensioning device. These one or two end-mounted deflectors often are comprised of a deflecting roller or a knife-edge rail, at which the grating belt is usually deflected at an acute angle. When this deflector or these deflectors can be removed, enough free length of the grating belt is created to lift the looped grating belt in the necessary amount and to support it at sufficient height on the supports of the frame of the coating machine so that the cleaning of the machines can be performed without problems. Primarily that deflector which is not driven will be formed to be detachable so that the detachability does not cause a lot of trouble. Usually one detachable deflector is sufficient, which should preferably be arranged at the intake end of the coating machine, in conjunction with the enlarged tensioning travel of the tensioning device, to achieve the intended lifting level of the grating belt.
It is also possible to provide one or both of the end-mounted deflectors on the frame of the coating machine to be pivotable. By this the required movability of the closed loop of the grating belt for lifting and supporting is also achieved. It is advantageous if one or both of the end-mounted deflectors also serves as the support for the lifted grating belt, so that the deflector rollers function as carriers at the same time.
It is further possible that one or both of the end-mounted deflectors are insertable into the supports on the frame of the coating machine and thus function as carriers for the lifted grating belt. By this the creation and use of special carriers for the grating belt is avoided. The rollers or rails which constitute the deflectors can simultaneously be used as carriers. The supports on the frame of the coating machine are then adapted correspondingly so that the distance is bridged by the imposed deflectors.
Essential parts of the coating machine positioned below the upper run of the grating belt which are accessible when the grating belt is raised, especially the plates of a dipping station of a bottom-covering station, can be arranged so that they are removable for cleaning purposes. This shows that the invention has the advantage of making it possible to form at least parts of the machine, which during the normal application of the coating machine are below the upper run of the grating belt, differently than has been realized in the state of the art. The trays of a dipping station of a bottom covering station, for instance, can be supported loosely, so that they are easily removed and cleaned on their back sides when the grating belt is raised. It is not necessary anymore to secure these trays with screws or even by welding. The same also holds for guide rails, parts of the tensioning device, bottom-wipe-off rollers, and/or parts of the usual shaking device.
The mixing chamber that is usually arranged beneath the lower run of the grating belt can have a connecting piece on its outlet side to be connected to a cleaning device working with a cleaning mass. This makes it possible to collect the cleaning mass in the mixing chamber during the cleaning and to withdraw it from the mixing chamber using the cleaning device or to recirculate the cleaning mass in this manner. When the connecting piece is arranged behind the return pump and provided with a valve, the return pump, which is normally used to transport the coating mass back to the tempering device, can advantageously be used to recirculate the cleaning mass through the cleaning device.
BRIEF DESCRIPTION OF THE DRAWINGS
The single FIGURE shows the parts of a coating machine relevant to the invention in a side view.
DETAILED DESCRIPTION
The coating machine has a frame 1, which is basically symmetric with respect to a logitudinal center plane of the coating machine. In the lower area the coating machine there is a grating belt 2 arranged in the form of a closed loop, which is driven by a drive roller 3 in the direction of the arrow 4. The grating belt 2 is shown in a bold dot-dashed line in its normal arrangement. It has an upper run 5 and a lower run 6. The upper run 5 extends from a deflector 7, which can be fashioned to be a rail or a roller, on the intake side to a deflector 8, which can also be fashioned to be a rail or a roller, on the outlet side. In the lower run 6 the grating belt 2 is lead via another deflector 9 to the drive roller 3. Following this is a tensioning device 10 with a tensioning roller 11. Further deflecting rollers 12 and 13 comlete the guidance of the lower run 6 until it reaches the deflector 7. The tensioning device 10 is shown in its normal tensioning position in a dashed line, while the solid line depicts the relaxed position. The length of the grating belt around the extreme positions of the tensioning roller 11 corresponds to twice the tensioning travel of the tensioning device 10.
During the normal operation of the coating machine the upper run 5 of the grating belt 2 will be approximately in the plane defined by the deflectors 7 and 8. Underneath the upper run 5 of the grating belt 2 different machine components are arranged. To clarify this a bottom covering station 14, a shaking device 15, a bottom-wipe-off station 16, as well as other not specified components are shown in an exemplary fashion. These components lie directly beneath the upper run 5 of the grating belt 2, and when the coating station is working properly, they come more or less into contact with the liquid coating mass, which then sticks to these parts, so that they have to be cleaned when the coating mass is changed. The bottom coating station 14 has a dipping roller 17, a bottom-surge-plate 18, as well as various plates 19 in the lower region, which also come into contact with the chocolate. The bottom of the grating belt 2 is surrounded by a tub 20, which in a hollow portion 21 extending downwards has a mixing chamber 22 with a mixing screw 23, in which the liquid chocolate is collected and recirculated in the known way by a circulating pump not shown.
In the upper region of the coating machine on the frame 1 a covering or coating station 24 is provided, whose essential component includes a curtain station 25, from which the chocolate pumped from the mixing chamber 22 falls onto the articles on the upper run 5 of the grating belt 2. The covering station 24 has a height-changing device 26, which is driven by a motor 27, to move the covering station 24 in a vertical direction. The covering station 24 is shown in a fully raised position, so that the curtain station 25 is separated by a large distance from the upper run 5 of the grating belt 2, which position is employed for cleaning only. Of course, when working with the coating machine, the curtain station 25 and the covering station 24 are in a much lower position, adjusted to the height and kind of articles to be coated on the grating belt 2.
In the direction of travel of the articles on the grating belt 2 a blower 28, which has a motor 29 for a turbine 30 to draw in and accelerate air, is arranged behind the coating station 24. The air is ducted through a hose 31 into a blower pipe 32 and streams through a nozzle-like lip 33 onto the articles just previously coated with liquid chocolate, so that the excess chocolate is blown off, passes through the upper run 5 of the grating belt 2 and flows through the tub 20 back into the mixing chamber 22. The blower 28 has a height-changing device 34 and the blower pipe 32 is arranged so that it is pivotable about a horizontal axis 35. The working position is depicted by the solid line. Swung by about 90° is the cleaning position, shown in dot-dashed line. By raising and/or swinging away the covering station 24 and/or the blower 28 a space 36 above the upper run 5 of the grating belt 2 is created, into which the grating belt 2 is lifted, when the components 14, 15, 16, 10 and so on are to be cleaned when changing the coating mass. The tensioning device 10 has to be relaxed beforehand, of course, so that at least the upper run 5 of the grating belt 2 is readily movable for lifting. In a corresponding height above the components 14, 15, and 16 supports 37, 38 are provided on the frame 1, which are arranged on both sides relative to the grating belt 2 on the frame 1. To facilitate the lifting and securing of the grating belt to the position shown by line 39, carriers 40 are inserted underneath the upper run 5 of the grating belt 2, after the tensioning device 10 has been relaxed. It is then, after raising the covering station 24 and/or swinging away the blower 28, possible to lift the carriers 40 and with these the grating belt 2, and to rest the carriers 40 in the supports 37 and 38. It is then, easy to approach components 14, 15, 16, 10, 3, 19, 20, so that cleaning is much more certain with the cleaning mass and can be done without the spraying effect through the grating belt 2. After the cleaning the cleaning mass is removed and the new coating mass can be put into the coating machine. The grating belt 2 is then lowered again, of course, and the tensioning device 10 supplies the necessary tension. The covering station 24 and the blower 28 are lowered into their normal operating positions, too.
A return pump 41 is connected to the mixing chamber 22 in the known way. In a pipe line 42 a valve 43 is provded, through which in its opened position the chocolate mass is normaly returned to a tempering device. The return pump 41 can also be used to empty the coating machine. The pipe line 42 is provided with a connecting piece 44 and a valve 45, to which a cleaning device 46 can be connected for cleaning with a cleaning mass when the valve 43 is closed, so that using the return pump 41 the cleaning mass can be recirculated. The cleaning mass is directed onto the machine components to be cleaned using a lance-like device, of course, and subsequently is returned to the mixing chamber 22.
One or both of the deflectors 7, 8 can be made to be removable and/or pivotable to replace or simplify at least partially the function of relaxing the tensioning device 10, so that the grating belt 2 is more readily movable for lifting. It is also possible, though, that the deflectors 7 and 8 are provided in a pivotable way on the frame 1, so that they can also take on the function of the carriers 40. Then it is either possible to do without the supports 37 and 38, because this function will be fulfilled also by the swung-up deflectors 7 and 8, or it is possible to put the rail- or roller-like deflectors 7 and 8 directly onto the supports 37 and 38, and to thereby maintain the grating belt 2 in the raised position during cleaning.
While a preferred embodiment of the invention has been disclosed in the foregoing specification and in the drawing, it will be apparent to those skilled in the art that variations and modifications thereof can be made without departing from the spirit and scope of the invention, as set forth in the following claims.
LIST OF REFERENCE NUMERALS
1-frame
2-grating belt
3-drive roller
4-arrow
5-upper run
6-lower run
7-deflector
8-deflector
9-deflecting roller
10-tensioning device
11-tensioning roller
12-deflecting roller
13-deflecting roller
14-bottom-coating station
15-shaking device
16-bottom-wipe-off roller
17-dipping roller
18-bottom-surge-plate
19-plate
20-tub
21-hollow
22-mixing chamber
23-mixing screw
24-covering station
25-curtain station
26-height-changing device
27-motor
28-blower
29-motor
30-turbine
31-hose
32-blower pipe
33-lip
34-height-changing device
35-axis
36-space
37-support
38-support
39-line
40-carrier
41-return pump
42-pipe line
43-valve
44-connecting piece
45-valve
46-cleaning device
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A coating machine for the processing of chocolate and similar masses having a frame and a circularly driven grating belt supported thereon for the reception of the articles to be coated. The grating belt is guided by deflectors and has a tensioning device. Coating machine components are arranged below the upper run of the grating belt. The tensioning device has an extended travel enabling the lifting of the grating belt. A plurality of supports are provided to support the lifted grating belt, the supports including carriers on the frame of the coating machine.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to polymer latices and more particularly to polymer latices which are prepared by polymerizing alpha, beta-ethylenically unsaturated monomers or mixtures of such monomers in the presence of a polymeric surfactant.
2. Brief Description of the Prior Art
Polymer emulsion products are prepared by polymerizing under free radical initiated polymerization conditions a polymerizable alpha, beta-ethylenically unsaturated monomer in water and in the presence of a low molecular weight emulsifier. The resulting polymers are high molecular weight and have been found useful in many applications including coatings applications. However, the low molecular weight emulsifiers have also been found to adversely affect the water sensitivity and adhesion of coatings prepared from such latices. To overcome these problems, it is known in the prior art to polymerize the polymerizable alpha, beta-ethylenically unsaturated monomer component in the presence of a polymeric surfactant which overcomes many of the problems associated with a low molecular weight emulsifier.
In accordance with this invention, it has been found that if polymerization is conducted with a particular type of polymeric surfactant and with specific mixtures of polymerizable alpha, beta-ethylenically unsaturated monomers, greatly improved polymer emulsion products can be obtained.
SUMMARY OF THE INVENTION
This invention provides for a latex polymer which has been formed by free radical initiated polymerization of a polymerizable alpha, beta-ethylenically unsaturated monomer component in aqueous medium in the presence of the salt of an acid group-containing polymer. The polymerizable alpha, beta-ethylenically unsaturated monomer component is a mixture of monomers which contains from 0.1 to less than 30 percent by weight of an epoxy group-containing alpha, beta-ethylenically unsaturated monomer.
Although not intending to be bound by any theory, it is believed that the epoxy monomer provides for a high degree of grafting of the monomer component onto the carboxylic acid group-containing polymer backbone via epoxy-acid reaction. This provides for a higher molecular weight polymer with improved properties over similar polymers without this mechanism of grafting.
DETAILED DESCRIPTION
The alpha, beta-ethylenically unsaturated monomer component is a mixture of monomers which is capable of free radical initiated polymerization in aqueous medium. The monomer mixture contains from 0.1 to less than 30, preferably 1 to 20, more preferably from 1 to 10 percent by weight of an epoxy group-containing alpha, beta-ethylenically unsaturated monomer such as glycidyl acrylate, glycidyl methacrylate and allyl glycidyl ether. When the amount of epoxy group-containing monomer is less than 0.1 percent by weight, there is insufficient grafting of the monomers to the acid group-containing polymer. As a result, the molecular weight of the polymer is lower than desired and the properties of coating compositions formulated with the polymeric latices are poorer. When the amount of epoxy group-containing monomer is greater than 30 percent by weight, there are problems with coagulation of the latex.
The other monomer in the mixture is preferably selected from vinylidene halides, with chlorides and fluorides being preferred; alkyl acrylates and methacrylates, vinyl esters of organic acids and alkyl esters of maleic and fumaric acid.
Among the vinylidene halides which can be used are vinyl chloride, vinylidene chloride, vinyl fluoride, vinylidene fluoride, tetrafluoroethylene, hexafluoropropylene and mixtures thereof.
Among the alkyl acrylate and methacrylates which can be used are those which contain from 1 to 20 carbon atoms in the alkyl groups. Examples include methyl acrylate, ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, methyl methacrylate, butyl methacrylate, 2-ethylhexyl methacrylate and the like.
Among the vinyl esters which can be used are vinyl acetate, vinyl versatate and vinyl propionate.
Among the esters of maleic and fumaric acid which can be used are dibutyl maleate and diethyl fumarate.
Besides the preferred comonomers mentioned above, other polymerizable alpha, beta-ethylenically unsaturated monomers can be used and include olefins such as ethylene and propylene; hydroxy functional monomers such as hydroxyalkyl esters of acrylic and methacrylic acid, for example, hydroxyethyl methacrylate and hydroxypropyl methacrylate; vinyl aromatic compounds such as styrene and vinyl toluene; vinyl ethers and ketones such as methyl vinyl ether and methyl vinyl ketone; conjugated dienes such as butadiene and isoprene; nitriles such as acrylonitrile; amides such as acrylamide and methacrylamide and alkoxyalkyl derivatives thereof such as N-butoxymethylmethacrylamide.
Since the epoxy group-containing vinyl monomer constitutes from 0.1 to less than 30, preferably from 1 to 20 percent by weight of the monomer component, the other monomer or monomers in the mixture constitute the remainder of the monomer component, that is, from greater than 70 to 99.9, preferably from 80 to 99 percent by weight, the percentage by weight being based on total weight of the monomer mixture. Preferably, at least 50 percent, more preferably from 60 to 99 percent by weight of the other monomers will be selected from the other preferred monomers with the vinylidene chlorides, fluorides and/or alkyl acrylates and methacrylates being the most preferred other monomers.
With regard to the amount of the alpha, beta-ethylenically unsaturated monomer component, it is usually used in amounts of from 5 to 95, preferably 25 to 75 percent by weight based on total weight of polymerizable alpha, beta-ethylenically unsaturated monomer component and salt of the acid group-containing polymer.
Among the acid-containing polymers which can be employed are virtually any acid-containing polymer which can be neutralized or partially neutralized with an appropriate basic compound to form a salt which can be dissolved or stably dispersed in the aqueous medium. Acid-containing polymers which may be employed include acid-containing acrylic polymers and copolymers, alkyd resins, polyester polymers and polyurethanes.
Acid-containing acrylic polymers are well known in the art and are prepared by polymerizing an unsaturated acid, preferably an alpha, beta-ethylenically unsaturated carboxylic acid with at least one other polymerizable monomer.
The unsaturated acid contains at least one polymerizable double bond and at least one acid group, preferably one CH 2 ═C< group, one carboxylic acid group and containing from 3 to 12 carbon atoms. Examples of suitable unsaturated acids include acrylic acid, methacrylic acid, crotonic acid, itaconic acid and C 1 to C 8 alkyl half-esters of maleic acid and fumaric acid including mixtures of acids.
The other polymerizable monomer contains at least one polymerizable double bond, preferably one CH 2 ═C< group. Examples of suitable polymerizable monomers include alkyl acrylates and methacrylates, vinylidene halides, vinyl esters and the other polymerizable alpha, beta-ethylenically unsaturated monomers mentioned above.
Polymerization of the monomers is usually conducted by organic solution polymerization techniques in the presence of a free radical initiator as is well known in the art.
The molecular weight of the resulting acid-containing acrylic polymers is usually between about 2000 to 50,000 on a number average molecular weight basis and the polymers have acid numbers of at least 50, usually between about 50 to 250.
Besides the acid-containing acrylic polymers, alkyd resins prepared by reacting an oil with a polycarboxylic acid or acid anhydride can also be used in the practice of the invention. Oils which may be used are drying oils which are esters of fatty acids which can be obtained from naturally occurring sources or by reacting a fatty acid with a polyol. Drying oils all contain at least a portion of polyunsaturated fatty acids.
Examples of suitable naturally occurring drying oils are linseed oil, soya oil, tung oil, tall oil esters, dehydrated caster oil, and the like.
The drying oils may also be obtained by reacting fatty acids with a polyol. Suitable fatty acids are oleic, linoleic and linolenic. Various polyols which can be used include butanediol, glycerol, trimethylolpropane, pentaerythritol and sorbitol. Also acid group-containing polyols such as dimethylolpropionic acid can be used. The drying oils can be modified with other acids including saturated, unsaturated or aromatic acids such as adipic acid, maleic acid, phthalic acid, or an anhydride of such an acid where it exists.
The polycarboxylic acid utilized in forming the alkyd can be an alpha, beta-ethylenically unsaturated dicarboxylic acid or its anhydride such as maleic acid, fumaric acid, itaconic acid, maleic anhydride and itaconic anhydride; an aromatic acid and a saturated dicarboxylic acid or their anhydrides where they exist such as phthalic acid, isophthalic acid, adipic acid, sebacic acid or the like. Mixtures of the same or different acids and anhydrides may also be utilized. Ordinarily, the acid and anhydride employed should contain from about 4 to about 10 carbon atoms, although longer chain compounds can be employed if desired.
In addition to acid-containing acrylic polymers and alkyd resins, conventional polyester resins formed by reacting a polyol and a polycarboxylic acid may be employed. Various polyols can be employed including ethylene glycol, propylene glycol, neopentyl glycol, glycerol, pentaerythritol, trimethylolpropane, and the like. Also acid group-containing polyols such as dimethylolpropionic acid can be used.
Various polycarboxylic acids may be employed including dicarboxylic acids such as phthalic acid, tetrahydrophthalic acid, hexahydrophthalic acid, maleic acid, itaconic acid, adipic acid, sebacic acid, and the like. Also, anhydrides of the polycarboxylic acids where they exist can be used.
The preparation of acid group-containing alkyd resins and polyesters is well known in the art and usually involves preparation in organic solvent with sufficient acid group-containing ingredients to form an acid group-containing material at the completion of the reaction.
In the case of alkyd and polyester polymers, a sufficient excess of the acid component is employed in forming the polymers to provide an acid value of from 10 to 120 with a preferred acid value being from 30 to 60.
Acid group-containing polyurethanes can also be used in the practice of the invention. These can be prepared by first preparing a polyurethane polyol and then reacting with a polycarboxylic acid or anhydride to introduce the necessary acid functionality into the polymer. Other examples of acid-containing polyurethanes are described in U.S. Pat. No. 3,479,310 to Dieterich et al and U.S. Pat. No. 4,147,679 to Scriven et al. The acid value of the polyurethane may range from 10 to 120, preferably 30 to 60.
The salt or partial salt of the acid-containing polymer is formed by neutralizing or partially neutralizing the acid groups of the polymer with an appropriate basic compound. Suitable basic compounds which may be utilized for this purpose include inorganic bases such as alkali metal hydroxides, for example, sodium or potassium hydroxide or organic bases such as ammonia or a water-soluble amine such as methylethanolamine or diethanolamine.
The degree of neutralization required to form the desired polymer salt may vary considerably depending upon the amount of acid included in the polymer, and the degree of solubility or dispersibility of the salt which is desired. Ordinarily in making the polymer water-dispersable, the acidity of the polymer is at least 25 percent neutralized with the water-soluble basic compound.
The amount of the salt of the acid group-containing polymer which is used in the polymerization is usually from 5 to 95, preferably 25 to 75 percent by weight based on total weight of polymerizable alpha, beta-ethylenically unsaturated monomer component and the salt of the acid group-containing polymer.
With regard to the conditions of polymerization, the polymerizable alpha, beta-ethylenically unsaturated monomer component is polymerized in aqueous medium with a free radical initiator and in the presence of the salt of the acid group-containing polymer. The temperature of polymerization is typically from about 0° C. to about 100° C., usually from about 20° to 85° C. and the pH of the aqueous medium is usually maintained from about 5 to about 12.
The free radical initiator can be selected from one or more peroxides which are known to act as free radical initiators and which are soluble in aqueous medium. Examples include the persulfates such as ammonium, sodium and potassium persulfate. Also, oil-soluble initiators may be employed either alone or in addition to the water-soluble initiators. Typical oil-soluble initiators include organic peroxides such as benzoyl peroxide, t-butyl hydroperoxide, and t-butyl perbenzoate. Azo compounds such as azobisisobutyronitrile can also be used.
The polymerization reaction may be conducted as batch, intermittent or a continuous operation. While all of the polymerization ingredients may be charged initially to the polymerization vessel, better results normally are obtained with proportioning techniques.
Typically, the reactor is charged with an appropriate amount of water, acid polymer salt and free radical initiator. The reactor is then heated to the free radical initiation temperature and charged with the monomer component. Preferably only water, initiator and part of the acid polymer salt and part of the monomer are initially charged to the reactor. After this initial charge has been allowed to react for a period of time, the remaining monomer component and acid polymer salt are added incrementally with the rate of addition being varied depending on the polymerization temperature, the particular initiator employed and the type and amount of monomers being polymerized. After all the monomer components have been charged, a final heating is usually done to complete polymerization. The reactor is then cooled and the latex recovered.
The following examples are submitted for the purpose of further illustrating the nature of the present invention and should not be construed as a limitation upon the scope thereof. Unless otherwise indicated, all parts and percentages in the examples are by weight.
EXAMPLES
The following examples, Examples A-G, show the preparations of salts of various carboxylic acid group-containing polymers which are used in subsequent examples for aqueous polymerization of vinyl monomer mixtures containing epoxy group-containing alpha, beta-ethylenically unsaturated monomers.
EXAMPLE A
A salt of a carboxylic acid group-containing acrylic polymer was prepared from the following mixture of ingredients:
______________________________________Ingredient Parts by weight (in grams)______________________________________Feed AAcrylic acid 160.9N--butoxymethylacrylamide 201.3 (61.5% active in 75/25 butanol-xylene mixture)Styrene 121.3Ethyl acrylate 831.7Feed XBenzoyl peroxide 15.8 (78% active)Methyl ethyl ketone 70.0Toluene 60.0Feeds B and Ct-butyl perbenzoate 6.02-butoxyethanol 6.0______________________________________
Butanol, 509 grams, was charged to a reactor and heated under a nitrogen atmosphere to reflux. Feeds A and X were added incrementally to refluxing butanol over a three-hour period. At the completion of the additions of Feeds A and X, Feed B was added and the reaction mixture held at reflux for two hours. Feed C was then added and the reaction mixture held at reflux for an additional two hours. The reaction mixture was then cooled and vacuum stripped (to remove any remaining unreacted monomers). The reaction mixture was then neutralized (54 percent total theoretical neutralization) by adding 73.5 grams of 28 percent aqueous ammonia and 73.5 grams of deionized water. The ammonia addition was beneath the surface and at a temperature of 68° C. The reaction mixture was held at 68° C. for 15 minutes followed by the addition of 1642.5 grams of deionized water. The reaction mixture was held at 70° C. for an additional 30 minutes and then cooled to room temperature. The resultant reaction mixture had a solids content (measured at 150° C.) of about 34 percent. The acrylic polymer had a weight average molecular weight (Mw) of 48,082 as determined by gel permeation chromatography using a polystyrene standard.
EXAMPLE B
A salt of a carboxylic acid group-containing acrylic polymer was prepared from the following mixture of ingredients.
______________________________________Ingredient Parts by weight (in grams)______________________________________Initial Reactor ChargeButanol 667.0Ethyl acetate 351.0Feed AEthyl acrylate 1769.9Methyl methacrylate 371.3Acrylic acid 334.2Feed XMethyl ethyl ketone 140.0Toluene 120.0Benzoyl peroxide 23.8 (78% active)Feed B28% aqueous ammonia 225.5Deionized water 147.0Feed CDeionized water 3285.0Feed DDeionized water 2400.0______________________________________
The procedure for preparing the acrylic polymer, neutralizing the polymer and dispersing the acrylic polymer salt in water is as generally described in Example A. The resultant dispersion had a solid content of about 28 percent. The acrylic polymer had a Mw of 36,201.
EXAMPLE C
A salt of a carboxylic acid group-containing acrylic polymer similar to Example B was prepared from the following mixture of ingredients:
______________________________________Ingredient Parts by weight (in grams)______________________________________Initial Reactor ChargeButanol 667.0Ethyl acetate 351.0Feed AEthyl acrylate 1769.9Acrylic acid 334.2Methyl methacrylate 371.3Feed A'Acrylic plasticizer 423.1Feed B28% aqueous ammonia 225.5Deionized water 147.0Feed CDeionized water 3285.0Feed DDeionized water 3000.0______________________________________
The acrylic plasticizer was prepared from the following ingredients:
______________________________________Ingredient Parts by weight (in grams)______________________________________Initial Reactor ChargeMonobutylether of diethylene glycol 600.0Butanol 320.0Feed AEthyl acrylate 2111.0N--butoxymethylacrylamide 184.6Methacrylic acid 22.7Styrene 22.7Feed XMonobutylether of diethylene glycol 135.0t-butyl perbenzoate 45.4Feeds B, C and DMonobutylether of diethylene glycol 13.5t-butyl perbenzoate 7.6______________________________________
The initial reactor charge was heated to reflux under a nitrogen atmosphere. Feeds A and X were added incrementally over a three-hour period. At the completions of Feeds A and X, Feed B was added and the dropping funnels were rinsed with monobutylether of diethylene glycol (16.9 grams total) and the rinse added to the reaction mixture which was held at reflux for an additional 11/2 hours, followed by the addition of Feeds C and D with a 11/2 hour hold at reflux between additions. The reaction mixture was then cooled to room temperature. The reaction mixture had a solids content of 65.5 percent and had a Mw of 11,332.
The procedure for preparing the acrylic polymer of Example C was as generally described in Example A with the acrylic plasticizer (Feed A') being added after the addition of Feeds A and X. Neutralization and dispersion in water was generally described in Example A. The resultant dispersion had a solids content of about 27 percent. The acrylic polymer had a Mw of 37,072.
EXAMPLE D
A salt of a carboxylic acid group-containing acrylic polymer similar to Examples B and C was prepared from the following mixture of ingredients:
______________________________________Ingredient Parts by weight (in grams)______________________________________Initial Reactor ChargeButanol 1018.0Feed AAcrylic acid 990.2Methyl methacrylate 742.6Ethyl acrylate 742.6Feed XMethyl ethyl ketone 140.0Toluene 120.0Benzoyl peroxide 63.2 (78% active)Feeds B and C2-butoxyethanol 12.0t-butyl perbenzoate 12.0Feed D28% aqueous ammonia 710.8Deionized water 147.0Feed EDeionized water 3285.0______________________________________
The procedure for preparing the acrylic polymer, neutralizing the polymer and dispersing the acrylic polymer salt in water is as generally described in Example A. The resultant dispersion had a solids content of about 35 percent. The polymer had a Mw of 25,642.
EXAMPLE E
A salt of a carboxylic acid group-containing acrylic polymer similar to Examples B, C and D was prepared from the following mixture of ingredients:
______________________________________Ingredient Parts by weight (in grams)______________________________________Initial Reactor ChargeButanol 458.1Feed AEthyl acrylate 746.3Acrylic acid 200.6Methyl methacrylate 167.1Feed XMethyl ethyl ketone 63.0Toluene 54.0Benzoyl peroxide 14.2Feeds B and C2-butoxyethanol 5.4t-butyl perbenzoate 5.4Feed D28% aqueous ammonia 84.6Deionized water 1600.0Feed EDeionized water 1600.0______________________________________
The procedure for preparing the acrylic polymer, neutralizing the polymer and dispersing the acrylic polymer salt in water was as generally described in Example A. The resultant dispersion had a solids content of about 35 percent. The polymer had a Mw of 13,535.
EXAMPLE F
A salt of a carboxylic acid group-containing polyurethane was prepared from the following mixture of ingredients:
______________________________________Ingredient Parts by weight (in grams)______________________________________Initial Reactor ChargePolyurethane polyol 644.3 (500 grams solids)Hexahydrophthalic anhydride 142.9Feed IIButanol 160.7Feed III28% aqueous ammonia 45.0Deionized water 81.1Feed IVDeionized water 677.6______________________________________
The polyurethane polyol was prepared by condensing trimethylhexamethylene diisocyanate with neopentyl glycol hexahydrophthalate and 1,6-hexanediol (25.67/49.84/24.49) weight ratio. The polyurethane dissolved in methyl isobutyl ketone had a solids content of 77.6 percent and a hydroxyl value of 80.73.
The carboxylic acid group-containing polyurethane was prepared by heating the initial reactor charge to 120° C. and holding at this temperature until the disppearance of anhydride groups as determined by Infra Red (IR) analysis. The methyl isobutyl ketone was vacuum stripped followed by the addition of Feed II. The reaction mixture was cooled to 70° C. followed by the addition of Feed III beneath the surface of the reaction mixture. The reaction mixture was then diluted with Feed IV. The resultant dispersion had a solids content of about 40.7 percent.
EXAMPLE G
A salt of a carboxylic acid group-containing alkyd resin was prepared as follows: A mixture of 581 grams of conjugated tall oil fatty acid (PAMOLYN 300 from Hercules Chemical Co.), 223.5 grams of isophthalic anhydride, 31 grams of xylene and 1.5 grams of dibutyl tin oxide were charged to a reaction vessel and heated to reflux to a stalled acid value (i.e. acid value of 2.6 to 2.8 as 85 percent by weight solution in dipropylene glycol monomethyl ether). The reaction mixture was cooled to 180° C. and 65 grams of maleic anhydride added. The reaction mixture was held for three hours at 200° C., cooled to 90° C., followed by the addition of 50 grams of water and the reaction mixture held at 93° C. until the disappearance of anhydride functionality as determined by IR. The reaction mixture was sparged with nitrogen for 15 minutes followed by the addition of 100 grams of diethylene glycol monobutyl ether. The reaction mixture was cooled to 50° C. and 90 grams of 28 percent aqueous ammonia and 50 grams of diethylene glycol monobutyl ether added. A mixture of 1400 grams of deionized water and 220 grams of diethylene glycol monobutyl ether was then added dropwise to the reaction mixture with vigorous stirring to solubilize the resin. The resin had a solids content of about 34 percent and an acid value of 23.0.
EXAMPLES 1-6
The following Examples 1-6 show the preparation, by aqueous latex polymerization techniques, of various vinyl chloride polymers and copolymers with glycidyl methacrylate and methyl methacrylate in the presence of salts of carboxylic acid group-containing acrylic polymers of Example A. The examples show the importance of polymerizing the vinyl chloride with small amounts of epoxy group-containing alpha, beta-ethylenically unsaturated monomers.
For all the examples, the polymerizations were conducted in a sealed reactor equipped with an agitator, a means for heating, cooling and purging with inert gas. In general, a reactor charge comprising a dispersion of the acrylic polymer salt and deionized water was first charged to the reactor, followed by the incremental addition of the monomers and the catalyst. The monomers were added to the reactor neat. When the pressure increased to about 150 psig, the monomer addition was stopped until the pressure decreased and then monomer addition was continued.
EXAMPLE 1
In this example, vinyl chloride was homopolymerized in the presence of the acrylic polymer salt of Example A as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeAcrylic polymer salt of Example A 1500 (33% solids)Deionized water 1200Monomer CnargeVinyl chloride 495Catalyst ChargeAmmonium persulfate 8Deionized water 72______________________________________
The reactor charge was added to the reactor and heated to 70° C. over 20 minutes. Seventy (70) grams of the catalyst solution was then added to the reactor and the vinyl chloride monomer was added slowly (200 grams/hour) and incrementally to the reactor while maintaining the pressure below 150 psig. The vinyl chloride addition was completed in 51/20 hours with intermittent stops because of excessive pressure build-up in the reactor. If addition were continuous, the vinyl chloride addition would have been completed in about 21/2 hours. Also, duing addition of the vinyl chloride, 10 grams of catalyst solution were added. After completion of the vinyl chloride addition, the temperature of the reactor was then raised to 78° C. and held at this temperature for about 2 hours to complete the polymerization. The latex was cooled to room temperature, the reactor vented and the latex removed from the reactor and vacuum stripped to remove residual vinyl chloride. The properties of the latex are reported in Table I below.
EXAMPLE 2
In this example, 90 percent by weight vinyl chloride was copolymerized with 10 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeAcrylic polymer salt of Example A 1200 (33% solids)Deionized water 960Vinyl Monomer ChargeVinyl chloride 356.4Glycidyl methacrylate 39.6Catalyst ChargeDeionized water 63Ammonium persulfate 7______________________________________
The reactor charge was added to the reactor and heated to 70° C. over a 20-minute period. As the reactor charge was being heated, the catalyst charge was added incrementally at the rate of 200 grams per hour. After the catalyst charge was added, the vinyl chloride monomer was then added continuously to the reactor at the rate of 200 grams per hour and the glycidyl methacrylate was added at 22.5 grams per hour. The addition of the monomers was continuous with the pressure in the reactor increasing to 140 psig but not exceeding 150 psig. At the time the monomer feeds were completed, the pressure had dropped to 100 psig. The temperature of the reactor was then increased to 78° C. and held for about 2 hours to complete the polymerization. The latex was cooled to room temperature and recovered as described in Example 1. The properties of the latex are reported in Table I below.
EXAMPLE 3
In this example, 95 percent by weight vinyl chloride was copolymerized with 5 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeAcrylic polymer salt of Example A 1457.5 (25.7% solids)Deionized water 702.5Vinyl Monomer ChargeVinyl chloride 376.2Glycidyl methacrylate 19.8Catalyst ChargeDeionized water 63Ammonium persulfate 7______________________________________
The latex was prepared as generally described above in Example 2 with the exception that the glycidyl methacrylate was added at the rate of 100 grams per hour. The properties of the latex are reported in Table I below.
EXAMPLE 4
In this example, 98 percent by weight vinyl chloride was copolymerized with 2 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeAcrylic polymer salt of Example A 1457.5 (25.7% solids)Deionized water 702.5Vinyl Monomer ChargeVinyl chloride 388.08Glycidyl methacrylate 7.92Catalyst ChargeDeionized water 63Ammonium persulfate 7______________________________________
The latex was prepared as generally described above in Example 3. The properties of the latex are reported in Table I below.
EXAMPLE 5
In this example, 99 percent by weight vinyl chloride was copolymerized with 1 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeAcrylic polymer salt of Example A 1457.5 (25.7% solids)Deionized water 702.5Vinyl Monomer ChargeVinyl chloride 392.02Glycidyl methacrylate 3.96Catalyst ChargeDeionized water 63Ammonium persulfate 7______________________________________
The latex was prepared as generally described above in Example 3. The properties of the latex are reported in Table I below.
EXAMPLE 6
In this example, 99.5 percent by weight vinyl chloride was copolymerized with 0.5 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeAcrylic polymer salt of Example A 1457.5 (25.7% solids)Deionized water 702.5Vinyl Monomer ChargeVinyl chloride 394Glycidyl methacrylate 1.98Catalyst ChargeDeionized water 63Ammonium persulfate 7______________________________________
The latex was prepared as generally described above in Example 3. The properties of the latex are reported in Table I below.
EXAMPLE 7
In this example, 90 percent by weight of vinyl chloride was copolymerized with 10 percent by weight methyl methacrylate in the presence of the salt of the acrylic polymer of Example A as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeAcrylic polymer salt of Example A 1200 (33% solids)Deionized water 960Monomer ChargeVinyl chloride 356.4Methyl methacrylate 39.6Catalyst ChargeAmmonium persulfate 7Deionized water 63______________________________________
The latex was prepared as generally described in Example 2 above with the exception that methyl methacrylate was used in place of glycidyl methacrylate.
The properties of the latex are reported in Table I below.
TABLE I__________________________________________________________________________Latex Properties of Examples 1-7 Weight % by Weight % by Weight AverageExample% by Weight Glycidyl Methyl Condition Molecular Film Properties.sup.3No. Vinyl Chloride Methacrylate Methacrylate of Latex % Solids.sup.1 Weight.sup.2 Appearance.sup.4 Wedge Bend.sup.__________________________________________________________________________ 51 100 0 0 good 30.3 39,432 cloudy complete delamination2 90 10 0 good 32.4 27,606 clear 67 mm (soluable fraction)3 95 5 0 good 29.8 2.1 × 10.sup.6 clear 29 mm4 98 2 0 slight 29.5 2.3 × 10.sup.6 clear 11 mm coagulum5 99 1 0 slight 29.6 41,804 clear 15 mm coagulum6 99.5 0.5 0 slight 29.2 5.9 × 10.sup.5 slightly 10 mm coagulum cloudy7 90 0 10 good 32.1 56,449 cloudy complete__________________________________________________________________________ delamination .sup.1 Percent solids measured at 110° C. .sup.2 Weight average molecular weight determined by gel permeation chromatography using polystyrene standard. .sup.3 Latices were formulated with dimethylethanolamine and the viscosit adjusted with water to 35 seconds as measured with a No. 4 Ford cup. .sup.4 The latices were drawn down over aluminum panels and then cured by heating to a peak metal temperature of 420° F. (216° C.) in 25 seconds to form films having a dry film thickness of about 0.35 mils. The appearance of the cured film was noted. .sup.5 The wedge bend test is conducted by first coating a 41/2 × 11/2 inch aluminum panel and bending the coated panel in the long direction over a 1/4 inch mandrel. The folded panel is then impacted (200 gram weight dropped 12 inches) to form a wedge shaped bend, i.e., flat at one end, 1/4 inch at the other end. The test panel is then immersed in an artificially sweetened citric acid flavored soft drink for 2 minutes. The crack in the film measured from the flat end in millimeters (mm) is recorded.
The results of the experiments summarized in Table I above show that by the increase in molecular weight of Examples 3-6 over Example 1 and 7, a graft copolymer is probably being formed. Although the molecular weight of the Example 2 is low, it was observed that this example had a high level of insoluble material which was filtered and not measured in the molecular weight determination. This high molecular weight insoluble fraction is also evidence of high levels of grafting.
The film properties also evidence increased levels of grafting with increasing glycidyl methacrylate levels. Clearer films and better wedge bend results indicate the formation of a more uniform high molecular weight graft copolymer.
EXAMPLES 8-14
The following Examples 8-14 show copolymerizing vinyl chloride, vinyl acetate and glycidyl methacrylate in which increasing amounts of glycidyl methacrylate and correspondingly decreasing amounts of vinyl chloride were used. The examples show the adverse effects of using too much glycidyl methacrylate. The examples were prepared in the reactor and in the manner generally described for Examples 1-6 above with the exception that the vinyl monomers were pre-emulsified with the acrylic polymer salt of Examples B and C in deionized water prior to polymerization.
EXAMPLE 8
In this example, 89.5 percent by weight vinyl chloride was copolymerized with 0.5 percent by weight glycidyl methacrylate and 10 percent by weight vinyl acetate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeAmmonium persulfate 4.28Deionized water 500Pre-Emulsified Monomer ChargeAcrylic polymer salt of Example B 1200.2 (33.7% solids)Vinyl acetate 94.3Glycidyl methacrylate 4.71Deionized water 1156.20Vinyl chloride 844.2______________________________________
The vinyl acetate and glycidyl methacrylate were first pre-emulsified by adding them to a solution of the acrylic polymer and deionized water. The vinyl chloride was then pumped into the tank containing the pre-emulsified vinyl acetate and glycidyl methacrylate. When all the vinyl chloride had been pumped into the tank containing the other pre-emulsified monomers, 400 grams of the pre-emulsified monomer charge were then added to the reactor along with the reactor charge. The ingredients in the reactor were heated to 70° C. over 20 minutes, followed by the incremental addition of 2600 grams of the remaining pre-emulsified monomer charge which was completed in a period of about 3 hours. During the addition of the pre-emulsified monomer charge, the temperature of the reactor was kept at 70° C. and the pressure remained below 85 psig. At the completion of the pre-emulsified monomer charge, the reactor was heated to 78° C. and held for 2 hours to complete the polymerization. The resulting latex was then cooled and recovered as described in Example 1. The properties of the latex are reported in Table II below.
EXAMPLE 9
In this example, 87 percent by weight vinyl chloride was copolymerized with 10 percent by weight vinyl acetate and 3 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeDeionized water 500Ammonium persulfate 4.04Pre-Emulsified Monomer ChargeAcrylic polymer salt of Example B 1241.93 (27.9% solids)Vinyl acetate 80.85Glycidyl methacrylate 24.25Deionized water 1229.50Vinyl chloride 703.4______________________________________
The latex was prepared as generally described above in Example 8. The properties of the latex are reported in Table II below.
EXAMPLE 10
In this example, 85 percent by weight vinyl chloride was copolymerized with 10 percent by weight vinyl acetate and 5 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeDeionized water 571.4Ammonium persulfate 4.4Pre-Emulsified Monomer ChargeAcrylic polymer salt of Example C 1491.52 (27.5% solids)Vinyl acetate 88.0Glycidyl methacrylate 44.0Deionized water 1408.0Vinyl chloride 748.0______________________________________
The latex was prepared as generally described above in Example 8. The properties of the latex are reported in Table II below.
EXAMPLE 11
In this example, 80 percent by weight vinyl chloride was copolymerized with 10 percent by weight vinyl acetate and 10 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeDeionized water 500.0Ammonium persulfate 4.28Pre-Emulsified Monomer ChargeAcrylic polymer salt of Example B 1199.5 (33.7% solids)Vinyl acetate 94.32Glycidyl methacrylate 94.32Deionized water 1166.8Vinyl chloride 754.6______________________________________
The latex was prepared as generally described above in Example 8. The properties of the latex are reported in Table II below.
EXAMPLE 12
In this example, 70 percent by weight vinyl chloride was copolymerized with 10 percent by weight vinyl acetate and 20 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeDeionized water 500.0Ammonium persulfate 4.28Pre-Emulsified Monomer ChargeAcrylic polymer soap of Example B 1199.5 (33.7% solids)Vinyl acetate 94.32Glycidyl methacrylate 188.64Deionized water 1166.8Vinyl chloride 660.27______________________________________
The latex was prepared as generally described above in Example 8. The properties of the latex are reported in Table II below.
EXAMPLE 13
In this example, 60 percent by weight vinyl chloride was copolymerized with 10 percent by weight vinyl acetate and 30 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeDeionized water 500Ammonium persulfate 4.28Pre-Emulsified Monomer ChargeAcrylic polymer salt of Example B 1199.5 (33.7% solids)Vinyl acetate 94.32Glycidyl methacrylate 282.96Deionized water 1166.8Vinyl chloride 565.96______________________________________
The latex was prepared as generally described in Example 8. The properties of the latex are reported in Table II below.
EXAMPLE 14
In this example, 40 percent by weight vinyl chloride was copolymerized with 10 percent by weight vinyl acetate and 50 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeDeionized water 500Ammonium persulfate 4.28Pre-Emulsified Monomer ChargeAcrylic polymer salt of Example B 1448.9 (27.9% solids)Vinyl acetate 94.32Glycidyl methacrylate 471.75Deionized water 907.72Vinyl chloride 377.40______________________________________
The latex was prepared as generally described above in Example 8. The properties of the latex are reported in Table II below.
TABLE II__________________________________________________________________________Latex Properties of Examples 8-14 % by Weight % by WeightExample% by Weight Vinyl Glycidyl Condition Film Properties.sup.1No. Vinyl Chloride Acetate Methacrylate of Latex % Solids Appearance Wedge Bend__________________________________________________________________________8 89.5 10 0.5 good 34.8 clear 21 mm9 87 10 3 good 30.3 clear 20 mm10 85 10 5 good 29.7 clear 15 mm11 80 10 10 good 34.4 clear 26 mm12 70 10 20 some 34.9 clear 28 mm coagulation13 60 10 30 gelled -- -- --14 40 10 50 gelled -- -- --__________________________________________________________________________ .sup.1 Latices were thickened and viscosity adjusted as generally described in Table I. Also, 5 percent by weight of an aminoplast crosslinker CYMEL 1116 (from American Cyanamid Co.) was added to the latices.
The results of the experiments summarized in Table II above show that the use of glycidyl methacrylate at levels of 30 percent or more by weight result in coagulation of the latex.
EXAMPLES 15-16
The following Examples 15-16 show the preparation of copolymers of glycidyl methacrylate with monomers other than vinyl chloride. The procedure for preparing the latex copolymers was as generally described above in Examples 8-14 with the exception that the other vinyl monomers were used in place of vinyl chloride.
EXAMPLE 15
In this example, 98 percent by weight vinylidene chloride was copolymerized with 2 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeDeionized water 500Azobisisobutyronitrile (VAZO 64 10from E. I. du Pont de Nemours)Pre-Emulsified Monomer ChargeAcrylic polymer salt of Example D 811.09 (35.6% solids)Vinylidene chloride 673.5Glycidyl methacrylate 13.50Deionized water 1780.7______________________________________
The resultant acrylic polymer had a Mw of 178,149.
EXAMPLE 16
In this example, 97 percent by weight styrene was copolymerized with 3 percent by weight glycidyl methacrylate as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeDeionized water 500.0Ammonium persulfate 5.0Pre-Emulsified Monomer ChargeAcrylic polymer salt of Example E 1167.6 (34.8% solids)Styrene 943.25Glycidyl methacrylate 28.29Deionized water 1189.15______________________________________
The resultant acrylic polymer had a Mw of 706,197.
EXAMPLES 17-18
The following Examples 17-18 show the preparation of copolymers of glycidyl methacrylate and styrene by latex polymerization in the presence of salts of carboxylic acid group-containing polyurethanes and salts of carboxylic acid group-containing alkyd resins. The procedure for preparing the latex copolymer was as generally described above in Examples 8-14 with the exception that the polyurethane and alkyd resin salts were in place of the acrylic polymer salts.
EXAMPLE 17
In this example, 97 percent by weight styrene was copolymerized with 3 percent by weight glycidyl methacrylate in the presence of a salt of a carboxylic acid group-containing polyurethane of Example F as follows:
______________________________________Ingredient Parts by Weight (in grams)______________________________________Reactor ChargeDeionized water 215.0Ammonium persulfate 1.31Pre-Emulsified Monomer ChargePolyurethane surfactant of 434.4 (40.7% solids)Example FStyrene 254.63Glycidyl methacrylate 7.88Deionized water 588.8______________________________________
The styrene and glycidyl methacrylate were first pre-emulsified by adding them to a solution of the polyurethane polymer and deionized water. The reactor charge was added to the reactor and heated to 78° C. The pre-emulsified monomer charge was added over a three-hour period, after which the mixture was held for two hours at 78° C. The percent conversion was 84 percent.
Example 18
In this example, 99 percent by weight styrene was copolymerized with 1 percent by weight glycidyl methacrylate in the presence of a salt of the carboxylic acid group-containing alkyd resin of Example G as follows:
______________________________________Pre-Emulsified Monomer ChargeIngredient Parts by Weight (in grams)______________________________________Alkyd salt of Example G 397.05 (34% solids)Styrene 311.50Glycidyl methacrylate 3.15Deionized water 707.95______________________________________
The styrene and glycidyl methacrylate were first pre-emulsified by adding them to a solution of the alkyd polymer and deionized water. Three hundred (300) grams of this pre-emulsified monomer charge was added to the reactor and heated to 78° C. Twenty (20) grams of a 10 percent ammonium persulfate solution was added. The mixture was held for 1/2 hour and then the remaining pre-emulsified monomer charge was added over three hours. The mixture was held for two hours at 78° C. The percentage conversion was 94 percent.
The results of Examples 15-18 show that monomers other than vinyl chloride can be successfully copolymerized with glycidyl methacrylate and that salts of polymers other than acrylic polymers can be used as surfactants in the graft copolymerization process.
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Polymeric latices formed by free radical initiated polymerization of a polymerizable alpha, beta-ethylenically unsaturated monomer component which contains from 0.1 to less than 30 percent by weight of an epoxy group-containing alpha, beta-ethylenically unsaturated monomer in aqueous medium and in the presence of a salt of an acid group-containing polymer are disclosed. The resultant polymeric latices have higher molecular weights than polymeric latices prepared without the epoxy group-containing alpha, beta-ethylenically unsaturated monomer. The polymeric latices are useful as resinous binders in coating compositions where they provide for excellent adhesion and flexibility in the coating.
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CROSS-REFERENCE TO RELATED PATENT APPLICATION
[0001] This application claims the benefit of Korean Patent Application No. 10-2005-0069115, filed on Jul. 28, 2005, in the Korean Intellectual Property Office, the disclosure of which is incorporated herein in its entirety by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a data recording medium and method of manufacturing the same, and more particularly, to a ferroelectric recording medium and method of manufacturing the same.
[0004] 2. Description of the Related Art
[0005] As internet technology develops, demand for recording media which can record a huge amount of information such as moving pictures, in particular, portable recording media, has increased. This demand is an important factor leading the next-generation information recording media market.
[0006] Recording media which can record a huge amount of information and devices for recording and reading information in the recording medium are the most essential issues for the information recording media market.
[0007] Portable, non-volatile data recording devices are classified into solid-state memory devices, for example, flash memory, and disk type memory devices, for example, hard disks.
[0008] Since the capacity of solid-state memory devices will only increase up to several gigabites (GB) in the next several years, solid-state memory devices may not be used as large data recording devices whose capacity must be greater than several gigabites in the near future. However, solid-state memory devices may be used for high speed apparatuses such as personal computers (PC). For the time being, hard disk type memory devices may be used as a main recording apparatus.
[0009] A typical magnetic hard disk mounted in a portable apparatus will have a capacity of 10 GB in the near future, but a capacity of more than 10 GB may not be accomplished due to a superparamagnetic effect.
[0010] A memory device using a scanning probe technique for recording data and using a ferroelectric material as a recording material has been developed. When using the scanning probe technique, i.e., a scanning probe microscope (SPM) technique, an area of several to tens of nanometers can be probed by a probe. In addition, since a ferroelectric material is used as a recording medium, a superparamagnetic effect will not occur, unlike in a magnetic recording medium. The recording density in the recording device using ferroelectric material can be greater than in the magnetic recording medium.
[0011] In the recording medium using an SPM technique, recorded data are defined by the polarity of the polarization of the ferroelectric material.
[0012] Due to ferroelectric polarization, an electric field is emanating from the surface. When an appropriate probe is placed into that field, the field induces a charge depletion or accumulation region at the apex of the tip. This in turn induces a capacitance or resistance change of the probe. Depending on the polarity of the ferroelectric polarization, the resistance or capacitance is increased or decreased. Data recorded on a ferroelectric recording medium using the SPM technique can be read by measuring the change in the capacitance or resistance of the probe. Writing is done by locally changing the ferroelectric polarization of the medium. This is done by applying an electric voltage to the probe, where the voltage is high enough to induce ferroelectric switching in the medium.
[0013] As described above, a ferroelectric recording medium using an SPM can have higher data recording density than a magnetic recording medium. However, it should be considered that the region of one bit data recording is a polarized area. In order to further increase a data recording density of a ferroelectric recording medium, the size of the bit data recording region in a ferroeletric recording medium should be reduced.
[0014] However, since the reduction in the size of the bit data recording region is very much dependent on the reduction of the probe size, a further increase of the data recording density of the ferroelectric recording medium will be difficult unless epoch-making technology for reducing the probe size is developed.
SUMMARY OF THE INVENTION
[0015] The present invention provides a ferroelectric recording medium with an increased data recording density.
[0016] The present invention also provides a method of manufacturing the ferroelectric recording medium having an increased data recording density.
[0017] According to an aspect of the present invention, there is provided a ferroelectric recording medium including: a substrate; a patterned supporting layer which is formed on the substrate, the patterns having at least two lateral surfaces; and data recording layers formed on the lateral surfaces of the patterns.
[0018] The data recording layers may include several data recording layers disposed on the lateral surfaces of the patterns of the supporting layer. The patterns of the supporting layer may have a polygonal shape having at least three lateral surfaces or may be a bar type.
[0019] A plurality of patterns may be formed on the substrate and disposed at uniform intervals.
[0020] The supporting layer may be formed of one or more selected from the group consisting of but not limited to titanium dioxide (TiO 2 ), vanadium dioxide (VO 2 ), niobium dioxide (NbO 2 ), zirconium dioxide (ZrO 2 ), oxides of iron, titanium nitride (TiN), vanadium nitride (VN), niobium nitride (NbN), zirconium nitride (ZrN), iron nitride (Fe 2 N), strontium oxide (SrO), strontium nitride (Sr 2 N 3 ), tantalum oxide (Ta 2 O 5 ) and tantalum nitride (Ta 2 N). The supporting layer may also be formed of one or more selected from the group consisting of titanium (Ti), vanadium (V), niobium (Nb), zirconium (Zr), iron (Fe), strontium (Sr) and tantalum (Ta).
[0021] The data recording layers may be formed of one selected from the group consisting of but not limited to lead zirconate titanate (PZT), strontium bismuth tantalate (SBT), strontium bismuth titanate (SBT) lithium titanate (LTO), lithium tantalate (LTO), strontium bismuth niobate (SBN), lead titanate (PTO), bismuth ferrite (BFO), bismuth titanate (BTO), and potassium niobate (KNO).
[0022] According to another aspect of the present invention, there is provided a method of manufacturing a ferroelectric recording medium, the method including: forming a supporting layer on a substrate; patterning the supporting layer into patterns having at least two lateral surfaces; forming source material layers on the lateral surfaces of the patterns; and diffusing a source material into the patterns of the supporting layer and reacting the source material with the material of the supporting layer. To trigger the reaction between the source material and the material of the supporting layer, and for diffusion, a temperature of 400° C. or more may be used.
[0023] The source material layers may be formed of a material that reacts with the material of the supporting layer to form a layer formed of one selected from the group consisting of but not limited to PZT, strontium bismuth tantalate (SBT), strontium bismuth titanate (SBT), lithium titanate (LTO), lithium tantalate (LTO), strontium bismuth niobate (SBN), PTO, BFO, BTO, and KNO on the lateral surfaces of the patterns. The basis for the source material may be, but is not limited to lead (Pb), potassium (K), bismuth (Bi), or lithium (Li).
[0024] According to another aspect of the present invention, there is provided a method of manufacturing a ferroelectric recording medium, the method including: forming a supporting layer on a substrate; forming a mask on the supporting layer to define a portion of the supporting layer; etching the supporting layer around the mask which produces patterns; placing the etched product in a gas atmosphere including a source material gas that reacts with the lateral surfaces of the patterns and diffuses into the pattern to form a ferroelectric lateral layer. To trigger the reaction between the source material and the material of the supporting layer, and for diffusion, a temperature of 400° C. or more may be used.
[0025] In the forming of the mask, the supporting layer may be defined into patterns of polygonal shapes having at least three lateral surfaces or may be a bar type.
[0026] The supporting layer may be formed of one or more selected from the group consisting of but not limited to TiO 2 , VO 2 , NbO 2 , ZrO 2 , oxides of iron, TiN, VN, NbN, ZrN, Fe 2 N, SrO, Sr 2 N 3 , Ta 2 O 5 and Ta 2 N. The supporting layer may also be formed of one or more selected from the group consisting of but not limited to Ti, V, Nb, Zr, Fe, Sr and Ta.
[0027] The source material gas may be a material gas that reacts with the supporting layer to form a layer formed of one selected from the group consisting of but not limited to PZT, strontium bismuth tantalate (SBT), strontium bismuth titanate (SBT), lithium titanate (LTO), lithium tantalate (LTO), SBN, PTO, BFO, BTO, and KNO on the lateral surfaces of the supporting layer. The basis for the source material gas may be, but is not limited to Pb, K, Bi, or Li.
[0028] To trigger the reaction between source material and the material of the supporting layer, and for diffusion the fabrication may be performed at 400° C. or more. At the end, a final heat treatment using for example a rapid thermal annealing (RTA) process may be applied.
[0029] The ferroelectric recording medium has a high data recording density and offers high speed data recording and reading capabilities.
BRIEF DESCRIPTION OF THE DRAWINGS
[0030] The above and other features of the present invention will become more apparent by describing in detail exemplary embodiments thereof with reference to the attached drawings in which:
[0031] FIG. 1 is a perspective view of a ferroelectric recording medium according to a first exemplary embodiment of the present invention;
[0032] FIG. 2 is a perspective view of a ferroelectric recording medium according to a second exemplary embodiment of the present invention;
[0033] FIG. 3 is a cross-sectional view of the ferroelectric recording medium taken along the line 3 - 3 ′ of FIG. 1 or 2 ;
[0034] FIGS. 4 through 8 are cross-sectional views illustrating steps in a method of manufacturing a ferroelectric recording medium according to a first exemplary embodiment of the present invention;
[0035] FIGS. 9 and 10 are cross-sectional views illustrating steps in a method of manufacturing a ferroelectric recording medium according to a second exemplary embodiment of the present invention;
[0036] FIG. 11 is a cross-sectional view illustrating access by a probe in a conventional recording medium; and
[0037] FIG. 12 is a cross-sectional view illustrating access by a probe in a recording medium according to an exemplary embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0038] Hereinafter, the present invention will be described more fully with reference to the accompanying drawings, in which exemplary embodiments of the present invention are shown. In the drawings, the sizes and thicknesses of layers and regions are exaggerated for clarity.
[0039] A ferroelectric recording medium according to a first exemplary embodiment of the present invention (hereinafter, referred to as a first recording medium) is explained.
[0040] Referring to FIG. 1 , the first recording medium includes bar type data recording units S 1 in which data is recorded and which is formed on a substrate 40 . The substrate 40 is used as a lower electrode. The substrate 40 is formed of a predetermined metal, for example, platinum (Pt) or iridium (Ir). Each of the data recording units S 1 may include a supporting layer 42 , and first and second recording layers 44 and 46 . The supporting layer 42 supports the first and second recording layers 44 and 46 . Both lateral surfaces of the supporting layer 42 are vertical. The first recording layer 44 covers one side of the supporting layer 42 and the second recording layer 46 covers another side of the supporting layer 42 .
[0041] In FIG. 1 , the first and second recording layers 44 and 46 appear that they are formed on both the lateral surfaces of the supporting layer 42 or that they are adhered to the both lateral surfaces of the supporting layer 42 . However, considering a method of manufacturing the data recording unit S 1 described below, the first and second recording layers 44 and 46 are formed by diffusing a source material into both the lateral surfaces of the supporting layer 42 . Therefore, the first and second recording layers 44 and 46 are disposed in a predetermined depth inward from the lateral surfaces of the supporting layer 42 . The supporting layer 42 is formed of TiO 2 or one or more selected from the group consisting of but not limited to TiO 2 , VO 2 , NbO 2 , ZrO 2 , oxides of iron, TiN, VN, NbN, ZrN, Fe 2 N, SrO, Sr 2 N 3 , Ta 2 O 5 and Ta 2 N.
[0042] Alternatively, the supporting layer 42 may be formed of a pure metal. The pure metal may be one or more metals selected from the group consisting of Ti, V, Nb, Zr, Fe, Sr and Ta. The first and second recording layers 44 and 46 may be ferroelectric layers. For example, each of the first and second recording layers 44 and 46 may be formed of one selected from the group consisting of but not limited to PZT, strontium bismuth tantalate (SBT), strontium bismuth titanate (SBT), lithium titanate (LTO), lithium tantalate (LTO), SBN, PTO, BFO, BTO, and KNO. Like this, the first and second recording layers 44 and 46 are ferroelectric layers.
[0043] The polarization of the first and second recording layers 44 and 46 is initially aligned in a certain direction. The polarization of the first and second recording layers 44 and 46 is maintained in the initially aligned direction until an external predetermined voltage, which can change the polarization, is applied thereto. The polarization in certain areas of the first and second recording layers 44 and 46 , which may be upward or downward, indicates that a bit of data is recorded in the certain area of the first and second recording layers 44 and 46 .
[0044] Accordingly, data recorded on the first and second recording layers 44 and 46 is maintained until a voltage is applied to the first and second recording layers 44 and 46 to change data. A plurality of data recording units S 1 are disposed on the substrate 40 . The data recording units S 1 are disposed parallel to each other and are separated from each other by predetermined intervals.
[0045] Next, a ferroelectric recording medium according to a second exemplary embodiment of the present invention (hereinafter, referred to as a second recording medium) is explained. Referring to FIG. 2 , the second recording medium includes data recording units S 2 , in which data is stored, on a substrate 40 . The data recording unit S 2 is similar to the data recording unit S 1 of the first recording medium of FIG. 1 , but the structures are different.
[0046] Each of the data recording units S 2 may include a supporting layer 48 and a recording layer 50 . The supporting layer 48 may be composed of the same material as the supporting layer 42 of the first recording medium of FIG. 1 and the recording layer 50 may be composed of the same material as the first or second recording layer 44 or 46 of the first recording medium of FIG. 1 . However, the supporting layer 48 has a polygonal structure, for example, a square pillar or a pillar comprising three lateral surfaces, and the recording layer 50 covers four lateral surfaces of the supporting layer 48 . The relationship between the supporting layer 48 and the recording layer 50 may be the same as the relationship between the supporting layer 42 and the first and second recording layers 44 and 46 of the first recording medium of FIG. 1 .
[0047] Since the recording layer 50 covers the four lateral surfaces of the supporting layer 48 of the second recording medium of FIG. 2 , the recording layer 50 can be divided into four portions corresponding to the four lateral surfaces of the supporting layer 48 . Bit data is independently recorded on each lateral surface of the recording layers 50 . Accordingly, the first recording medium of FIG. 1 can record 2-bit data in the data recording unit S 1 , but the second recording medium of FIG. 2 can record 4 -bit data in the data recording unit S 2 . A plurality of the data recording units S 2 are disposed on the substrate 40 of the second recording medium of FIG. 2 , and the data recording units S 2 are separated from each other by equal intervals in the four directions.
[0048] According to the first and second recording media illustrated in FIGS. 1 and 2 , a ferroelectric recording medium of an exemplary embodiment of the present invention may be modified in various ways. For example, the supporting layer in the ferroelectric recording medium according to an exemplary embodiment of the present invention may be a pentagonal, a hexagonal or even a circular pillar instead of the square pillar illustrated in FIG. 2 .
[0049] FIG. 3 is a cross-sectional view of the first recording medium taken along the line 3 - 3 ′ of FIG. 1 or the second recording medium taken along the line 3 - 3 ′ of FIG. 2 . The resultant structure shown in FIG. 3 may be formed by the methods described below.
[0050] First, a method of manufacturing a ferroelectric recording medium according to a first exemplary embodiment of the present invention (hereinafter, referred to as a first manufacturing method) is explained with reference to FIGS. 4 through 8 .
[0051] Referring to FIG. 4 , a supporting layer 42 is formed on a substrate 40 . The substrate 40 is used as a lower electrode. The substrate 40 may be formed of a predetermined metal, for example, platinum (Pt) or iridium (Ir). The supporting layer 42 is used to support recording layers. The supporting layer 42 may be formed by depositing TiO 2 on the substrate 40 . Alternatively, the supporting layer 42 may be formed of one or more selected from the group consisting but not limited to TiO 2 , VO 2 , NbO 2 , ZrO 2 , oxides of iron, TiN, VN, NbN, ZrN, Fe 2 N, SrO, Sr 2 N 3 , Ta 2 O 5 and Ta 2 N. The supporting layer 42 may also be formed of one or more selected from the group consisting of Ti, V, Nb, Zr, Fe, Sr and Ta.
[0052] The supporting layer 42 may be formed on the substrate 40 . After forming the supporting layer 42 , a mask P 1 defining a predetermined region of the supporting layer 42 is formed on the supporting layer 42 . The mask P 1 may be a photosensitive layer pattern.
[0053] Referring to FIG. 5 , the supporting layer 42 is etched until the upper surface of the substrate 40 is exposed. Through the etching process, the portion of the supporting layer 42 not disposed under the mask P 1 is removed.
[0054] Next, referring to FIG. 6 , a source material layer 60 is formed to cover exposed surfaces of the supporting layer 42 on the substrate 40 . The source material layer 60 can react with the supporting layer 42 during an annealing process to form a ferroelectric layer. For example, when the supporting layer 42 is a TiO 2 layer, the source material layer 60 may be a lead oxide layer. The source material layer 60 may cover the whole surface of the mask P 1 .
[0055] After forming the source material layer 60 , the mask P 1 is removed. The portion of the source material layer 60 formed on the surface of the mask P 1 is removed together with the mask P 1 in this process. Thus, as shown in FIG. 7 , the source material layer 60 is left on the top surface of the substrate 40 and the lateral surfaces of the supporting layer 42 , and the top surface of the supporting layer 42 is exposed. After the mask P 1 is removed, heat treatment for the resultant structure from which the mask P 1 is removed is performed at predetermined temperature ranges. For example, when a rapid thermal annealing (RTA) process is performed, the temperature range may be 400 to 1400° C. or, in an exemplary embodiment, 500° C. or more.
[0056] During the annealing process, the source material layer 60 formed on the substrate 40 is removed through evaporation, and the source material layer 60 formed on the lateral surfaces of the supporting layer 42 diffuses into and reacts with the supporting layer 42 . Therefore, first and second recording layers 44 and 46 are formed on the lateral surfaces of the supporting layer 42 , as illustrated in FIG. 8 . For example, each of the first and second recording layers 44 and 46 may be formed of one selected from the group consisting of but not limited to PZT, strontium bismuth tantalate (SBT), strontium bismuth titanate (SBT), lithium titanate (LTO), lithium tantalate (LTO), SBN, PTO, BFO, BTO, and KNO.
[0057] Bit data is recorded in the first and second recording layers 44 and 46 . The diffusion rate of the source material layer 60 is controlled by controlling heat treatment conditions such as heat treatment time or heat treatment temperature. Therefore, the widths of the first and second recording layers 44 and 46 are also controlled by controlling the heat treatment conditions. Consequently, the width of a bit data recording region can be controlled by control of the heat treatment conditions and by the thickness of the source material layer.
[0058] Next, a method of manufacturing a ferroelectric recording medium according to a second exemplary embodiment of the present invention (hereinafter, referred to as a second manufacturing method) is explained with reference to FIGS. 9 and 10 .
[0059] Referring to FIG. 9 , the mask P 1 is formed according to the first manufacturing method. After forming the mask P 1 , the product is placed in a gas atmosphere including a source material gas 70 . The source material gas 70 may be a material gas which can react with the supporting layer 42 to form a ferroelectric layer. For example, when the supporting layer 42 is formed of TiO 2 , the source material gas 70 may be PbO gas. While the supporting layer 42 is placed in the source material gas 70 , the lateral surfaces of the supporting layer 42 contact the source material gas 70 . While the temperature is above a certain value, for example 400 C, reaction of the source material with the supporting material occurs and diffusion into the supporting material takes place.
[0060] Referring to the mentioned example, if the source material gas is PbO and the supporting material is TiO 2 , lead titanium oxide (PbTiO 3 ) may be formed in that way. The heating may be obtained in the same way as the above-described heat treatment in the first manufacturing method. During the heat treatment, the source material gas 70 contacting the lateral surfaces of the supporting layer 42 , diffuses into and reacts with the supporting layer 42 as shown on the right of FIG. 9 . Consequently, a ferroelectric layer 95 is formed inward from the lateral surfaces of the supporting layer 42 . In this exemplary embodiment, the mask P 1 should be resistant to the temperature used in this manufacturing process.
[0061] Referring to FIG. 10 , the first and second recording layers 44 and 46 formed of the ferroelectric material are thus formed on the lateral surfaces of the supporting layers 42 through the heat treatment. The mask P 1 is removed after the heat treatment.
[0062] The difference in operating speeds of a conventional recording medium and a recording medium according to an exemplary embodiment of the present invention will now be described. FIG. 11 is a cross-sectional view illustrating access by a probe in a conventional recording medium. FIG. 12 is a cross-sectional view illustrating access by a probe in a recording medium according to an exemplary embodiment of the present invention.
[0063] In the case of a conventional recording medium as illustrated in FIG. 11 , a case when a probe 90 accesses first and second recording layers 80 and 82 will be considered. The probe 90 searches for and accesses the first recording layer 80 , and then a predetermined operation is performed. Subsequently, the probe 90 searches for the second recording layer 82 in order to access the second recording layer 82 . That is, the probe 90 should search for each recording layer one by one in order to access it. However, in the case of a recording medium according to an exemplary embodiment of the present invention, at least the two recording layers 44 and 46 are disposed on opposite surfaces of the supporting layer 42 .
[0064] Accordingly, when the probe 90 accesses the recording layer 44 of the two recording layers 44 and 46 , the probe 90 can access the recording layer 46 by only moving across the upper surface of the supporting layer 42 . That is, it is unnecessary to search for the subsequent recording layer when the probe 90 has already accessed one of two adjacent recording layers which are opposite to each other and where the supporting layer 42 exists between the two recording layers 44 and 46 . Therefore, the ferroelectric recording medium according to an exemplary embodiment of the present invention can read and record data faster than the conventional recording medium.
[0065] When a portion of the source material layer 60 remains on the lateral surfaces of the supporting layer 42 after the heat treatment process in the first method, the residual portion of the source material layer 60 may be removed. The heat treatment may be performed using various heat treatment apparatuses. In addition, the data recording layer may be formed of other ferroelectric materials which are not described above.
[0066] As described above, the ferroelectric recording unit according to the exemplary embodiments of the present invention includes a supporting layer and at least two data recording layers formed on the lateral surfaces of the supporting layer. Bit data is independently recorded in the data recording layers. The data recording density of ferroelectric recording medium according to the present invention is increased by a factor corresponding to the number of lateral recording layers.
[0067] In addition, since two data recording layers are formed on opposite sides of a supporting layer in the ferroelectric recording medium according to the exemplary embodiments of the present invention, when a probe accesses a selected one of the two data recording layers, searching for the other data recording layer is not necessary because the location of the other data recording layer is exactly defined from the selected one. That is, in the recording medium of the present invention, the probe can access two data recording layers by searching for only one of the data recording layers. Therefore, the ferroelectric recording medium according to the exemplary embodiments of the present invention has a high operating speed for recording and reading data.
[0068] While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined by the following claims.
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Provided are a ferroelectric recording medium and a method of manufacturing the same. The ferroelectric recording medium includes a substrate, a plurality of supporting layers which are formed on the substrate, each of the supporting layers having at least two lateral surfaces; and data recording layers formed on the lateral surfaces of the supporting layers. First and second data recording layers may be respectively disposed on two facing lateral surfaces of each of the supporting layers. The supporting layers may be polygonal pillars having at least three lateral surfaces. A plurality of the supporting layers can be disposed at uniform intervals in a two-dimensional array.
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BACKGROUND OF THE INVENTION
The present invention relates to a digital computer and more particularly to a microprogrammable digital processor, memory, logic and control and addressing structure which may be implemented in TTL logic or as an LSI (large scale integration) chip. Moreover, this invention particularly relates to a processor apparatus and method for the microinstruction memory addressing of expanded memory space connected, externally, to the processor. The subject invention, furthermore, is designed for a particular type of microprogrammable units as embodied in the teachings of Faber in patent application U.S. Ser. No. 307,863, now U.S. Pat. No. 3,878,514, filed Nov. 20, 1972 and assigned to the assignee of the present application. The programmable unit disclosed therein is a self-contained serial-bit-by-byte processor employing a soft machine architecture through microprogramming. An instruction set, at the microprogram level, is provided for controlling the specific circuitry of the processor in executing basic computer operations. Essentially, the specific circuitry represents minimally committed logic or hardware which becomes committed to a specific task by control signals originating in the instruction set. Logic, control and addressing functions are performed by circuitry which includes only those gates, registers, drivers, and related logic, which are necessary to implement the basic operations.
Such a processing unit may be comprised of five functional parts: (1) a logic unit which performs shifting, arithmetic and logic functions; (2) a microprogram memory which stores both literals and control words; (3) a memory control unit which provides the registers mircoprogram memory addressing; (4) a control unit which provides timing and conditional control, successor determination and instruction decoding; and (5) an external interface.
In the microprocessor, cited above, a microprogram memory (MPM) is addressed by a memory program count register (MPCR). Feeding this (MPCR) register is an alternate memory program count register (AMPCR). The AMPCR receives instructions from the microprogram memory as well as from other registers within the processor.
Microprocessors of the Faber type are being used in larger and more complicated processing tasks than for which they were originally designed. While this processor's logic units and control units are sophisticated enough to handle the enlarged processing tasks, the micromemory capacity as designed into the basic apparatus is not large enough. This disadvantage exists in most microprocessors in the class of Faber-size processors. The compactness of the basic processor as implemented in a single MOS chip or in a single TTL-printed circuit card unit did not, with yesterday's technology, permit extensive micromemory capacity.
It is, therefore, desirable to be able to increase micromemory capacity. One approach is to connect external memory modules to the basic processor, accessing external memory locations from within the processor, and calling in instructions and data words from the external locations as needed. However, when the basic processor is one wherein component-resources, such as buffer capacities, and address register capacities, are already fully utilized, the implementation of increased micromemory capacity via externally coupled memories is not easily accomplished.
An objective of this invention therefore is to provide an apparatus for accessing external micromemory capacity from within a microprocessor.
Another objective of this invention is to provide an apparatus for accessing microinstruction memory locations external to a microprocessor without the alteration of the hardware design of the basic microprocessor.
A further objective of this invention is to provide simplified firmware for driving the external micromemory apparatus with the base processor, operating within pre-existing format specification.
SUMMARY OF THE INVENTION
The objectives of this invention are realized by an expanded-memory paging apparatus and method for a bit-serial programmable microprocessor wherein a number of processor-external microprogram memories may be addressed from within the microprocessor for conducting normal microprogram operations. Available memory locations may be addressed consistent with memory addresses instruction addresses as defined within the microprocessor operation periods.
A plurality of identical micromemory modules may be connected to the base microprocessor via the paging apparatus for expanding in predetermined increments the memory space available to the microprocessor.
Included in the paging apparatus may be a decoding apparatus for reading memory access instructions for selecting the proper memory module to be accessed. Temporary storage registers may be associated with this decoding apparatus as well as with interlocking and timing circuitry for temporarily holding memory module or page designations for sequencing paging operations to base processor operation periods.
All information is received from and sent to the base processor in serial form. Information transfer within the paging apparatus may be in parallel.
Firmware microinstructions may be resident within the system to control the operation of the paging apparatus.
DESCRIPTION OF THE DRAWINGS
The features of this invention will become more fully apparent from the following detailed description, attached claims and accompanying drawings in which like characters refer to like parts and in which:
FIG. 1 is a detailed block diagram of the base processor.
FIG. 2 is a general block diagram of the paging apparatus.
FIG. 3 is a more detailed diagram of the paging apparatus.
FIG. 4 is a logic flow chart of the microinstructions used to initiate operations within the paging apparatus.
FIG. 5 is a timing diagram for the operation of the paging apparatus.
DETAILED DESCRIPTION
The invention is an apparatus which may be added to a microprogrammable processing system to enhance processing capabilities by making more microinstruction memory capacity available to the base processor without disrupting or altering the internal base processor structure. The apparatus is designed to be compatible with, but is not exclusively limited to, a serial-bit microprocessor described as follows.
The base microprocessor 10 includes a logic unit 11 (FIG. 1). The logic unit 11 is comprised of three 8-bit recirculating shift registers 13, 15, and 17 connected in parallel and denominated registers A1, A2 and A3, respectively, an 8-bit recirculating shift register 19, denominated the B register, and a serial adder 21. The recirculating capability of registers 13, 15, 17 and 19 enables information to be transferred into the adder 21 without changing the contents of the respective input register. Further functions of the processor as illustrated in this FIG. 1 will be brought out in the discussion below.
A registers 13, 15 and 17 are functionally identical and may be used to temporarily store data within the logic unit 11. A selection gate network 23 permits the contents of any of A registers 13, 15 or 17 to be loaded as one input, denominated the X input 25 of adder 21.
B register 19 is the primary interface into the processor. Data from external sources is entered via data interface 27 and DATA-IN bus 29. The B register 19 also serves as a second, or Y input 31 via a selection network 33 to the adder 21, and collects certain side effects of arithmetic operations. A selection network 35 selects the input to B register 19 from DATA-IN, external interface 27, the output of adder 21 via a selection network 37 or a recirculating feedback loop of the "true" contents of the B register 19 from its "true" output. Selection network 37 also permits the output of adder 21 to be fed to A registers 13, 15, 17. In addition, literal values which are decoded from certain microinstructions stored in an optional microprogram memory 39 are fed directly to the B register 19 via microinstruction decoder 41. As implied above, B register 19 has a true-false output which may be selected to be fed as the Y input 31 of adder 21 by the selection network 33. The purpose is to provide adder 21 with either the true value or the one's complement of the value in B register 19. Adder 21 is a conventional type serial adder as known in the art. The output of adder 21 besides being tied to components within the processor is connected via information-data out bus 30 to interface 27 for communication to devices external to the processor.
Microprogram memory (MPM) 39, is a 256 word, 12 bit, read-only memory which may optionally be included in the processor hardware configuration or which may be located externally to the processor and accessed via external interface 27. In this latter case an external memory capacity can be expanded via memory access circuitry.
A memory control unit comprises two 8-bit registers, i.e., a microprogram count register 43 (MPCR) and an alternate microprogram count register 45 (AMPCR). MPCR 43 is an 8-bit counter which can be incremented by one or two and is used to address MPM 39 (select each instruction from microprogram memory 39) or any external memories connected via bus 47 and interface 27. MPCR 43 may be expanded to 12 or 16 bits by the substitution of a 12 or 16 bit counter for the 8-bit counter.
AMPCR 45 can hold an alternate address which is needed for microprogram manipulation. When not required for this purpose, AMPCR 45 can be used by the logic unit 11 as a scratch pad register. The contents of AMPCR 45 can be fed to adder 21 as its Y input 31 via selection network or can be clocked directly into MPCR 43. AMPCR 45 can be loaded by the output from adder 21 via selection logic 37, or from MPCR 43 or from microprogram memory 39 (MPM) or from an instruction register 49 which is tied to the output of microprogram memory 39 or to external memories via bus 51. When more than 8 bits are to be transferred into AMPCR 47 they may be concatenated with the use of instruction register 49.
The microprogrammable processor 10 requires a source of microprogram instructions to define the operation of the processing unit 11. This source is provided by microprogram memory 39 or external microprogram memory which can either be a Read/Write or a Read Only memory. Memory 39 is a read-only memory (ROM) that contains the program defining the processing unit's function when the ROM enable line is true. ROM enable line select enables the instruction source to be from the internal memory 39 in the presence of a true bit, and from the external source in the presence of a false bit. In any event, the program stored in either the internal memory 39 or an external memory characterizes the processor unit to perform specific tasks in an optimum manner.
Presently, for purposes of discussion only, a ROM memory 39 will be considered. In the preferred embodiment, microprogram memory 39 is comprised of 256 words, each 12 bits in length. The memory 39, contains only executable instructions and cannot be changed under program control. Each microinstruction which comprises the microprogram stored in microprogram memory 39 is 12-bits in length and is decoded by the decoder 41. The 12-bits of each instruction are decoded into one of four types, namely (1) literal, (2) condition, (3) logic and (4) external. A more thorough discussion of these four instruction types will be described in detail later.
The processor control unit includes a microinstruction decoder 41, successor (or next instruction) determination logic 53, condition selection logic 55, and a condition register 57. The successor determination logic 53, the condition selection logic 55 and the condition register 57 are activated by the output of the microinstruction decoder 41. In addition, the adder 21 feeds four condition bits to the condition register 57, namely, the least significant bit true (LST) condition 59, the most significant bit true (MST) condition 61, the adder overflow bit (AOV) 63, and an all bits true indicator bit (ABT) 65 (if all bits of the adder output are true 1's). The successor determination logic 53 determines whether to use the contents of the MPCR, register 43, incremented by 1 or by 2, or to use the contents of AMPCR, register 45 for addressing the next instruction stored in microprogram memory 39 or external memories. Additionally, condition register 57 feeds 8 bits to condition select logic 55 which in turn selects one bit for transfer to successor select logic 53.
The condition register 57 stores three resettable local condition bits (LC1 bit 67, LC2 bit 69 and LC3 bit 71, respectively), and selects one of 8 condition bits (the 4 adder condition bits, MST bit 61, LST bit 59, AOV bit 63 and ABT bit 65; an external condition bit EXT 73; and the three local condition bits LC1, LC2 and LC3 stored in condition register 57).
External interface 27 connects the programmable unit with external elements related to a multiprocessing system. This connection is synchronized by one internally generated clock signal train available to aid in performing 8-bit serial transfers into and out of the programmable unit. The external asynchronous input EXT 73 to condition register 57 is available for signalling from the external environment in the form of the EXT condition bit, while the four external control lines 75, from decoder 41 are utilized to control the use of external registers.
The timing Generator 77, includes a hexadecimal counter and is interconnected to all components. In addition to generating basic clock pulses, it generates control pulses for information transfers within the system.
As stated above, memory 39 may or may not be included as part of the base processor. In the case where memory 39 is present in the base processor an address from MPCR 43 to micromemory 39 will contain an access bit enabling that particular instruction from MPCR 43 to operate upon the memory 39. All other addresses, i.e., addresses to external memory locations, are shunted via processor bus 47 and processor interface 27 to external memory locations.
In the case where micromemory 39 is not present in the base processor all instructions from MPCR 43 are directed via bus 47 and interface 27 to external memory locations.
Instruction register 49 accepts information either directly from micromemory 39, if present in the system, or from external memories via interface 27 and processor bus 51.
Operational component blocks included in the expanded memory paging apparatus are shown in FIG. 2. Connected to the processor's B register 19 via adder 21, data-out bus 30 and interface 27 is a serial to parallel buffer 79. An output from buffer 79 is connected to a page-designation interlock circuit 81. In addition, a decoder 83 is fed by interlock circuit 81. The output from decoder 83 comprises a plurality of enable lines, with one enable line being connected to the read-enable terminal of each of a plurality of microinstruction memories 85.
The outputs (from the output register) of the memories 85 are ganged together and connected via an information bus 87, processor interface 27 and processor bus 51 to the instruction register 49. The micromemories 85 are addressed via a common bus 89, by MPCR 43 via processor address line 47 and processor interface 27.
Micromemories 85 are read only memory ROM chips of the type, Texas Instrument (T.I.) number 74187. These chips have tri-state outputs and gated address inputs which eliminates the need for AND gates on the bus 89 input and OR gate on the bus 87 output. If it is desirable that each of the memories 85 be of 256 word capacity, three T.I. 74187 may be ganged together to form the 256 word capacity.
The paging apparatus of FIG. 2 must operate compatibly with the activity cycles of the base processor. The microprocessor (FIG. 1) has fixed operational cycles wherein external control 75 signals are available from the instruction decoder 41, as outputs via interface 27. These signals, as shown in FIG. 1, include BEX, OUT, DEV and are defined by two signal lines, N9 and N10, from the instruction register 49 via decoder 41; and two signal lines A and B generated from the decoder 41.
BEX is an instruction to an external device indicating that the processor is ready to receive data into B register 19 via data-in bus 29.
OUT is an instruction to an external device indicating that the processor is sending, via data-out bus 30, an instruction to an external register.
DEV is an instruction to an external device indicating that the processor is sending, via data-out bus 30, a "literal" to an external register. A "literal" is a non-instruction or operator word as defined in the above-cited Faber processor specification.
Also available from the processor (FIG. 1) timing generator 77, as an output from interface 27, is a pulse train CP out. CP is a repetitive pulse series of 8 pulses followed by two blank spaces. An input to timing generator 77 is clock pulse input (CP in). This pulse stream is transmitted via interface 27 from pulse generator or clock 80. CP in and CP out are in synchronism.
Other timing pulses available from the timing generator 77 are a preset strobe and a last strobe. The present strobe establishes the start of the operation period of the processor during which one operation or operation step is conducted. The last pulse defines the end of the operation period of the processor. The number of clock pulses which comprise an operation period may be varied, but most commonly the operation period is 8 clock pulses long, including the preset strobe and the last pulse. While the processor may be run at various speeds as determined by the basic timing generator, for present purposes the speed will be denoted as one megahertz. Under this condition an 8 clock pulse period is 8μ seconds long.
The buffer 79, the page designation and interlock circuit 81, the decoder 83 and the microprogram memories 85 are shown in greater detail in FIG. 3. For ease of discussion below, repeated references to interface 27 will be eliminated. Signals which are received from or sent to the microprocessor 10 will be discussed in reference to their component and/or bus designation within the microprocessor 10. However, it is to be understood that all signals enter and leave the microprocessor 10 via the interface 27.
Referring now to FIG. 3, control decoder 87 receives bits N9 and N10 and bits A and B from instruction decoder 41 (FIG. 1). Connected in parallel to the output of control decoder 87 is an OR-gate tree circuit 89.
The serial to parallel register 79 receives serial information from the data-out bus 30 on its A terminal, while the B terminal of this register 79 is connected to the output of gate circuit 88. Clock pulses to the clock input of register 79 are provided via AND gate 93 and NAND gate 95.
This pulse circuit also includes a two-input AND gate 91 which receives clock out pulses from timing generator 77, simultaneously on both of its inputs. The output of gate 91 is connected to an input of a two-input, AND gate 93. The other input of the AND gate 93 is tied to the output of the gate circuit 89. The output of the AND gate 93 is connected to the inputs of a NAND gate 95, while the output of NAND gate 95 drives the clock input to the register 79.
The serial to parallel register 79 stores data received serially on its A terminal when enabled on its B terminal, and clocks this stored data through as an 8-bit parallel output.
A buffer or page select register 97 has its 8-bit parallel input terminals connected to the 8-bit parallel outputs of register 79. The respective terminals are connected so that the most significant bit is entered on the A input terminal of register 97, the least significant bit on the H terminal of the register 97, with the other bits on respective terminals therebetween. The J, K and S/L terminals of register 97 are grounded.
An output from a dual J-K flip-flop interlocking circuit 99,101 drives the C/I terminal of the register 97.
This dual flip-flop circuit includes a first J-K flip-flop 99 with its J input connected to the output of And gate 93, and its clock input connected to the output of AND gate 91. The Q or complementary output of flip-flop 99 is connected to the C/I terminal of register 97.
A second J-K flip-flop 101 has its J-input connected to the Q-output of flip-flop 99. The clock and K inputs of flip-flop 101 are tied to the output of the memory cycle complete circuit which will be discussed below, while the Q output of flip-flop 101 connects to the K input of flip-flop 99.
The memory cycle complete circuit includes a pair of interconnected J-K flip-flops 103 and 105. Flip-flops 103 and 105 are each clocked from the system's basic "clock-in" signal via a two-input AND gate 107, which is used as a driver wherein its inputs are tied together. Moreover, flip-flops 103 and 105 are further inter-connected with the Q output of flip-flop 103 tied to the J-input of flip-flop 105. In addition, the K inputs of the flip-flops 103 and 105 are each grounded. A last pulse signal from timing generator 77 of processor 10 is fed to the clear terminals of the flip-flops 103 and 105 and to the J input to flip-flop 103 simultaneously, via an inverter 109. The Q output of flip-flop 105 is AND'ed through two-input AND gate 111 by the clock input signal from microprocessor 10 to yield the gate 111 output or memory cycle complete signal which, as described above, is fed to AND gate 91 and to flip-flop 101.
A decoder 113 obtains instructions from the page select register 97 and decodes these instructions to enable a reading of one of the microprogram memory pages 85. Connected to the four least-significant-bit output terminals (QE, QF, QG, QH) of the register 97 are the four least-significant-bit input terminals (D, C B, A) of the decoder 113, with QE tied to E, QF to C, QG to B, and QH to A respectively, between register 97 and decoder 113. Decoder 113 has its G1 and G2 inputs grounded and its clock input connected to the output of gate 111, the memory cycle complete signal. The output of the decoder 113 comprises a plurality of pins whereupon an enable, "high-signal", appears on only one pin at a time. In the present embodiment, decoder 113 has its "0" output pin connected to the enable gate of the first of 4 identical memory pages 85, its "1" output connected to the enable of the second memory 85, its "2" output connected to the enable of the third memory 85 and its "3" output connected to the enable of the fourth memory 85.
A clear pulse is connected to the clear or reset terminals of registers 79 and 97 and flip-flops 99 and 101. This clear pulse may be a function of the last pulse or the memory cycle complete signal. The circuit is easily reset by the memory cycle complete signal. When this is the case, for the circuit as shown by FIG. 3, the clear line is connected to the output of AND gate 111.
An address word bus 115 from the microprogram count register 43 which carries the address for a location within a page is connected to the address inputs of each of the memories 85. An output instruction bus 117 commonly connects all of the memories 85 outputs to processor 10 instruction bus 51. The choice of the memory module 85 with an enable controlled address input and tri-state type output eliminates the need for buffer gating, and permits input and output wires to each memory 85 to be ganged directly to the buses 115 and 117, respectively.
In the present embodiment, the specific manufacturers components utilized for the page select register 97 and the decoder 113, (further specified below), each have additional unused terminals. These terminals are to be utilized when the number of memories 85 (pages) are increased. While the hardware requirements for the instant circuit may be further optimized with the employment of a register 97 and a decoder 113 of the size needed to address exactly four memory pages, it may be desirable and in fact, more practical to be able to address additional pages without significantly changing the hard-wired circuitry. With this in mind, the instant circuit is designed with a register 97 and decoder 113 of a size to be able to address up to 16 microprogram memories 85.
A memory group select circuit may be utilized when the memory 85 pages in the system number more than four. This select can be driven by the quadralincremental bits of the page instruction which designate when a page amongst a grouping of four is being addressed. Given 8 memory 85 pages in a system, a select group 1 and select group 2 could be used. These respective select group signals would enable groups of four memories and would act as an error check on the addressing components.
A two-group select as shown in FIG. 3 includes a pair of two-input NAND gates 119, 121. The inputs of gate 119 are connected to the most significant bit of the four bit instruction fed into the decoder 113. The output of gate 119 is the "select group 1" enable signal which is available for the first group of memory 85 pages. The output of NAND gate 119 is also tied to the inputs of NAND gate 121. Similarly, to gate 119, the output of gate 121 is the "select group 2" enable signal which is available for the second group of memory 85 pages.
A partial listing of some of the components which may typically be used in the circuit includes:
ITEM REFERENCE MANUFACTURER CHARACTER IDENTIFICATION______________________________________AND gate 91, 93, 107, Texas Instrument 109, 111 No. 7408NAND gate 95, 119, 121 Texas Instrument No. 7438J-K Flip-Flop 99, 101, 103, Texas Instrument 105 No. 7473Memory 85 Texas Instrument No. 74187Serial to Parallel 79 Texas InstrumentRegister No. 74164Buffer Register 97 Texas Instrument No. 74199Decoder 113 Texas Instrument No. 74154______________________________________
A microinstruction routine as illustrated in FIG. 4 may be used to initiate operation of the paging apparatus. This routine is to be resident in the memory 85 (herein called a page) currently addressed by processor 10.
FIG. 4 shows the flow chart for a sequence of microinstructions, for calling a new page, and for addressing memory locations on that page. FIG. 4 also shows a table of the steps performed wherein the microinstructions specify the calling of a new page. For example, for addressing location 20 of Page 1 from the existing operating memory. The memory in current use is Page 2.
The first microinstruction, LIT=DEV, is the output command which selects a device number. It is an instruction which initiates the connection of a specific input-output device to the processor 10 interface 27. This is an operation by components pre-existing in the basic system.
The second microinstruction LIT=B, defines the B register 19 value to be read. This second microinstruction, LIT=B, defines the B register 19 value to be read as the literal (LIT). This instruction loads the new page number of the next page to be addressed.
The third microinstruction, B=OUT 1, shifts the new page. This means that the B register 19 value is defined equal to the new page number, thus causing the processor 10 in its normal operation to jump to the new page.
The fourth instruction, GO TO LIT, initiates the addressing of the new address in the new page.
Presented in FIG. 4 along with the flow chart of microinstructions is a tabloid presentation of the paging sequence in going from a presently addressed page (2) to a new page (1) and specific location on the page (1), location 20. The microinstructions which control the paging operations are located in locations 10-13 of memory page 2.
Microprogram memory count register MPCR 43 sequentially steps through instructions 10, 11, 12 and 13 of page 2 enabling the circuitry to sequentially perform the following operations: load device = 9, load page = 1, shift out page = 1, load MPCR = 20, and jump to page 1.
A timing diagram of microprogram memory page control for the example as discussed above in connection with FIG. 4 is shown in FIG. 5.
Line 1, FIG. 5, shows the clock-in pulses received by the paging circuitry, FIG. 3, and the processor 10, FIG. 1. This pulse train is the basic clock for the entire system.
Clock-out timing pulses as generated by the timing generator 77 and received by the paging circuitry are shown in line 2, FIG. 5.
Line 2, FIG. 5, shows the memory complete pulses generated by the interconnected flip-flops 103, 105 and their associated gating as discussed above. These pulses are generated on a count of two after the last pulse.
Microprogram memory count register 43 address operations are shown in line 4, FIG. 5. Each operation is labelled for the fetch (read) of an instruction from locations 10, 11, 12, 13 of page 2 and 20 of page 1, sequentially, as presented in the example above in connection with the discussion of FIG. 4.
Line 5, FIG. 5, shows the operation periods for performing each of the steps of paging. Each operation cycle is labelled to reflect the sequential steps discussed in the example above and as shown in FIG. 4. In the first period, Device = 9, the I/O device to processor 10 is selected. In the second period, B = 1, the new page designation is entered into B register 19. In the third operation period, B = OUT 1, the paging control instruction is decoded, the page designation data is loaded into register 79, clocked through register 97 as input to decoder 113. During the fourth operation period, JUMP to PAGE 1 and GO TO 20, decoder 113 is clocked to enable reading of the new page while the new instruction location is addressed on this new page.
Last pulses as received from the timing generator 77 are shown in line 6, FIG. 5.
Line 7 is the control decode enable to register 79.
The new page designation word clock through register 79 is shown in line 8.
Line 9 represents the clocking of register 97 and the data transmission out of this register of the new page designate.
Line 10 shows the clocking of decoder 113 which decodes the page designate to enable the read terminal of one of the memories 85.
The MPCR 43 operation which fetches the next (new) instruction 20 from the next (new) page is redrawn from line 4 to line 11.
What has been shown and described in the foregoing is a method and means of expanding the memory capacity of a serial bit, programmable microinstruction processor. While many different embodiments of the above-described invention could be made without departing from the scope thereof, it is intended that the above-description not be taken in the limiting sense, but be interpreted as illustrative of a best mode for a particular application as developed by the inventor.
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For a serial-bit, programmable microinstruction processor having serial-byte internal transfers, an expanded-memory addressing apparatus and method is provided by the incorporation into the processor system a plurality of external memory units and a selection and transfer circuitry for accessing external memory space from within the processor. The accessing of external memory locations may be controlled by programmed memory access command instructions. These instructions may be operated upon by decoding components and buffer storage components to make available, concurrently, the entire contents of a particular one of the external memory units. Once a particular memory, or page is selected, a location within that page may then be addressed by memory address registers within the base processor.
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FIELD OF THE INVENTION
This invention relates to a method for transferring a protective overcoat for a thermal print wherein the protective overcoat is applied to a dye-donor element under predesigned conditions after thermal dye transfer, the dye-donor element comprising patches of dyes for transfer to a thermal print to provide a protective layer thereon. In particular, the invention improves the process of providing an improved level of gloss to the transferred protective overcoat.
BACKGROUND OF THE INVENTION
In recent years, thermal transfer systems have been developed to obtain prints from pictures that have been generated electronically from a color camera. According to one way of obtaining such prints, an electronic picture is first subjected to color separation by color filters. The respective color-separated images are then converted into electrical signals. These signals are then operated on to produce cyan, magenta and yellow signals. These signals are then transmitted to a thermal printer. To obtain the print, a cyan, magenta or yellow dye-donor element is placed face-to-face with a dye-receiving element. The two are then inserted between a thermal printing head and a platen roller. A line-type thermal printing head is used to apply heat from the back of the dye-donor sheet. The thermal printing head has many heating elements and is heated up sequentially in response to one of the cyan, magenta and yellow signals. The process is then repeated for the other two colors. A color hard copy is thus obtained which corresponds to the original picture viewed on a screen. Further details of this process and an apparatus for carrying it out are contained in U.S. Pat. No. 4,621,271, the disclosure of which is hereby incorporated by reference.
Thermal prints are susceptible to retransfer of dyes to adjacent surfaces and to discoloration by fingerprints. This is due to dye being at the surface of the dye-receiving layer of the print. These dyes can be driven further into the dye-receiving layer by thermally fusing the print with either hot rollers or a thermal head. This will help to reduce dye retransfer and fingerprint susceptibility, but does not eliminate these problems. However, the application of a protection overcoat will practically eliminate these problems. This protection overcoat is applied to the receiver element by heating in a likewise manner after the dyes have been transferred. The protection overcoat will improve the stability of the image to light fade and oil from fingerprints.
In a thermal dye transfer printing process, it is desirable for the finished prints to compare favorably with color photographic prints in terms of image quality. The look of the final print is very dependent on the surface texture and gloss. Typically, color photographic prints are available in surface finishes ranging from very smooth, high gloss to rough, low gloss matte.
The transferable protection layer of the dye donor that has a glossy finish is manufactured by a gravure coating process between the temperatures of 55° F. and 120° F., preferably between 65° F. and 100° F. A coating melt or solution is prepared from a solvent soluble polymer, a colloidal silica and organic particles and is transferred in the liquid state from the etching of the gravure cylinder to the dye donor support. The coated layer is dried by evaporating the solvent.
The transferable protection layer is usually one of at least two patches on the dye donor. It is transferred after printing an image from the dye donor to the surface of the dye receiving layer of the receiver by heating the backside of the donor causing the transferable protection layer to adhere to the dye receiving layer. The dye donor is peeled away from the receiver after cooling resulting in transfer of the protective layer. The surface of the transferred protective layer adhered to the dye-receiving layer has a measurable 60 degree gloss that is usually between 65 and 85 gloss units.
It has been found that the gloss on a laminated print decreases as the printing line time decreases, which is a problem as printing times become faster.
SUMMARY OF THE INVENTION
A solution to this problem is achieved in accordance with this invention that relates to a process for transferring a protection layer or overcoat material from a dye-donor element to a printed receiver after thermal dye transfer to the receiver. In one embodiment, the dye-donor element comprises a support having thereon at least one dye layer area comprising an image dye in a binder and another area comprising a transferable protection layer, the transferable protection layer area being approximately equal in size to the dye layer area. In one embodiment, the transferable protection layer contains inorganic particles, a polymeric binder, and organic particles.
By use of the present process, a dye-donor element is provided containing a transferable protection layer that is capable of giving a higher gloss to an image after transfer.
In particular, predesigned adjustment of the time between applying the protection layer to a thermal print and then peeling them apart has been found to provide increased gloss to the print. A means for stripping the portion of protection overcoat (adhered to the thermally printed receiver by the thermal-print head) from the rest of the dye-donor element provides improved results especially at faster print times. The time of peeling can be adjusted by the relative position of the means for stripping, such as a stripper plate, relative to the print head or other parts of the thermal printer.
Increased gloss of a glossy print is an advantage in the physical quality of the print. This is particularly advantageous at lower line times, faster printing. In one embodiment, the method of the invention employed with respect to a protection overcoat transferred from the fourth patch laminate of a thermal donor results in a higher gloss on the print after the laminate has been transferred to the receiver when compared to the control with current methods.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a side view of one embodiment of a thermal printing head and peeling plate interface that can be used in accordance with the process of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
As indicated above, the present invention relates to a process of forming a protection layer with an improved level of gloss on top of a thermal dye transfer image comprising: (a) imagewise-heating a dye-donor element comprising a support having thereon a dye layer comprising an image dye in a binder, said dye donor being in contact with a dye-receiving element, thereby transferring a dye image to said dye-receiving element at a line time of 0.4 to 2 milliseconds, preferably 0.5 to 1.4 milliseconds, more preferably 0.5 to 1 milliseconds, to form said dye transfer image; and (b) thermally transferring a protection layer on top of said transferred dye image at a line time (not necessarily the same line time as the dye image) of 0.4 to 2 milliseconds, preferably 0.5 to 1.4 milliseconds, more preferably 0.5 to 1 milliseconds, wherein a means for stripping the protection layer from the dye-donor element is adjusted so that the distance the donor and receiver travel before peeling is preselected such that the time from printing of a line to peeling of the line, when the dye donor substrate is separated from the protection layer adhered to said dye-receiving element, is 68.21 to 69.00 millisec, preferably 68.25 to 68.75 millisec. In a preferred embodiment, the angle between donor and receiver from the thermal head to the stripping plate (taking into account the radius of the platen roller) from a true vertical axis is between 0 and 32.14 degrees, preferably 1.19 to 2.39 degrees.
The means for stripping the protection layer from the dye-donor element can be a printer stripper plate or equivalent means. One embodiment of such a printer stripper plate is described below with respect to FIG. 1 .
Preferably, the printing line time is 2 millisecond or less, more preferably 1.5 or less, most preferably, 1.2 millisecond or less per line. The line time can be as low as 0.5 milliseconds. Thus, previous line-times of about 4 milliseconds are relatively slow. Such fast line times allow printing of at least or greater than 300 lines per inch, preferably at least or greater than 600 lines per inch.
In a preferred embodiment of the invention, the dye-donor element is a multicolor element comprising repeating color patches of yellow, magenta and cyan image dyes, respectively, dispersed in a binder, and a patch containing the protection layer. Preferably, the protection layer or overcoat is transferred over an image made from a single thermal head. In one embodiment, the invention is used in a kiosk.
In another embodiment of the invention, the dye-donor element is a monochrome element and comprises repeating units of two areas, the first area comprising a layer of one image dye dispersed in a binder, and the second area comprising the protection layer.
In still another embodiment of the invention, the dye-donor element is a black-and-white element and comprises repeating units of two areas, the first area comprising a layer of a mixture of image dyes dispersed in a binder to produce a neutral color, and the second area comprising the protection layer.
The present invention provides a protection overcoat layer on a thermal print by uniform application of heat using a thermal head. After transfer to the thermal print, the protection layer provides superior protection against image deterioration due to exposure to light, common chemicals, such as grease and oil from fingerprints, and plasticizers from film album pages or sleeves made of poly(vinyl chloride). The protection layer is generally applied at a coverage of at least about 0.03 g/m 2 to about 1.7 g/m 2 to obtain a dried layer of preferably less than 1 μm.
As noted above, the transferable protection layer comprises inorganic and organic particles dispersed in a polymeric binder. Many such polymeric binders have been previously disclosed for use in protection layers. Examples of such binders include those materials disclosed in U.S. Pat. No. 5,332,713, the disclosure of which is hereby incorporated by reference. In a preferred embodiment of the invention, poly(vinyl acetal) is employed.
Preferably, the transferable protection layer area being approximately equal in size to the dye layer area, wherein the transferable protection layer comprises poly(vinyl formal), poly(vinyl benzal) or poly(vinyl acetal) containing at least about 5 mole % hydroxyl.
In a preferred embodiment of the invention, the protection layer comprises:
wherein:
R is H, CH 3 or C 6 H 5 ; A is at least about 25 mole percent; B is from about 5 to about 75 mole percent; Z is another monomer different from A and B such as vinyl acetate, vinyl chloride, styrene, methyl methacrylate, butyl acrylate, isopropyl acrylamide, and acrylate ionomer; A+B is at least about 65 mole percent; and A+B+C=100.
Preferably, the Tg of the surface material on the overcoat in contact with the print is in the range of 100 to 125° C., more preferably below 120° C., most preferably 110 to 120° C. Suitably, the protective overcoat is heated by the thermal head at a temperature of 130 to 150° C. This allows a gloss level of at least 70.
The present invention preferably provides a protective overcoat layer applied to a thermal print by uniform application of heat using a single thermal head.
In use, yellow, magenta and cyan dyes are thermally transferred from a dye-donor element to form an image on the dye-receiving sheet. The thermal head is then used to transfer a clear protective layer, from another clear patch on the dye-donor element or from a separate donor element, onto the imaged receiving sheet by uniform application of heat. The clear protection layer adheres to the print and is released from the donor support in the area where heat is applied.
The clear protective layer adheres to the print and is released from the donor support in the area where heat is applied.
Binder materials for the protective overcoat include, for example, but are not limited to the following:
1) Poly(vinyl benzal) in 2-butanone solvent.
2) Poly(vinyl acetal) KS-5 (Sekisui Co) (26 mole % hydroxyl, 74 mole % acetal) in a 3-pentanone/methanol solvent mixture (75/25).
3) Poly(vinyl acetal) KS-3 (Sekisui Co) (12 mole % hydroxyl, 4 mole % acetate, 84 mole % acetal) in a 3-pentanone/methanol solvent mixture (75/25).
4) Poly(vinyl acetal) KS-1 (Sekisui Co) (24 mole % hydroxyl, 76 mole % acetal) in a 3-pentanone/methanol solvent mixture (75/25).
5) Poly(vinyl acetal) (26 mole % hydroxyl, 74 mole % acetal) in a 3-pentanone/methanol solvent mixture (75/25).
6) Poly(vinyl acetal) (29 mole % hydroxyl, 71 mole % acetal) in a 3-pentanone/methanol solvent mixture (75/25).
7) Poly(vinyl acetal) (56 mole % hydroxyl, 44 mole % acetal) in a 3-pentanone/methanol solvent mixture (75/25).
8) Poly(vinyl acetal) (15 mole % hydroxyl, 77 mole % acetal, 8 mole % acetate) in a methanol/3-pentanone solvent mixture (75/25).
9) Poly(vinyl acetal) (20 mole % hydroxyl 51 mole % acetal, 29 mole % acetate) in a methanol/3-pentanone solvent mixture (75/25).
10) Poly(vinyl acetal) (24 mole % hydroxyl, 76 mole % acetal) in a methanol/3-pentanone solvent mixture (75/25).
11) Poly(vinyl acetal) (44 mole % hydroxyl, 43 mole % acetal, 13 mole % acetate) in a methanol/water solvent mixture (75/25).
12) Poly(vinyl acetal) (65 mole % hydroxyl, 35 mole % acetal) in a methanol/water solvent mixture (75/25).
13) Poly(vinyl acetal) (18 mole % hydroxyl, 64 mole % acetal, 18 mole % acetate) in a methanol/3-pentanone solvent mixture (75/25).
14) Poly(vinyl acetal) (16 mole % hydroxyl, 84 mole % acetal) in a methanol/3-pentanone solvent mixture (75/25).
15) Poly(vinyl formal) (Formvar®, Monsanto Co.) (5% hydroxyl, 82% formal, 13% acetate) in a toluene/3A alcohol/water mixture (57/40/3).
Inorganic particles are present in the protection layer used in the method of the invention. There may be used, for example, silica, titania, alumina, antimony oxide, clays, calcium carbonate, talc, etc. as disclosed in U.S. Pat. No. 5,387,573. In a preferred embodiment of the invention, the inorganic particles are silica. The inorganic particles improve the separation of the laminated part of the protection layer from the unlaminated part upon printing.
In a preferred embodiment of the method, the protection layer contains from about 5% to about 60% by weight inorganic particles, from about 25% to about 80% by weight polymeric binder and from about 5% to about 60% by weight of the organic particles. The protection layer may further comprise a UV absorber or gloss-enhancing agent as described in commonly assigned copending application U.S. Ser. No.07/682,798 hereby incorporated by reference in its entirety.
Any dye can be used in the dye layer of the dye-donor element used in the method of the present invention provided it is transferable to the dye-receiving layer by the action of heat. Especially good results have been obtained with sublimable dyes. Examples of sublimable dyes include anthraquinone dyes, e.g., Sumikaron Violet RS® (Sumitomo Chemical Co., Ltd.), Dianix Fast Violet 3R FS® (Mitsubishi Chemical Industries, Ltd.), and Kayalon Polyol Brilliant Blue N BGM® and KST Black 146® (Nippon Kayaku Co., Ltd.); azo dyes such as Kayalon Polyol Brilliant Blue BM®, Kayalon Polyol Dark Blue 2BM®, and KST Black KR® (Nippon Kayaku Co., Ltd.), Sumikaron Diazo Black 5G® (Sumitomo Chemical Co., Ltd.), and Miktazol Black 5GH® (Mitsui Toatsu Chemicals, Inc.); direct dyes such as Direct Dark Green B® (Mitsubishi Chemical Industries, Ltd.) and Direct Brown M® and Direct Fast Black D® (Nippon Kayaku Co. Ltd.); acid dyes such as Kayanol Milling Cyanine 5® (Nippon Kayaku Co. Ltd.); basic dyes such as Sumiacryl Blue 6G® (Sumitomo Chemical Co., Ltd.), and Aizen Malachite Green® (Hodogaya Chemical Co., Ltd.);
or any of the dyes disclosed in U.S. Pat. No. 4,541,830, the disclosure of which is hereby incorporated by reference. Other dyes are disclosed in U.S. Pat. Nos. 4,698,651; 4,695,287; 4,701,439; 4,757,046; 4,743,582; 4,769,360 and 4,753,922, the disclosures of which are hereby incorporated by reference. The above dyes may be employed singly or in combination to obtain a monochrome. The dyes may be used at a coverage of from about 0.05 to about 1 g/m 2 and are preferably hydrophobic.
A dye-barrier layer may be employed in the dye-donor elements used in the invention to improve the density of the transferred dye. Such dye-barrier layer materials include hydrophilic materials such as those described and claimed in U.S. Pat. No. 4,716,144.
The dye layers and protection layer of the dye-donor element may be coated on the support or printed thereon by a printing technique such as a gravure process.
A slipping layer may be used on the back side of the dye-donor element to prevent the printing head from sticking to the dye-donor element. Such a slipping layer would comprise either a solid or liquid lubricating material or mixtures thereof, with or without a polymeric binder or a surface-active agent. Preferred lubricating materials include oils or semi-crystalline organic solids that melt below 100° C. such as poly(vinyl stearate), beeswax, perfluorinated alkyl ester polyethers, poly-caprolactone, silicone oil, poly(tetrafluoroethylene), carbowax, poly(ethylene glycols), or any of those materials disclosed in U.S. Pat. Nos. 4,717,711; 4,717,712; 4,737,485; and 4,738,950. Suitable polymeric binders for the slipping layer include poly(vinyl alcohol-co-butyral), poly(vinyl alcohol-co-acetal), polystyrene, poly(vinyl acetate), cellulose acetate butyrate, cellulose acetate propionate, cellulose acetate or ethyl cellulose.
The amount of the lubricating material to be used in the slipping layer depends largely on the type of lubricating material, but is generally in the range of about 0.001 to about 2 g/m 2 . If a polymeric binder is employed, the lubricating material is present in the range of 0.05 to 50 weight %, preferably 0.5 to 40 weight %, of the polymeric binder employed.
Any material can be used as the support for the dye-donor element provided it is dimensionally stable and can withstand the heat of the thermal printing heads. Such materials include polyesters such as poly(ethylene terephthalate); polyamides; polycarbonates; glassine paper; condenser paper; cellulose esters such as cellulose acetate; fluorine polymers such as poly(vinylidene fluoride) or poly(tetrafluoroethylene-co-hexafluoropropylene); polyethers such as polyoxymethylene; polyacetals; polyolefins such as polystyrene, polyethylene, polypropylene or methylpentene polymers; and polyimides such as polyimide amides and polyetherimides. The support generally has a thickness of from about 2 to about 30 μm.
The dye-receiving element that is used with the dye-donor element usually comprises a support having thereon a dye image-receiving layer. The support may be a transparent film such as a poly(ether sulfone), a polyimide, a cellulose ester such as cellulose acetate, a poly(vinyl alcohol-co-acetal) or a poly(ethylene terephthalate). The support for the dye-receiving element may also be reflective such as baryta-coated paper, polyethylene-coated paper, white polyester (polyester with white pigment incorporated therein), an ivory paper, a condenser paper or a synthetic paper such as DuPont Tyvek®.
The dye image-receiving layer may comprise, for example, a polycarbonate, a polyurethane, a polyester, poly(vinyl chloride), poly(styrene-co-acrylonitrile), polycaprolactone or mixtures thereof. The dye image-receiving layer may be present in any amount that is effective for the intended purpose. In general, good results have been obtained at a concentration of from about 1 to about 5 g/m 2 .
As noted above, the dye donor elements used in the present process are used to form a dye transfer image. Such a process comprises imagewise heating a dye-donor element as described above and transferring a dye image to a dye receiving element to form the dye transfer image. After the dye image is transferred, the protection layer is then transferred on top of the dye image.
The dye donor element may be used in sheet form or in a continuous roll or ribbon. If a continuous roll or ribbon is employed, it may have only one dye or may have alternating areas of other different dyes, such as sublimable cyan and/or magenta and/or yellow and/or black or other dyes. Thus, one-, two-, three- or four-color elements (or higher numbers also) are included within the scope of the invention.
The dye-donor element may comprise a poly(ethylene terephthalate) support coated with sequential repeating areas of yellow, cyan and magenta dye, and the protection layer noted above, and the above process steps are sequentially performed for each color to obtain a three-color dye transfer image with a protection layer on top. Of course, when the process is only performed for a single color, then a monochrome dye transfer image is obtained.
Thermal printing heads that can be used to transfer dye and a protection overcoat from dye-donor elements are available commercially. There can be employed, for example, a Fujitsu Thermal Head FTP-040 MCSOO1, a TDK Thermal Head LV5416 or a Rohm Thermal Head KE 2008-F3.
A thermal dye transfer assemblage typically comprises
(a) a dye-donor element as described above, and (b) a dye-receiving element as described above, the dye receiving element being in a superposed relationship with the dye donor element so that the dye layer of the donor element is in contact with the dye image-receiving layer of the receiving element.
The above assemblage comprising these two elements may be preassembled as an integral unit when a monochrome image is to be obtained. This may be done by temporarily adhering the two elements together at their margins. After transfer, the dye-receiving element is then peeled apart to reveal the dye transfer image.
When a three-color image is to be obtained, the above assemblage is formed on three occasions during the time when heat is applied by the thermal printing head.
After the first dye is transferred, the elements are peeled apart. A second dye-donor element (or another area of the donor element with a different dye area) is then brought in register with the dye-receiving element and the process is repeated. The third color is obtained in the same manner. Finally, the protection layer is applied on top.
Referring now to FIG. 1 , one embodiment for carrying out the method of the present invention using a thermal print head is illustrated. During the printing operation, the following components are employed: a thermal print head 1 which also has an IC (integrated circuit) cover 2 attached for the protection on the thermal head integrated circuitry, an attached heat sink 3 to dissipate heat from the thermal head, a single compression spring 4 (or multiple compression springs) to apply the correct pressure for transfer of ink or dye, a method for causing the spring or springs to be compressed which creates the pressure, in this case a driven compression plate 5 , a method to drive the compression plate to provide compression such as a drive cam 7 . The ink ribbon which carries the ink or dye is supplied by a ribbon supply spool 10 to provide fresh, unused ink. The used or depleted portion of the ink ribbon after printing is taken up by ribbon take-up spool 11 . (A patch for the transparent overcoat material can be on the same ribbon as the ink or dye patches for transfer, or the overcoat material can be on a separate ribbon, although for simplicity the ribbon having the overcoat patch will be referred to as the “ink” ribbon. For proper conveyance of the ink ribbon web, there may be one or more than one guide rollers for proper steering, first ribbon guide roller 8 and second ribbon guide roller 9 . The ink or dye is transfer to a receiver sheet that is on a pre-print paper driven path 12 and printed paper driven path 14 . This assembly is driven in to contact with an elastomer roller typically called a platen roller 13 . During printing, the used or depleted ink ribbon holding the transparent overcoat layer is peeled from the receiver sheet, leaving the overcoat on the receiver sheet. The peeling is accomplished through the use of a stripping plate or similar means such as a peeling plate, nose piece or the like. The peeling plate may be directly attached to the heat sink or to the compression plate, and both are at a set position with respect to the platen roller, receiver paper, ink ribbon and thermal head during printing. The means for stripping typically has a radius edge for applying pressure at the point of peeling without damage to the moving web or ribbon.
For example, in a thermal printer an 18-mm diameter platen roller, having a horizontal distance of stripper plate to the platen roller center line of 4.8 mm, the vertical distance of stripper plate to the platen roller tangent point is −1.38 mm, preferably distance from a true horizontal line between the thermal head and platen roller is 0.1 mm to −0.5 mm, most preferably about −0.35 mm. This results in a deviation from the nominal manufacturing set point of the stripper plate on a KODAK Photo Printer to equal −0.15 mm. In the case of −1.38 mm, the arc length between the horizontal tangent point and vertical tangent Point is 5.062 mm. In such a case, the smallest angle between platen roller and the stripper plate is 0 degrees, which is a true horizontal line, and the largest angle from a true horizontal line between the platen roller and stripper plate is 32.14 degrees. Consistent with these dimensions, the preferred angle between platen roller and stripper plate is 1.19 to 3.58 degrees.
EXAMPLES
Printing
This example shows improved gloss from adjustment of stripper plate assembly according to the present invention. Using KODAK Photo Printer® Kit 6400 (Eastman Kodak Co. Catalog No. 180-2016) receiver with the test color ribbon given below and a KODAK Photo Printer® 6400, a Status A neutral density image with a maximum density of at least 2.3 was printed on the receiver described above.
The color ribbon-receiver assemblage was positioned on an 18 mm platen roller and a thermal print head with a load of 3.18 Kg pressed against the platen roller. The thermal print head has 1844 independently addressable heaters with a resolution of 300 dots/inch and an average resistance of 4800 ohms. The imaging electronics were activated when an initial print head temperature of 37° C. had been reached. The assemblage was drawn between the printing head and platen roller at 70.5 mm/sec (1.2 ms line time) for yellow, magenta and cyan, 42 mm/sec (2.0 ms line time) for clear protective coat layer. Printing maximum density required a duty cycle of 90% “on” time per printed line.
The voltage supplied was 25 volts resulting in an instantaneous peak power of approximately 0.131 Watts/dot and the maximum total energy required to print Dmax was 0.1216 mJoules/dot for the sequential printing process of yellow, magenta, cyan and 0.2026 mJoules/dot for clear protective coat layer to obtain the desired neutral image.
In addition to the printing head and platen roller, a metal plate was positioned past the print head/platen interface to peel or strip the color ribbon from the receiver. Testing was conducted by changing the distance, or time, that the color ribbon is kept in contact with the receiver and measuring the gloss level.
The laminate formulations used in this aspect of the formulation are those described below
The gloss was determined at sixty degrees using a BYK-Gardner micro-TRI-gloss meter. The aperture of the gloss meter was placed perpendicular to the direction of printing.
Donor Element
Protection layer donor elements were prepared by coating on the back side of a 6 μm poly(ethylene terephthalate) support:
1) a subbing layer of titanium alkoxide, Tyzor TBT®, (DuPont Corp.) (0.13 g/m 2 ) from a n-propyl acetate and n-butyl alcohol solvent mixture (85/15), and 2) a slipping layer containing an aminopropyl-dimethyl-terminated polydimethylsiloxane, PS513® (United Chemical Technologies) (0.01 g/m 2 ), a poly(vinyl acetal) binder, KS-1, (Sekisui Co.), (0.38 g/m 2 ), p-toluenesulfonic acid (0.0003 g/m 2 ) and candellila wax (0.02 g/m 2 ) coated from a solvent mixture of 3-pentanone, methanol and distilled water (88.7/9.0/2.3).
On the front side of the element was coated a transferable overcoat layer of poly(vinyl acetal), KS-10, (Sekisui Co.), at a laydown of 0.63 g/m 2 , colloidal silica, IPA-ST (Nissan Chemical Co.), at a laydown of 0.46 g/m 2 , 4 μm divinylbenzene beads at a laydown of 0.11 g/m 2 and CGP1644 (Ciba Corp), a triazine UV absorber, at a laydown of 0.11 g/m 2 . The materials were coated from the solvent 3-pentanone.
Table 1 below shows increased Gloss as a result of stripper plate position or increased time to peel.
TABLE 1
Change
(Deviation) in
Stripper Plate
from Nominal
Stripper Plate
Manufacturing
Time in
Average Gloss
Position
Position
milliseconds
Measurement
1
+0.1 mm
68.046
67
2
0.0 mm
68.091
67
3
−0.1 mm
68.164
67
4
−0.2 mm
68.267
70
5
−0.3 mm
68.400
70
The data in Table 1 above indicates that a change in the stripper plate position such that the time between printing and peeling of the donor and receiver results in an increased gloss. During experimentation, the stripper plate position with respect to the thermal print head, ink ribbon, receiver paper and platen roller was adjusted using a fixture. Table 1 shows that position 2 of the stripper plate is the nominal manufacturing position and, therefore, the deviation from normal manufacturing procedures on the KODAK Photo Printer 6400 is 0.0 mm. Position 1 moves the stripper plate position upwards, or away from the platen roller. Positions 3 through 5 moves the stripper plate downwards, or closer to the platen roller. By moving the stripper plate position vertically down, the actual distance between the thermal head and stripper plate is increased. This increases in length also translates into an increase in time between printing and stripping or peeling of the ribbon and the receiver paper. Thus, in particular, testing has indicated that by maintaining, within a certain range, the time that the color ribbon is kept in contact with the receiver increases the gloss level.
PARTS LIST
1 thermal print head
2 IC (integrated circuit) cover
3 heat sink
4 compression spring
5 driven compression plate
6 stripping plate
7 drive cam
8 first guide roller
9 second guide roller
10 ribbon supply spool
11 ribbon take-up spool
12 pre-print paper driven path
13 platen roller
14 printed paper driven path
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This invention relates to a method for transferring a protective overcoat for a thermal print wherein the protective overcoat is applied to a dye-donor element under predesigned conditions after thermal dye transfer, the dye-donor element comprising patches of dye for transfer to a thermal print to provide a protective layer thereon. In particular, the invention improves the process of providing an improved level of gloss to the transferred protective overcoat. The method involves a preselected duration between printing and peeling the transferable laminate patch, respectively, to and from the donor. The invention is particularly advantageous at lower line times, faster printing, for thermal prints with high gloss.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims priority to and the benefit of co-pending U.S. provisional patent application Ser. No. 60/612,241, filed Sep. 22, 2004, which application is incorporated herein by reference in its entirety.
STATEMENT REGARDING FEDERALLY FUNDED RESEARCH OR DEVELOPMENT
This invention was made with government support awarded by the Department of Energy under Grant Number DE-FG02-96ER45571. The government has certain rights in the invention.
FIELD OF THE INVENTION
The invention relates to calculations of materials properties in general and particularly to computational methods that employ a combination of databases and algorithmic methods.
BACKGROUND OF THE INVENTION
Ab-initio calculations, using quantum mechanical principles to calculate properties of materials, have been used for some time to predict features of materials. However, such calculations do not make use of the wealth of computed and measured information obtained on materials, in studying a system that has not previously been investigated or for which certain compositions or properties have not been investigated.
Prior to this work, no algorithms to extract knowledge and mathematical rules from the body of existing data on solid materials have been identified, limiting the usefulness of such data in predicting unknown properties of materials. Only simple heuristic models currently exist, in which visual correlations between properties, or few-parameter fits with pre-conceived (and therefore limited) models, are used to make predictions. Examples of heuristic models are Miedema's rules for compound formation in alloys, or Pettifor maps for making predictions of the structure of a new binary compound.
A number of problems in trying to predict structure information about new compounds have been observed, including difficult and time consuming calculations in ab-initio methods, and difficulties in extracting rules for use in heuristic models.
There is a need for systems and methods that combine information already known in a mathematical framework which can either predict directly attributes of materials or points at a few ab-initio calculations, which, when performed, will give the attribute of interest for the material.
SUMMARY OF THE INVENTION
In one aspect, the invention relates to a method for predicting a structure of an inorganic material of interest. The method comprises the following steps. For an inorganic material of interest different from an inorganic reference material, the method comprises the steps of selecting the inorganic material of interest, obtaining for the inorganic material of interest an initial value, the initial value being a selected one of a computed initial value and a measured initial value of at least one parameter of the inorganic material of interest, the initial value differing from a descriptor of an element present in the inorganic material of interest, providing the initial value of the at least one parameter for the inorganic material of interest to a computational procedure, computing with the computational procedure to obtain a result, and deducing a candidate structure of the inorganic material of interest based on the result, whereby data is generated to predict the structure of the inorganic material of interest. The computational procedure is a selected one of a computation that obtains a relationship between a known structure of at least one known inorganic reference material and a known initial value of a parameter of the at least one known inorganic reference material and that applies the relationship to the initial value of the at least one parameter for the inorganic material of interest, and a computation that compares the initial value of the at least one parameter for the inorganic material of interest with a known value of a corresponding parameter of the at least one known inorganic reference material, and that applies the comparison to a structural parameter of the known reference material.
In one embodiment, the obtaining step includes obtaining an additional initial value of at least one parameter of the inorganic material of interest, the additional initial value comprises a descriptor of an element present in the inorganic material of interest. In one embodiment, the method further comprises the optional step of computing a new parameter value for the candidate structure of the inorganic material of interest. In one embodiment, the method further comprises the optional step of, as necessary, iteratively performing the steps of providing the initial value of the at least one parameter for the inorganic material of interest wherein the new computed parameter is substituted for the initial value, deducing a candidate structure of the inorganic material of interest, and computing yet another new parameter value for the candidate structure.
In one embodiment, the step of iteratively performing the steps of providing, deducing, and computing is terminated when a metric relating to an incremental change of the parameter of the inorganic material of interest is less than a predefined difference. In one embodiment, at least one of the steps of providing, computing, and deducing is performed in a computational system comprises a programmed computer. In one embodiment, the computational system comprises a programmed computer further comprises a computer program containing an algorithm. In one embodiment, the computational system comprises a programmed computer further comprises a knowledge machine. In one embodiment, the inorganic material of interest comprises a plurality of inorganic materials. In one embodiment, the inorganic reference material comprises a plurality of materials. In one embodiment, the initial value of the inorganic material of interest comprises a plurality of initial values for a plurality of parameters of the inorganic material of interest. In one embodiment, the initial value of the parameter of the inorganic reference material comprises a plurality of initial values for a plurality of parameters of the inorganic reference material. In one embodiment, the known value of the parameter of the inorganic reference material comprises at least one machine-readable datum. In one embodiment, the at least one machine-readable datum comprises an element of a database. In one embodiment, the structure is characterized uniquely. In one embodiment, the structure is partially described. In one embodiment, the structure comprises a selected one of a charge density, a structural property, a parameter of a crystal structure, a parameter of a non-crystalline structure, a symmetry of a structure, a space group, a point group, an electronic structure property, and a quantity calculable from one or more of a quantum-mechanical ground state, a quantum mechanical excited state, and a generalized thermodynamic susceptibility of the inorganic material of interest. In one embodiment, the prediction of the structure of the inorganic material of interest comprises a prediction that the inorganic material of interest is not stable under a defined condition. In one embodiment, the structure is a function of temperature. In one embodiment, the structure is a function of pressure. In one embodiment, the structure is a function of volume. In one embodiment, the structure is a function of a thermodynamic field or a thermodynamic force. In one embodiment, the structure is a function of chemical composition. In one embodiment, the step of computing comprises applying a computational method involving a selected one or more of a partial least square (PLS) method, a Principal Component Analysis (PCA) method, a data mining method, a knowledge discovery method, a visualization method, a statistical method, a regression method, a linear regression method, a non-linear regression method, a Bayesian method, a clustering method, a neural network method, a support vector machine method, a decision tree method, and a cumulant expansion.
In another aspect, the invention features a method for predicting a property of an inorganic material of interest. The method comprises the following steps. For an inorganic reference material, the steps of selecting an input data set and an output data set wherein the output data set is a subset of the input data set, and identifying a computational procedure that generates a member of the output data set when a member of the input data set comprises an initial value of a parameter of the inorganic reference material is used as input. For an inorganic material of interest different from the inorganic reference material, the steps of selecting the inorganic material of interest, obtaining for the inorganic material of interest an initial value, the initial value being a selected one of a computed initial value and a measured initial value of at least one parameter of the inorganic material of interest, providing the initial value of the at least one parameter for the inorganic material of interest to the computational procedure, computing with the computational procedure to obtain a result, and deducing a candidate property of the inorganic material of interest based on the result, whereby data is generated to predict the property of the inorganic material of interest.
In one embodiment, the method further comprises the optional step of computing a new parameter value for the candidate property of the inorganic material of interest. In one embodiment, the method further comprises the optional step of, as necessary, iteratively performing the steps of providing the initial value of the at least one parameter for the inorganic material of interest wherein the new computed parameter is substituted for the initial value, deducing a candidate property of the inorganic material of interest, and computing yet another new parameter value for the candidate property. In one embodiment, the step of iteratively performing the steps of providing, deducing, and computing is terminated when a metric relating to an incremental change of the parameter of the inorganic material of interest is less than a predefined difference. In one embodiment, at least one of the steps of providing, computing and deducing is performed in a computational system comprises a programmed computer. In one embodiment, the computational system comprises a programmed computer further comprises a computer program containing an algorithm. In one embodiment, the computational system comprises a programmed computer further comprises a knowledge machine. In one embodiment, the initial value of the parameter for the inorganic material of interest and the initial value of the parameter for the inorganic reference material are parameters that describe a corresponding material feature. In one embodiment, the inorganic material of interest comprises a plurality of inorganic materials. In one embodiment, the inorganic reference material comprises a plurality of materials. In one embodiment, the initial value of the inorganic material of interest comprises a plurality of initial values of the inorganic material of interest. In one embodiment, the initial value of the parameter of the inorganic reference material comprises a plurality of initial values for a plurality of parameters of the reference material. In one embodiment, the initial value of the parameter of the inorganic reference material comprises at least one machine-readable datum. In one embodiment, the at least one machine-readable datum comprises an element of a database. In one embodiment, at least one of the initial values of the inorganic material of interest and the predicted property of the inorganic material of interest is added to the database. In one embodiment, the property comprises a selected one of an energy, a charge density, a structural property, a parameter of a crystal structure, a parameter of a non-crystalline structure, a symmetry of a structure, a space group, a point group, an optical property, an electromagnetic property, a mechanical property, a quantum-mechanical property, an electronic structure property, a thermodynamic property, a magnetic property, and a quantity calculable from one or more of a quantum-mechanical ground state, a quantum mechanical excited state, and a generalized thermodynamic susceptibility of the inorganic material of interest. In one embodiment, the prediction of the property of the inorganic material of interest comprises a prediction that the inorganic material of interest is not stable under a defined condition. In one embodiment, the property is a function of temperature. In one embodiment, the property is a function of pressure. In one embodiment, the property is a function of volume. In one embodiment, in one embodiment, the property is a function of a thermodynamic field or a thermodynamic force. In one embodiment, the property is a function of chemical composition. In one embodiment, the step of computing comprises applying a computational method involving a selected one or more of a partial least square (PLS) method, a Principal Component Analysis (PCA) method, a data mining method, a knowledge discovery method, a visualization method, a statistical method, a regression method, a linear regression method, a non-linear regression method, a Bayesian method, a clustering method, a neural network method, a support vector machine method, a decision tree method, and a cumulant expansion.
In one aspect, the invention relates to a method for predicting a property of an inorganic material of interest. The method comprises the steps of, for an inorganic material of interest different from an inorganic reference material, selecting the inorganic material of interest; obtaining for the inorganic material of interest an initial value, the initial value being a selected one of a computed initial value of at least one parameter or attribute for at least one proposed feature of the inorganic material of interest and a measured initial value of at least one parameter for a known feature of the inorganic material of interest; providing the initial value of the at least one parameter for the inorganic material of interest and a selected one of a computed parameter of the reference material and a measured parameter of the reference material to a computational procedure to obtain a result; deducing a candidate feature or value of an attribute of the inorganic material of interest based on the result; optionally computing a new parameter value for the candidate feature of the inorganic material of interest; and optionally, as necessary, iteratively performing the steps of providing the initial value of the at least one parameter for the inorganic material of interest wherein the new computed parameter is substituted for the initial value, deducing a candidate feature of the inorganic material of interest, and computing yet another new parameter value for the candidate feature; whereby a suitable amount of data is generated to predict the property of the inorganic material of interest.
In one embodiment, the computed parameter for the inorganic material of interest and the selected parameter for the reference material are parameters of the same type. In one embodiment, at least one of the steps of providing, deducing and computing is performed in a computational system comprising a programmed computer. In one embodiment, the computational system comprising a programmed computer further comprises a computer program containing an algorithm. In one embodiment, the computational system comprising a programmed computer further comprises a knowledge machine. In one embodiment, the inorganic material of interest comprises a plurality of inorganic materials. In one embodiment, the reference material comprises a plurality of materials. In one embodiment, the initial value of the inorganic material of interest comprises a plurality of initial values of the inorganic material of interest. In one embodiment, the selected one of the computed parameter of the reference material and the measured parameter of the reference material comprises a plurality of parameters of the reference material. In one embodiment, the selected one of the computed parameter of the reference material and the measured parameter of the reference material comprises at least one machine-readable datum. In one embodiment, the at least one machine-readable datum comprises an element of a database. In one embodiment, the property comprises a selected one of an energy, a charge density, a parameter of a crystal structure, a space group, a point group, an optical property, an electromagnetic property, a mechanical property, a quantum-mechanical property, an electronic structure property, a thermodynamic property, a magnetic property, and a quantity calculable from a quantum-mechanical ground state or generalized thermodynamic susceptibility of the inorganic material of interest. In one embodiment, the prediction of the property of the inorganic material of interest comprises a prediction that the inorganic material of interest is not stable under a defined condition. In one embodiment, the proposed feature is a function of temperature. In one embodiment, the proposed feature is a function of pressure. In one embodiment, the proposed feature is a function of a thermodynamic field or a thermodynamic force. In one embodiment, the proposed feature is a function of chemical composition. In one embodiment, the step of iteratively performing the steps of providing, deducing, and computing is terminated when a metric relating to an incremental change of the parameter of the inorganic material of interest is less than a predefined difference. In one embodiment, the step of computing comprises applying a computational method involving a selected one of a partial least squares (PLS) method, a Principal Component Analysis (PCA) method, a data mining method, a knowledge discovery method, a visualization method, a statistical method, a regression method, a linear regression method, a non-linear regression method, a Bayesian method, a clustering method, a neural network method, a support vector machine method, a decision tree method, and a cumulant expansion.
In one aspect, the invention relates to a method for generating a computational procedure applicable to predicting a property of an inorganic material of interest. The method comprises the steps of based on a selected one of an experimentally measured datum and a calculated datum for a reference material, deducing a mathematical relationship that employs parameters descriptive of the datum; and generating a computational procedure based on the mathematical relationship, the computational procedure employing a representation of the mathematical relationship that is other than a visual representation, the computational procedure comprising at least one computational step, the computational procedure useful to predict a property of a inorganic material of interest. In one embodiment, the mathematical relationship can be selected to have optimal predictive power.
In one embodiment, the method further comprises the step of applying the computational procedure to predict a property of the inorganic material of interest. In one embodiment, the method further comprises the step of adding the property of the inorganic material of interest to a database. In one embodiment, the method further comprises the step of refining the computational procedure based on the contents of the database after the addition of the property of the inorganic material of interest to the database.
In another aspect, the invention relates to a method for generating a computational procedure applicable to predicting a property of an inorganic material of interest. The method comprises the steps of based on a selected one of an experimentally measured datum and a calculated datum for a reference material, deducing a mathematical relationship that employs parameters descriptive of the datum; and generating a computational procedure based on the mathematical relationship, the computational procedure comprising at least one computational step, the computational procedure employing a representation of the inorganic material using a combination of at least two chemical elements as an independent variable of the representation, the computational procedure useful to predict a property of a inorganic material of interest.
In one embodiment, the method further comprises the step of applying the computational procedure to predict a property of the inorganic material of interest. In one embodiment, the method further comprises the step of adding the property of the inorganic material of interest to a database. In one embodiment, the method further comprises the step of refining the computational procedure based on the contents of the database after the addition of the property of the inorganic material of interest to the database.
In yet another aspect, the invention relates to a method of predicting at least one candidate structure for a compound not known to exist comprising at least two chemical elements. The method comprises the steps of employing as input a selected one of known information about at least one stable structure in a chemical system comprising the at least two chemical elements and a calculated energy of a proposed structure in the chemical system comprising the at least two chemical elements; providing the input to a computational element operating a selected one of an algorithm and a knowledge machine; and calculating the at least one candidate structure for the compound comprising the at least two chemical elements.
In one embodiment, the method further comprises repetition of the steps of employing as input a selected one of known information, providing the input to a computational element, and calculating at least one additional candidate structure, whereby a plurality of predicted candidate structures is generated as output. In one embodiment, the list of predicted candidate structures comprises fewer than 20 structures. In one embodiment, a probability exceeds 90% that the correct structure for the compound comprising the at least two chemical elements is present in the list of predicted candidate structures. In one embodiment, the algorithm or knowledge machine is derived by applying a data mining algorithm on a database of computed energies of at least one crystal structure in at least one materials system. In one embodiment, the data mining algorithm is an algorithm involves a selected one of a partial least square (PLS) method, a Principal Component Analysis (PCA) method, a data mining method, a knowledge discovery method, a visualization method, a statistical method, a regression method, a linear regression method, a non-linear regression method, a Bayesian method, a clustering method, a neural network method, a support vector machine method, a decision tree method, and a cumulant expansion. In one embodiment, the data mining algorithm is exercised on a database of experimentally identified crystal structures. In one embodiment, the database of experimentally identified crystal structures is a selected one of a Crystmet database, an ICSD database, and a Pauling File. In one embodiment, the algorithm or knowledge machine is derived by applying a data mining algorithm on a database of measured energies of at least one crystal structure in at least one materials system.
In a still further aspect, the invention relates to a computer program recorded on a machine-readable medium, the computer program configured to predict a property of the inorganic material of interest. The computer program comprises a selection module for selecting a inorganic material of interest different from an inorganic reference material; an estimation module that provides an initial value for the inorganic material of interest, the initial value being a selected one of a computed initial value of at least one parameter for at least one proposed feature of the inorganic material of interest and a measured initial value of at least one parameter for a known feature of the inorganic material of interest; a calculation module that receives the initial value of the at least one parameter for the inorganic material of interest and a selected one of a computed parameter of the reference material and a measured parameter of the reference material and that calculates a result; a state deducing module that deducing a candidate feature of the inorganic material of interest based on the result; and a computation module that computes a new parameter value for the candidate feature of the inorganic material of interest.
In one embodiment, the computer program further comprises an iteration module that, optionally, as necessary, iteratively command the performance of the steps of receiving the initial value of the at least one parameter for the inorganic material of interest wherein the new computed parameter is substituted for the initial value, deducing a candidate feature of the inorganic material of interest, and computing yet another new parameter value for the candidate feature, so as to provide an improved prediction of the property of the inorganic material of interest. In one embodiment, the computer program further comprises a data storage module that controls the recording of the predicted property of the inorganic material of interest in a database. In one embodiment, the computer program further comprises a data retrieval module that controls the retrieval of data from a database.
The foregoing and other objects, aspects, features, and advantages of the invention will become more apparent from the following description and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
The objects and features of the invention can be better understood with reference to the drawings described below, and the claims. The drawings are not necessarily to scale, emphasis instead generally being placed upon illustrating the principles of the invention. In the drawings, like numerals are used to indicate like parts throughout the various views.
FIG. 1 is a diagram showing prediction test results, according to principles of the invention;
FIG. 2 shows the mixing energies as predicted by the algorithm for the Ag—Cd system at iteration 3, according to principles of the invention;
FIG. 3 shows the mixing energies as predicted by the algorithm for the Ag—Cd system at iteration 4, according to principles of the invention;
FIG. 4 shows the mixing energies as predicted by the algorithm for the Ag—Cd system at iteration 5, according to principles of the invention;
FIG. 5 shows the mixing energies as predicted by the algorithm for the Ag—Cd system at iteration 11, according to principles of the invention;
FIG. 6 shows the mixing energies as predicted by the algorithm for the Ag—Cd system at iteration 23, according to principles of the invention;
FIG. 7 shows the average number of calculated energies needed (averaged over all the predicted systems) as a function of the accuracy required, according to principles of the invention;
FIG. 8 shows a convex hull calculated for the Ru—Y alloy system using 174 different crystal structures, according to principles of the invention;
FIG. 9 is a flow diagram showing an exemplary method of calculation, according to principles of the invention; and
FIG. 10 is a high level flow diagram showing the relationships between reference data, new system data and a data mining method according to principles of the invention.
DETAILED DESCRIPTION OF THE INVENTION
The invention relates to systems and methods that utilize information in databases to provide guidance in selecting algorithmic methods of computation, and that generate information that is introduced into one or more databases so as to inform subsequent calculations, by which combination both the algorithmic methods are improved and the likelihood of obtaining correct results of calculation are also improved. In the present description, the systems and method of the invention are applied to chemical systems for prediction of the existence (or non-existence) of compounds and for prediction of the structures of compounds found to exist. The systems and methods of the invention provide efficient, cost-effective, and expeditious procedures for making assessments of features, properties and attributes of materials of interest when compared to experimental methods, in which a material of interest is first synthesized, and the features, properties and attributes are then measured. The information provided by the systems and methods of the invention can provide guidance in selecting a material to synthesize, based on the predicted features, properties and attributes.
According to systems and methods of the invention, one must distinguish between “computed” values (or alternatively, “calculated” values) and “measured” values for parameters or features of compounds. As used herein, the term “computed,” as in “computed value,” is intended to denote a value that is primarily derived from theory and computation, with limited experimental input. For example, a computed value is often obtained for a composition of matter that is not known to exist, or that has not been synthesized, and that is postulated or modeled, without a physical substance upon which a measurement can be performed. In contradistinction, a measured value is a value that is obtained by making one or more measurements on a real, physical substance, possibly with further mathematical manipulation of the results of the measurement, but clearly based upon one or more measurements that are actually performed. In some instances, a computed value can be obtained for comparison with a measured value, for example to confirm that the computational method that produces the computed value yields quantities that closely represent the value actually measured (e.g., to validate the computational tool as being reliable, rather than to obtain a value which is also available by experimental procedures on a real, physical substance).
For the purposes of this description, the following terms are defined, in keeping with the generally accepted usage in the field of study of inorganic materials in the liquid and solid states. A “system” is understood to denote a plurality of elements. A binary system denotes a system with two elements, a ternary system has three elements, and so on for additional numbers of elements. A system can often be represented diagrammatically, using such parameters as composition, temperature, pressure, and volume. Sometimes we also refer to a system as an alloy, or as a mixture. A “structure” (or crystal structure) denotes a specific structure, such as a crystallographic structure that can be described in terms of a unit cell, taken on by a system at a particular composition of the system under defined temperature and pressure. A crystallographic structure can be measured for a real structure (as opposed to a computed or calculated structure) by methods such as x-ray diffraction. It is to be understood that it is possible to have multiple structures in a system as one or more of the composition, the temperature, and/or the pressure varies. A “compound” refers to a system at a given composition, corresponding to the exact stoichiometry of the structure. In general, a compound may be thought of as a specific composition that is thermodynamically stable under some set of conditions of composition, temperature and pressure. As is known in the art, a compound may be referred to by a formula, such as A 2 B 3 or A 3 B, where A and B represent the chemical symbols of elements. The structure of a composition may also be referred to using a compound as a descriptor, using a nomenclature for a prototypical composition having the same or an isomorphic structure. As an example, many materials take on the sodium chloride, or NaCl, cubic structure. In addition, or alternatively, structures are also identified by space group and/or point group notation. While every compound does have a structure, the term compound typically does not include or connote crystal structure information. As is also well understood, for a specified composition, temperature and pressure, it may be that no stable compound exists, and correspondingly, no crystal structure is defined, or that a plurality of defined compounds and/or elements may coexist. All of the concepts presented in the above paragraph are well known and commonly used in the description of materials using phase diagrams.
The systems of the invention utilize, and the methods of the invention are carried out with, programmable computers and associated computer programs that are recorded on machine-readable media. The computers and software are in general (but are not required to be) part of computer systems, which can include computers having size and capacity ranging from hand held computational devices to supercomputers. In addition, the computers and software can interface with commonly used input/output devices (such as keyboards, pointing devices, touch screens, video screens, printers, speakers and enunciators), memory and/or storage devices (such as semiconductor, optical, and magnetic memory devices), communication devices (such as modems, networks, and commonly used hard-wired and wireless electronic communication media), and resources in both local and remote locations (such as databases and compendia of electronically accessible published information).
In describing the systems and methods of the invention, definitions for certain additional terms are useful. As used herein, the term “material of interest” is intended to denote a material one wishes to study or to make predictions about. As used herein, the term “reference material” is intended to denote any known material that appears as an entry in a database, or that is otherwise described in an electronically accessible medium or in a paper copy reference work, from which the information is transferred to a computing file for the purpose of the methods described in this work. A known material can be a physical material that has been prepared and studied, or a material studied in theoretical terms for which some characteristic, property, parameter or physical state has been calculated or computed. As used herein, the term “feature,” such as in the usage “a feature of a material,” is intended to denote a generalization that includes a physical state of a material, and any characteristic, property, or parameter of a material. As used herein, for the purposes of the examples given to describe the invention, the term “material” is intended to denote any of condensed matter, solid state material, crystalline material, and inorganic material. It is further contemplated that the kinds of systems and methods described herein may find useful application in studying substances other than those denoted as “materials” herein.
The description of the systems and the methods of the invention are described with respect to several examples.
EXAMPLE 1
Using a Database of Experimentally Measured Crystal Structures to Predict Unknown Structures
Several large experimental databases comprising thermodynamic data of alloy systems are now available. In one embodiment, the invention relates to methods that enable one to use these databases to build algorithms, which then in turn can be used to predict structures or material attributes not in the database. In this example, a cumulant expansion is built from a database of experimentally measured crystal structures. The cumulant expansion then gives with high accuracy candidate structures for systems that were not included in building the cumulant expansion. As such the method can predict structure for compounds in new systems or systems that are only partially characterized.
Extracting and Processing the Data:
In one embodiment, data was extracted from the Pauling File Inorganic Materials Database, Binaries Edition, Version 1.0. There are 28,457 structure type listings in this database. In this database, a listing includes prototype name, alloy system, formula and modifier (high temperature, high pressure), among other things (space group number, Pearson symbol, etc.).
In the present example, we are interested in looking at stable structure types at low temperature and pressure, so we have removed all listings identified by the Pauling File as high temperature or high pressure.
We determine a set of allowed compositions for each structure type, based on the distribution of entries for that structure type. Next we assign each of these composition to the nearest rational fraction, out of a set of fractions that includes the following:
0%
10% (1/10)
16.7% (1/6)
20% (1/5)
22% (2/9)
25% (1/4)
28.6% (2/7)
30% (3/10)
33.3% (1/3)
37.5% (3/8)
40% (2/5)
42.9% (3/7)
44.4% (4/9)
50% (1/2)
55.6% (5/9)
57.1% (4/7)
60% (3/5)
62.5% (5/8)
66.7% (2/3)
70% (7/10)
71.4% (5/7)
75% (3/4)
77.8% (7/9)
80% (4/5)
83.3% (5/6)
85.7% (6/7)
90% (9/10)
100%
This discretization (or binning) of compositions is performed to improve the statistics. The methods described herein are not limited to these compositions. After binning the listings into this set of compositions, we remove all duplicate entries. Two entries are considered to be duplicates if they have the same prototype name, composition and alloy system.
We have extracted a subset of the data in order to compare similar alloys. We are using entries for alloy systems that do not contain any non-metals, defined as the elements He, B, C, N, O, F, Ne, Si, P, S, Cl, Ar, As, Se, Br, Kr, Te, I, Xe, At, and Rn. This subset of the data contains 4,836 entries. The method can be extended to include alloys including these non-metals.
Statistics:
We have calculated some statistics for this dataset in order to evaluate the predictive ability of the data. First we define some variables. In general, c i and c j are fractions in the range of 0.0<c i , c j <1.0.
N α(i) =Number of unique entries for structure type alpha at composition c i .
N α(i)β(j) =Number of systems with structure type alpha at composition c i and structure type beta at composition c j .
We can improve the statistics by considering the symmetry of the data. The only difference between structure type α at composition c i and structure type α at composition 1-c i is how the system is defined. That is to say that the system A-B at composition c i in A can be represented as A(c i )−B(1-c i ), e.g., c i percent element A and (1-c i ) percent element B. In the statistical analysis we combine the statistics to include the symmetric equivalent structure type or pair of symmetric equivalent structure types.
Conditional Pair Probabilities:
The conditional pair probability is defined as the probability that structure type β appears in a system in which structure type α appears. This is the ratio of the number of times the two structures appear in the same system to the number of times structure type α appears.
P (β( j )|α( i ))= N α(i)β(j) /N α(i)
These pair probabilities embed information about correlation between the appearance of various structures and can be used to predict structure. The use of pair correlations in this example should be seen in no way as a limitation to pair correlations. Higher order correlations, such as the occurrence of three crystal structures together in one alloy can also be used if sufficient data is available. The conditional pair probabilities are collected based on all the data in the previously defined dataset which is extracted from the Pauling files.
Cumulant Expansion:
A cumulant expansion is built to give the model predictive power. A cumulant expansion is a decomposition of a probability mass function into smaller parts. Cumulant expansions are described in the appended document entitled “Coarse-Graining and Data Mining Approaches to the Prediction of Structures and their Dynamics,” which was filed as part of the disclosure of U.S. Ser. No. 60/612,241, the entire disclosure of which has been incorporated herein by reference. When no approximations are applied, a cumulant expansion is an exact representation of the full probability mass function. The exemplary method described herein determines the probability that some structures occur together in a new system of interest, from the limited information known about that new system, and the pair correlation determined from the Pauling file database. For example, given that two structures are known in the new system, the pair correlations from the Pauling files can be used to find which other crystal structures may occur in conjunction with these two structures. The cumulant expansion is a mathematical way to calculate proper probabilities for crystal structure to appear in a system, consistent with the structures already known about the system.
We define the term “event” to mean that α(c i )=TRUE when structure type alpha is present at composition c i in an alloy system.
An alloy system in a database can be represented as the logical conjunction of each of the individual events comprising the system (i.e., the logical conjunction of events is true for that particular system and any others which list the same structure types at the same compositions).
A measure of the predictive nature of this method is its ability to predict what structure type will appear at a composition given that everything else about the system in question is known. To generate a list of candidate structures we will compute the quantity p(β(c i )|α(c 1 ), . . . , α(c n ) which can be read as: “the probability of structure β(c i ) given that structures α(c 1 ) through α(c n ) have appeared.” Ranking the candidate structures {β(c i )} is based on this probability. The conditional probability can be represented approximately as a cumulant expansion in which only terms including up to two events are retained:
To determine the cumulant expansion, one first collects all known stable structure types for a system of interest. We identify these as structure types α 1 , α 2 . . . α n at compositions c 1 , c 2 , . . . c n . We compute the probability that structure β is present at composition c i as follows:
p
(
β
(
c
i
)
|
α
(
c
1
)
,
…
,
α
(
c
n
)
)
≈
[
p
(
β
(
c
i
)
]
1
-
n
∏
j
=
1
n
p
(
β
(
c
i
)
|
α
(
c
j
)
)
(
1
)
Using a Bayesian estimate for each conditional probability Equation 1 reduces to:
p
(
β
(
c
i
)
|
α
(
c
1
)
,
…
,
α
(
c
n
)
)
≈
p
(
β
(
c
i
)
∏
j
=
1
n
p
(
β
(
c
i
)
|
α
(
c
j
)
)
(
2
)
Each probability/conditional probability appearing on the right hand side of Equation 1 can be calculated with Laplace's rule of succession: and
p
(
β
(
c
i
)
)
=
N
β
(
c
i
)
+
1
N
sys
+
2
and
p
(
β
(
c
i
)
|
α
(
c
j
)
)
=
N
β
(
c
i
)
,
α
(
c
j
)
+
1
N
α
(
c
j
)
+
2
.
Prediction Tests:
We performed a set of prediction tests using the experimental database to assess how well the prediction test operates. To simulate a prediction we leave out, or deliberately omit, one alloy system from the dataset used to build the cumulant information. A prediction was made for every structure of the omitted system using two different algorithms described herein. Each of these methods includes creating a list of the structure types that could appear at the composition of interest, ordered by a different, selected, criterion. For each structure type prediction we leave out all entries from the alloy system of the entry we are trying to predict when determining the statistics for that test. To assess the efficiency of these novel algorithms, they are compared to two commonly used approaches.
The first commonly used approach is to randomly pick structures as candidate structures. This is the method that contains the least (e.g., zero) information. We refer to this as the random method. A more informed approach is to rank structures based on the frequency with which they occur in the database. We call this method the frequency of occurrence method. Our two knowledge methods are the following: 1) For each structure type beta that could appear at the composition of interest, we determine the conditional pair probability for beta with each of the other structure types that appear in the system. We then average these conditional pair probabilities, and order the structure types by this average. We refer to this as the averaged conditional pair probability method. The second method is the cumulant method described above. The results of this test are shown in FIG. 1 . FIG. 1 is a diagram that shows the fraction of structure types that one expects would need to be investigated for a given percentage chance of finding the correct structure type. In FIG. 1 , the curves representing each method of interest are indicated by the key in the upper left. The cumulant method gives the best results, slightly better than average conditional pair probability. This shows one way to determine the best prediction techniques. Both our knowledge methods are significantly better than either the random or frequency of occurrence method.
As an example of this technique consider alloy system Al—Pd. The Pauling File has 7 structure type entries for this system. They are presented in Table I as a function of composition.
TABLE I
Structure Type
Composition (percent Al)
Cu
0
Co 2 Si-b
0.33
FeSi
0.5
Ni 2 Al 3
0.6
CaF 2
0.667
Pt 8 Al 21
0.714
Cu
1
As a test of the method we assume we did not know the structure at composition 0.6 and see whether our method can predict it from the knowledge of the other structures. The six structures in the above table other than Ni 2 Al 3 are structures α 1 . . . α 6 for the statistical analysis. Tables II, III, and IV present the ranked lists of structure types with the frequency of occurrence method, averaged conditional pair probability method, and cumulant method.
For this example, the averaged conditional pair probability method ranks the structure 3 rd on a list of possible candidate structures, the cumulant method ranks it first, and the frequency of occurrence method results in a ranking of 7 th Ni2Al3 was ranked first by the cumulant method, and had a probability value with this method over three times as large as the second structure on the list, indicating the strength of cumulant method in predicting short list of very likely structures.
TABLE II
Frequency of Occurrence List
Structure Type
Occurrences
(Cr0.49Fe0.51)
24
Er3Ni2
21
U3Si2
16
Y3Rh2
11
Gd3Ga2
11
Ca16Sb11
10
Ni2Al3
9
Cu5Zn8
6
Zr3Al2
6
Er3Ru2
6
Zr7Ni10
5
Gd3Al2
5
Zr2Al3
4
Li3Al2
3
La2Ni3
3
Dy3Ni2
3
Sr2Sb3
3
Pu31Pt20
3
Ni3Sn2
3
Mg2Cu
3
Ba5Si3
3
Ni13Ga9
3
K2Au3
2
La2O3
2
TaIr
2
Tl2Pt3
2
Ru2Ge3
2
Rb2In3
2
Mg17Al12
2
Ranking 7
Fraction
0.241379310344828
TABLE III
Averaged Conditional Pair Probability List
Normalized Avg. Conditional Pair
Structure Type
Probability
Er3Ni2
0.163
Y3Rh2
0.12
Ni2Al3
0.108
U3Si2
0.09
(Cr0.49Fe0.51)
0.072
Gd3Al2
0.054
Zr3Al2
0.048
Gd3Ga2
0.036
Ca16Sb11
0.036
Cu5Zn8
0.036
Dy3Ni2
0.036
Zr7Ni10
0.03
Er3Ru2
0.024
Ni13Ga9
0.018
Pu31Pt20
0.018
TaIr
0.018
Zr2Al3
0.012
Tl2Pt3
0.012
Mg17Al12
0.012
K2Au3
0.012
Mg2Cu
0.006
Ba5Si3
0.006
La2Ni3
0.006
Sr2Sb3
0.006
Ni3Sn2
0.006
Li3Al2
0.006
Ru2Ge3
0.006
La2O3
0
Rb2In3
0
Ranking 3
Fraction 0.103448275862069
TABLE IV
Cumulant Method List
Normalized Cumulant
Structure Type
Expansion
Ni2Al3
0.593207771
Er3Ni2
0.167482327
Y3Rh2
0.071184933
(Cr0.49Fe0.51)
0.060556627
U3Si2
0.060507193
Gd3Ga2
0.008898117
Gd3Al2
0.008898117
Zr3Al2
0.007266795
Ca16Sb11
0.003806417
Dy3Ni2
0.003163775
Zr7Ni10
0.002966039
Cu5Zn8
0.002422265
Er3Ru2
0.001730189
Pu31Pt20
0.001186416
TaIr
0.000889812
Ni13Ga9
0.000790944
Zr2Al3
0.00074151
Tl2Pt3
0.000444906
Mg17Al12
0.000444906
K2Au3
0.000444906
Mg2Cu
0.000395472
Ba5Si3
0.000395472
La2Ni3
0.000395472
Li3Al2
0.000395472
Sr2Sb3
0.000395472
Ni3Sn2
0.000395472
Ru2Ge3
0.000296604
La2O3
0.000148302
Rb2In3
0.000148302
Ranking 1
Fraction
0.0344827586206897
EXAMPLE 2
Using a Library/Database of Calculated Energies of Structure in a Group of Binary Alloys
Just as experimental information can be used to extract knowledge and formulate algorithms used for predicting the structure of new materials, calculated data can be used in the database. In this example, we show how knowledge extracted with Partial Least Square Methods (PLS) from a dataset of calculated structure energies, is used to predict likely structures in a new system. Every time a structure is suggested, its energy can be calculated, which in turn improves the accuracy of the prediction. Partial Least Squares methods are known in the art and are described briefly in the document entitled “Coarse-Graining and Data Mining Approaches to the Prediction of Structures and their Dynamics” and references therein, which was filed as part of the disclosure of U.S. Ser. No. 60/612,241, the entire disclosure of which has been incorporated herein by reference.
A database was constructed containing the calculated energy of 114 structure types in 55 binary alloys. The ground state energy of these structures was computed with Density Functional Theory in the Local Density Approximation as implemented in the Vienna Ab-Initio Simulation Package (VASP). The method is not limited to energies obtained with this package, but can be used with any model for calculating the energy of structures, including quantum mechanical approaches, semi-empirical approaches or empirical energy models.
In some embodiments, the PLS/knowledge extraction step is applied to data to select an algorithmic method for application.
For a new system of interest, which is the Ag—Cd system in the present example, the algorithm is initialized with the calculated energies of pure elemental Ag and Cd in the fcc, bcc and hcp structures. In the first iteration, there is not enough information available for the Ag—Cd system to generate predictions from our algorithm. Hence the algorithm extracts a frequent structure prototype from the library and calculates its ab-initio energy. In this case, the suggested structure to calculate is DO 19 . This is repeated in iteration 2 with a suggested structure of Ll 0 . From iteration 3 on, the knowledge algorithm can be used to extract predictions from the database. In iteration 3, the PLS method is used to estimate the energy of all 114 structure types that have not been calculated yet for Ag—Cd. FIG. 2 shows the mixing energies as predicted by the algorithm for the Ag—Cd system at iteration 3 . The algorithm suggest a new ground state structure at concentration C=33% labeled as “130.” The label “130” refers to a label number in the database and is a structure with stoichiometry A 4 B 2 and is a decoration of an hcp lattice.
With the energy of structure “130” calculated the correlation with the database can be made better and the PLS prediction improved. This leads to a more accurate prediction of the energies for all the structures in the database. In the next iteration, the algorithm predicts that B 19 will be a stable structure, as shown in FIG. 3 .
At each iteration of this algorithm, the energy of a new structure is calculated based on the method's suggestion. If after the PLS prediction, there is no new stable structure suggested, the structure which is predicted closest to the convex hull is calculated. For example, in Iteration 5 , the energies and convex hull in FIG. 4 is obtained. Since the ground states are the same as in FIG. 3 , the structure C Cd =0.75 is taken as the next structure to compute as it is closest to the hull.
FIG. 5 shows the ground state hull after 11 iterations. At this point a total of 16 energies have been calculated (10 alloy structures and 6 elements).
This iterative scheme can be continued. At each iteration a new candidate ground state is suggested, which is then calculated. Once the energy of this structure is available the PLS prediction can be improved, which leads to the next iteration. In this example, 23 iterations were performed. FIG. 6 shows the ground states after 23 iterations. At this point, the algorithm has found all the ground states that it can find, based on the database used.
This prediction iteration can be performed on all the systems in the database. To “predict: each system, it is removed from the database and PLS is applied to the remaining database. FIG. 7 shows the average number of calculated energies needed (averaged over all the predicted systems) as a function of the accuracy required. Ninety percent accuracy can be achieved with on average 26 structural energy calculations. This is a significant improvement over randomly picking structures.
EXAMPLE 3
Combining Experimental and Calculated Data in Structure Search Algorithm
In this example we show how information contained within an experimental database of crystal structures can be combined with calculated energies of structures when performing a search for remaining, as yet unknown, stable structures in a materials system of interest. This method suggests the best structures for further calculation based upon what is known from previous calculations and the information in the experimental database.
Method:
Defining “known” information:
After a series of calculations have been conducted (using a pre-defined set of structures), a ground state convex hull can be constructed for the alloy system of interest. For example, FIG. 8 shows a convex hull calculated for the Ru—Y alloy system using 174 different crystal structures.
The convex hull is the T=0 boundary condition for the alloy phase diagram. The vertices of the convex hull are the stable phases at T=0. In this example the calculated energies indicate that structures C14 at x=0.33, C16 at x=0.66, and D 0 11 at x=0.75 are stable compounds. Experimentally, D 0 11 at x=0.75, C14 at x=0.33, and three others not yet calculated are observed, but C16 at x=0.66 is not. The objective of this example is to suggest other structures that may be stable in this system. To define the set of “known” events for this alloy system we will take the intersection of events defining the calculated and experimental results (i.e., D 0 11 and C14 along with the pure elements hcp-Ru, and hcp-Y). This set of events represents the knowledge that is consistent between the calculated and experimental results. Table V illustrates the data obtained from the experimental database, the calculations, and the events relevant to our algorithm.
TABLE V
Events common to- vs. unique to- experimental and calculated data
Experiment
Calculation
Intersection of events
Hcp-Ru
Hcp-Ru
Hcp-Y
Hcp-Y
D0 11
D0 11
C14
C14
(union minus intersection)
C 2 Mn 5
C16
of events
Ru 25 Y 44
Er 3 Ru 2
Calculating Candidate Structure Lists:
To proceed further, our algorithm next finds the set of most likely stable compounds to calculate. Our decision regarding the best candidate structure to calculate will be made based upon a ranking of probabilities similar to those calculated in Example 1. To construct an ordered list of “best” candidates, we will calculate p(β(c i )|α(c 1 ), . . . , α(c n )) for all structures {β(c i )} appearing at compositions other than (x=0.0, x=0.33, x=0.75, and x=1.0). The set of events common to the experimental and calculated information is taken as the known information upon which we will condition our probabilities. In particular, (α(c 1 ), . . . , α(c n )), comprises D 0 11 and C14, hcp-Ru, and hcp-Y.
The cumulant expansion technique described in Example 1 is used to calculate the set of probabilities {p(β(c i )|α(c 1 ), . . . , α(c n ))}, and the experimental database is used for the counts needed to calculate the quantities p(β(c i )|α(c j )) and p(β(c i )). Candidate structures are ordered at each composition by their respective values of p(β(c i )|α(c 1 ), . . . , α(c n )). The actual order in which calculations are conducted might be based on an estimate for the computational time requirement for descending down each list or the relative values of {p(β(c i )|α(c 1 ), . . . , α(c n ))}.
Calculation Followed by Update:
After calculating the best candidate structure, additional agreements/disagreements might be found between the calculated and experimental results. Therefore, what constitutes the known information for the next iteration would be updated for subsequent calculations. This process is shown schematically in FIG. 9 , a flow diagram.
Intersection of Events Yields the Null Set {}:
If the intersection of experimental and calculated results yields the null set, a start-up set of candidates will need to be generated. To address this situation, the search could be initiated in the following manner.
First, two sets of candidate lists are generated, one using only the experimental results as known information, and the other using only the calculated results. Next, the lists are merged, adding the probabilities for each structure type. Finally, candidate lists at compositions common to both sets of lists (i.e. compositions which do not have a listing in either the experimental or calculated results) are renormalized and new structures are then calculated based upon their ranking.
Results:
As stated above, the experimental and calculated data for this system agree on the stability of D 0 11 , C14, and elements hcp-(Ru and Y). The experimental data and calculations differ in that structures C2Mn5, Ru25Y44, and Er3Ru2 are found experimentally and calculation indicates that C16 is stable. In what follows we will attempt to predict the set of candidate structures to calculate at x=0.714, x=0.638, and x=0.60 conditioned on the knowledge of hcp-(Ru and Y), D 0 11 , and C14. In principle, candidate structure lists would be made at all compositions other than x={0.0, 0.33, 0.75, 1.0}, but the results at x={0.60, 0.638, 0.714} are of interest as compounds are known to appear experimentally (serving as our reference). Shown below in Tables VI, VII, and VIII are the rankings of candidate structures based on frequency of occurrence and the method developed in Example 1.
TABLE VI
Candidate Structure list at x = 0.714
Str_type(expt.)
comp
Mn5C2
0.71400
Ranking
Cumulant
Value
Freq
Value
1
Mn5C2
0.99976
Mn5C2
34
2
Sc11Ir4
0.00013
Dy2.12Pd0.88
7
3
Dy2.12Pd0.88
0.00004
Ce2Sn5
5
4
Co2A15
0.00003
5
TABLE VII
Candidate structure list for x = 0.638
Str_type(expt.)
comp
Y44Ru25
0.63800
Ranking
Cumulant
Value
Freq
Value
1
Mn5Si3
0.98836
Mn5Si3
118
2
Cr5B3
0.00375
Pu3Pd5
33
3
Y44Ru25
0.00369
W5Si3
28
4
Pu3Pd5
0.00181
Cr5B3
28
5
Pu5Rh3
14
6
Tm3Ga5
11
7
Y3Ge5
10
8
Y5Bi3
9
9
Yb5Sb3
7
10
Rh5Ge3
6
11
Y44Ru25
6
12
TABLE VIII
Candidate structure list for x = 0.60
Str_type(expt.)
comp
Er3Ru2
0.60000
Ranking
Cumulant
Value
Freq
Value
1
Er3Ru2
0.54381
(Cr0.49Fe0.51)
24
2
Y3Rh2
0.11078
Er3Ni2
21
3
(Cr0.49Fe0.51)
0.09791
U3Si2
16
4
U3Si2
0.09511
Y3Rh2
11
5
Gd3Ga2
11
6
Ni2Al3
10
7
Ca16Sb11
10
8
Cu5Zn8
6
9
Zr3Al2
6
10
Zr7Ni10
5
11
Gd3Al2
5
12
Er3Ru2
5
Although not yet calculated, the structures observed experimentally are likely candidates. At compositions x=0.638 and x=0.60, the cumulant method outperforms (in suggesting the structures observed experimentally) a ranking based on frequency of occurrence. Although the cumulant method does not render Y 44 RU 55 the first candidate to calculate, the method does move Y 44 Ru 55 up the candidate list from position 11 to position 3. Furthermore, the relative probabilities given for structures at x=0.714 suggest Mn5C2 as the best candidate by a large factor. In contrast, the relative frequency of occurrences for structures at x=0.714 do not favor Mn5C2 by as large a factor.
EXAMPLE 4
Prediction of Melting Temperatures of Alloys
It is also possible to use the methods described herein to predict materials attributes or features other than structure. In this example we build an algorithm that can estimate the melting temperature of an alloy.
Experimental melting data on melting points is extracted from published phase diagrams in Binary Alloy Phase Diagrams (Publisher ASM). We collect, at concentrations 25%, 50%, and 75% the maximum and minimum temperatures for the coexistence of the solid and the liquid phases. This table of melting data is given in Table IX. Also, we include the maximum and minimum melting temperature of the alloy in all its concentration range. The formation melting temperature, T f , is defined as the difference between the melting temperature and the weighted average of the pure elements melting point, with the concentrations as weights. For each alloy and concentration, we regress Tf with the coefficients given by PLS. The absolute error is defined as
dT f =T f (predicted)− T f ,
and prediction relative error is given by
ε= dT f /T melting .
Finally, we average the error over all the alloys and we obtain the RMS error of the melting temperature prediction. Because the RMS error is the relative deviation normalized over the melting temperature, the precision of the regression tends to be overestimated. We report the RMS error for all the temperatures, and for the maximum and the minimum temperatures. Table X is a listing of the average prediction error for the formation melting temperature (as defined before), the minimum and maximum melting temperature.
TABLE IX
0%
25%
25%
50%
50%
75%
75%
100%
c b
T A
T low
T high
T low
T high
T low
T high
T B
T min
T max
alloy
(° C.)
(° C.)
(° C.)
(° C.)
(° C.)
(° C.)
(° C.)
(° C.)
(° C.)
c b T min
(° C.)
c b T max
AgCd
951
830
855
630
710
450
530
321
321
1.00
981
0.00
AgMg
961
790
830
820
820
494
570
650
472
0.83
961
0.00
MoAg
2623
958
2310
958
2200
958
2075
951
951
1.00
2623
0.00
MoCd
2623
321
767
321
757
321
767
321
321
1.00
2623
0.00
MoPd
2623
1755
2270
1755
1850
1680
1710
1555
1700
0.54
2623
0.00
MoRh
2623
1940
2170
2020
2050
2015
2035
1963
1940
0.39
2623
0.00
MoRu
2623
2040
2180
1970
2040
2180
2210
2334
1955
0.42
2623
0.00
MoTc
2623
2135
2320
2027
2230
2080
2100
2204
2027
0.55
2623
0.00
NbMo
2459
2483
2515
2515
2560
2565
2595
2623
2469
0.00
2623
1.00
NbPd
2459
1380
2180
1520
1550
1625
1625
1555
1520
0.47
2469
0.00
NbRh
2469
1663
1860
1550
1560
1910
1940
1953
1502
0.45
2469
0.00
NbRu
2469
1930
1950
1942
1942
1360
1975
2334
1774
0.65
2469
0.00
PdAg
1555
1390
1445
1285
1330
1130
1170
961
961
1.00
1555
0.00
RhAg
1963
1900
951
1900
961
1900
961
961
961
1.00
1953
0.00
RhPd
1963
1860
1900
1730
1820
1620
1680
1555
1555
1.00
1963
0.00
RuPd
2334
1583
2100
1583
1980
1553
1800
1555
1555
1.00
2334
0.00
RuRh
2334
2240
2290
2110
2160
2040
2060
1963
1963
1.00
2334
0.00
StAl
1541
945
1140
1150
1300
655
1320
650
660
1.00
1541
0.00
TcPd
2155
1850
2100
1700
1900
1650
1680
1555
1555
1.00
2155
0.00
TcRh
2155
2120
2150
2100
2120
2050
2100
1953
1963
1.00
2155
0.00
TiAg
1670
1020
1530
1020
1455
1020
1330
961
961
1.00
1670
0.00
TiMo
1670
1810
1950
2030
2180
2310
2400
2623
1671
0.00
2623
1.00
TiPd
1670
1150
1280
1400
1400
1490
1530
1555
1120
0.32
1670
0.00
TiRh
1670
1300
1320
1940
1940
1750
1780
1963
1280
0.29
1963
1.00
TiRu
1670
1575
1610
2130
2130
1825
1860
2334
1575
0.25
2334
1.00
TiZr
1670
1560
1580
1550
1560
1690
1720
1855
1540
0.39
1855
1.00
YAg
1522
385
980
835
1160
900
940
961
799
0.88
1522
0.00
YMo
1522
1430
1780
1430
2080
1430
2380
2623
1430
0.10
2623
1.00
YNb
1522
1470
2000
1470
2400
1470
2400
2469
1470
0.06
2469
1.00
YPd
1522
907
907
1385
1440
1700
1700
1555
907
0.25
1700
0.75
YRh
1522
1200
1300
1500
1540
1470
1520
1953
1150
0.20
1963
1.00
YRu
1522
1250
1300
1350
1750
1840
1900
2334
1030
0.15
2334
1.00
YZr
1522
1360
1390
1360
1380
1350
1550
1855
1360
0.40
1855
1.00
ZrAg
1855
1190
1350
1136
1160
940
1120
961
940
0.97
1855
0.00
ZrMo
1855
1540
1700
1550
1600
1380
2220
2623
1550
0.45
2623
1.00
ZrNb
1855
1740
1750
1850
1930
2090
2220
2469
1740
0.21
2469
1.00
ZrPd
1855
1030
1030
1030
1600
1390
1780
1555
1030
0.25
1855
0.00
ZrRh
1855
1070
1130
1910
1910
1900
1930
1963
1070
0.23
1963
1.00
ZrRu
1855
1240
1500
2130
2130
1715
1780
2334
1240
0.21
2334
1.00
TABLE X
Lens-like systems predicted with lens-like systems
RMS c [T] = 12%
RMS c [T min ] = 19%
RMS c [T max ] = 14%
Non-Lens-like systems predicted with non-lens-like systems:
RMS c [T] = 12%
RMS c [T min ] = 15%
RMS c [T max ] = 18%
Lens-like system predicted with all the systems
RMS c [T] = 15%
RMS c [T min ] = 19%
RMS c [T max ] = 19%
Non-Lens-like system predicted with all the systems
RMS c [T] = 11%
RMS c [T min ] = 13%
RMS c [T max ] = 16%
All the systems predicted with all the systems
RMS c [T] = 12%
RMS c [T min ] = 15%
RMS c [T max ] = 17%
Data Mining: Organization of Methods
FIG. 10 is a high level flow diagram 1000 showing the relationships between reference system data 1010 , 1012 , new system data 1020 , 1022 , 1024 , and a data mining method 1030 according to principles of the invention. In one embodiment, the invention can be described with regard to the input data for the reference system (IDRS) 1010 , output data for the reference system (ODRS) 1012 , input data for new system (IDNS) 1020 , and output data for the new system (ODNS) 1022 , 1024 . An algorithm that learns, for example a neural network, seeks a correlation between IDRS and ODRS. The system then applies the correlation to the IDNS to predict unknown information for the new system (ODNS). In some embodiments, systematically stating the nature of this data makes clear the distinction between the inventive data mining methods and previous ones.
Data for the Reference System (DRS)
These are the data types which are used to build or discover a correlation. In some embodiments, these data can be referred to as a “training set” or “reference data.” One can distinguish Input DRS (IDRS) and Output DRS (ODRS). These sets can be distinct (e.g., their intersection is the null set) or they can overlap (e.g., their intersection is a set having at least one member). In one exemplary embodiment, involving Pauling files, the ODRS and IDRS are the same set and constitute the experimentally observed stable crystal structures as function of composition for a large number of alloys. In the PLS approach, these data are the computed energies of a set of structures, which are not limited to only the stable structures, in a series of reference alloys. For Pettifor maps, the IDRS are the ordinal numbers that represent elements in the Periodic Table (e.g., the Mendeleyev numbers of the elements) in an alloy and the ODRS is the crystal structure at a particular composition.
Inputs for the New System (IDNS)
This is the data that is available (or generated) for the new system and on which a prediction is based. Note that the kinds of data represented by an IDNS needs to be a subset of the kinds of data represented by the IDRS. For example, if the IDRS includes crystal structure data as a function of composition, temperature, and pressure, then the IDNS could be crystal structure data as a function of one or more of composition, temperature, and pressure. If the IDNS is not a subset of the IDRS, a correlation can not be built. For example, if the IDRS is structure data as a function of composition and temperature, while the IDNS is structure data as a function of composition and pressure, relationships that exist for the IDRS may not be informative for studying the IDNS.
Output Data Predicted for New System (ODNS)
The output data for the new system can be any type of information that is present in the ODRS. In some embodiments, in which there is overlap between the information present in the ODRS and the IDRS, an iterative method can be built. In the iterative method, some portion of the predicted data (output data) can be used as input for the next iteration. Note, the possibility of iteration when the input and output data sets include information of the same type applies to all of the techniques discussed herein.
Methods Used to Make the Prediction
The method is shown schematically in FIG. 10 . Different embodiments of the method will be presented as examples.
EXAMPLE 1
Predicting Structure Based Solely On First Principles Data
In this example, the IDRS and the ODRS represent calculated energies of structures at various compositions in a series of binary alloy systems. One can define at least one IDNS as the energy of at least one structure in a new alloy. For this example, the ODNS is calculated and includes a set of energies of all structures in the new alloy system. In such an embodiment, iteration is possible, since ODRS is a subset of IDRS.
EXAMPLE 2
Predicting Structures in a New System Based on the Knowledge That Some Structures are Present, and Given an Experimental Database of Stable Structures
In this embodiment, the IDRS and the ODRS represent a set of stable structures as a function of composition for all materials in the experimental database. In this example, the IDNS represents one or more known stable structures in a new system (e.g., a system that is of interest, or that is the subject of a technical investigation). The ODNS represents one or more candidate stable structures in the new system. Iteration is possible in this case in many ways. In one embodiment, one can use an “Expectation Maximization” algorithm wherein the calculated distribution is used to update the input data and the computation is iterated until convergence to within a desired error amount occurs. In another embodiment, one can use first principles computations to calculate one or more likely structures and add the result to the IDNS.
EXAMPLE 3
Predicting Melting Temperature from the Cohesive Energy of an Alloy
In this example, the IDRS represents at least one cohesive energy of at least one structure. In some embodiments, the IDRS includes a plurality of data for a series of structures. In this embodiment, the ODRS represents one or more melting points, one melting point corresponding to each structure in the IDRS. In this embodiment, the IDNS represents a cohesive energy of a new structure, and the ODNS represents a predicted melting point of the new structure. Because the information represented by the inputs (IDRS and IDNS) are not the same type of information as the outputs (ODRS and ODNS), that is, a cohesive energy and a melting point do not represent values for the same thing, no iteration is possible in this case. However, as more data appears in the IDRS and ODRS, e.g., new calculated information for a previously unknown structure is obtained, and is added to the IDRS and ODRS so as to augment the previous data contained therein, the precision of the computational procedure (that is, the data mining engine, or the algorithmic process for performing the calculation) can increase because the added data permits refinement of the computational procedure.
EXAMPLE 4
Prediction of Crystal Structure or Structure Descriptors
A crystal structure can be described in many ways. Examples of structural descriptors include: a prototype, for example a commonly used chemical name as structure descriptor such as NaCl; a Strukturbericht notation; a combination of space group, unit cell and coordinate data; a structure type; a Pauling symbol; and a lattice type. Most of these are complete descriptions, i.e. they characterize the structure uniquely. Structures can also be partially described, for example by structure descriptors: Coordination number, pair correlation function, space group, lattice type, short-range order parameter, one or more lattice parameters. These all describe a structure partially, but not completely.
We turn now to an example in which the goal is complete structure prediction (as for example by prototype). However, one can also predict a structure partially, by using various of the structure descriptors enumerated hereinabove. The general case for an ODNS is a generic property of the predicted phase/crystal structure, be it a full or partial structural descriptor, susceptibility, or bound on its stability.
Before presenting an example, we will indicate how a prior art predictor of structure can be understood in the present formalism. Consider a Pettifor map. A Pettifor map is constructed at a fixed composition (e.g. AB or A 2 B, or A 3 , etc.). The IDRS represents the Mendeleyev number of two or more elements in a known material at the composition of the Pettifor map, and the_ODRS represents the crystal structure of the known material. For the new system, the IDNS represents the Mendeleyev numbers of the elements present in the material of interest, and the_ODRS represents the predicted crystal structure of the material of interest at the composition of the Pettifor map. In such a system, no iteration is possible and in a Pettifor map of given composition, no information from other compositions (besides the trivial elemental ones) is used to improve the prediction. In general, for prior art systems that rely on structure maps, it appears that the following limiting attributes are common. The IDNS comprises elemental data, such as ionic size, electronegativity, pseudopotential radius, and electron per atom ratio, but the IDNS does not include or provide information about crystal structure stability. In general, the ODRS is the stable crystal structure at the composition for which one is trying to make the prediction (generally at a defined temperature, such as room temperature or 20° C.). No information about crystal structure stability is used at the composition of interest and at other compositions. In general, only information about known materials and structures is used. The inventors are unaware of any such system that uses computed ODRS. In general, the structure assigned in such a mapping analysis is by comparing the nearest chemical systems in the map, and deducing from their structures which is the most likely structure. No iteration of the output data or results is possible in such mapping systems.
In contradistinction to prior art mapping systems, the systems and methods of the invention provide IDRS and ODRS that contain crystal structure information from multiple compositions in a given data set. According to principles of the invention, one can build (or identify) correlations between information (such as crystal structure stability) across compositions, and relate it not only to information about the elements (as is the case for the previous schemes), but to information about the relative stability of different crystal structures, and/or the thermal behavior of crystal structures of specific compositions, such as phase transitions and/or stability of a given structure as a function of temperature.
Furthermore, in systems and methods of the invention, one can establish or identify correlations between a property of the structure of a new system (e.g., a property as ODNS that is a function of structure) and one or more properties (i.e., ODRS) of other compounds in the same alloy system (e.g., reference systems in the same alloy system). The systems and methods of the invention provide a general framework through which correlations (and anti-correlations) can be established and used. By comparison, what has been done thus far is a limiting case of the systems and methods of the invention, namely, the case where IDNS represents only element data. Furthermore, because in the systems and methods of the invention, there are cases where IDRS data is the same type as ODRS data, one can iterate and at each step improve the prediction in the inventive system. As another benefit, the systems and methods of the invention can mix computed stability data and experimentally obtained data.
Structure parameters include but are not limited to structure type (for example using a chemical compound descriptor such as NaCl cubic structure), Pearson symbol, Pauling symbol, space group, lattice type, order parameter, coordination number, and lattice parameters. Phase transitions can include but are not limited to transitions that occur with changes in temperature, transitions that occur with changes in pressure and changes that occur with changes in composition. Electronic, magnetic, photonic and thermodynamic properties include but are not limited to conductivity, mobility (such as mobility of electrical charge, of ions, and of features such as phonons), carrier concentration, energy gap (including electronic and photonic band gaps), effective mass, transition temperatures (such a Curie temperature, a semiconductor-to-metal transition temperature, a Neel temperature, a critical temperature for superconductivity), magnetic susceptibility, color, refractive index, permittivity, compressibility, bulk modulus, thermal expansion coefficient, elastic stiffness, hardness, specific heat capacity, density, enthalpy of formation, and entropy of formation.
Until now, the systems and methods of the invention have been used to study materials at low temperatures and pressures. It is believed that the systems and methods of the invention can be used to predict phase transitions. It is also believed that if high temperature and high pressure data are included in the reference data sets, it is possible to predict phase changes with temperature, pressure or composition.
Machine-readable storage media that can be used in the invention include electronic, magnetic and/or optical storage media, such as magnetic floppy disks and hard disks; a DVD drive, a CD drive that in some embodiments can employ DVD disks, any of CD-ROM disks (i.e., read-only optical storage disks), CD-R disks (i.e., write-once, read-many optical storage disks), and CD-RW disks (i.e., rewriteable optical storage disks); and electronic storage media, such as RAM, ROM, EPROM, Compact Flash cards, PCMCIA cards, or alternatively SD or SDIO memory; and the electronic components (e.g., floppy disk drive, DVD drive, CD/CD-R/CD-RW drive, or Compact Flash/PCMCIA/SD adapter) that accommodate and read from and/or write to the storage media. As is known to those of skill in the machine-readable storage media arts, new media and formats for data storage are continually being devised, and any convenient, commercially available storage medium and corresponding read/write device that may become available in the future is likely to be appropriate for use, especially if it provides any of a greater storage capacity, a higher access speed, a smaller size, and a lower cost per bit of stored information. Well known older machine-readable media are also available for use under certain conditions, such as punched paper tape or cards, magnetic recording on tape or wire, optical or magnetic reading of printed characters (e.g., OCR and magnetically encoded symbols) and machine-readable symbols such as one and two dimensional bar codes.
Many functions of electrical and electronic apparatus can be implemented in hardware (for example, hard-wired logic), in software (for example, logic encoded in a program operating on a general purpose processor), and in firmware (for example, logic encoded in a non-volatile memory that is invoked for operation on a processor as required). The present invention contemplates the substitution of one implementation of hardware, firmware and software for another implementation of the equivalent functionality using a different one of hardware, firmware and software. To the extent that an implementation can be represented mathematically by a transfer function, that is, a specified response is generated at an output terminal for a specific excitation applied to an input terminal of a “black box” exhibiting the transfer function, any implementation of the transfer function, including any combination of hardware, firmware and software implementations of portions or segments of the transfer function, is contemplated herein.
While the present invention has been particularly shown and described with reference to the structure and methods disclosed herein and as illustrated in the drawings, it is not confined to the details set forth and this invention is intended to cover any modifications and changes as may come within the scope and spirit of the following claims.
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Systems and methods for predicting features of materials of interest. Reference data are analyzed to deduce relationships between the input data sets and output data sets. Reference data includes measured values and/or computed values. The deduced relationships can be specified as equations, correspondences, and/or algorithmic processes that produce appropriate output data when suitable input data is used. In some instances, the output data set is a subset of the input data set, and computational results may be refined by optionally iterating the computational procedure. To deduce features of a new material of interest, a computed or measured input property of the material is provided to an equation, correspondence, or algorithmic procedure previously deduced, and an output is obtained. In some instances, the output is iteratively refined. In some instances, new features deduced for the material of interest are added to a database of input and output data for known materials.
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REFERENCE TO RELATED APPLICATION
This is a continuation-in-part application of Ser. No. 227,601, filed Feb. 18, 1972, and application Ser. No. 712,398, filed Mar. 12, 1968, Both applications are now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the dyeing of keratinous materials. More particularly, it relates to coloring compositions for producing a semi-permanent dyeing of hair for cosmetic purposes. The dyeing of the hair is accurately reproducible, nonstaining to the skin and is advantageously accomplished by directly applying the coloring composition of this invention to the hair at normal room temperature.
2. Description of the Prior Art
Coloring preparations for modifying or changing the natural hair color may be classed generally into the permanent colors and the temporary colors. In current practice permanent colors are oxidation dyes based on certain coal tar intermediates which develop color in the presence of an oxidizing agent such as hydrogen peroxide in an alkaline solution. The permanent colors are retained by the hair until the hair grows out, although the original shade may become altered as the result of frequent shampooing, perspiration, exposure to light, use of permanent waves or other chemical hair treatments.
The temporary colors are used to give color highlights to the hair, to correct yellowish streaks in gray hair, to blend in mixed gray hair and to brighten and intensify the natural hair color.
The temporary dyes are of several different types. There are acid dyes in conjunction with organic acids such as citric and tartaric, and sometimes with a surfactant. Another type is the cationic or basic dyes combined with buffering salts such as borates, citrates or phosphates. Still another type comprises the complex dyes which are formed by the interaction of acid dyes (including direct dyes) with cationic surfactants.
The dyes of all these types of temporary dyes impart color to the hair by way of forming a film on the hair surface. These films are of varying durability. Thus, the first-mentioned type, the acid dyes, can be completely removed by a single shampooing, while the second-mentioned type, the buffering cationic or basic dyes, usually last through a few shampooings.
In recent years, a demand has been created for hair colors of the temporary type--which do not require irritating oxidative dyes or high temperatures as is the case for some permanent colors--but which as well would provide a hair coloring with longer-lasting characteristics, in effect, a hair coloring which will withstand many shampoo treatments and will be semipermanent in its lasting properties. The present invention is directed towards fulfilling this need.
SUMMARY OF THE INVENTION
The principal object of this invention relates to the semi-permanent dyeing of keratinic fibers including human hair and furs at body and room temperatures, thereby preventing damage to the hair and the likelihood of toxic irritation which are associated with permanent type colors utilizing hydrogen peroxide or other oxidants in an alkaline solution while being non-staining to the skin of the user. The present invention may also be employed for dyeing either natural or synthetic polyamide fibers such as silk or animal bristles. As the dye compositions of the present invention are non-reactive, it is possible to obtain superior control over the final hair colors obtained. This is particularly so as the extent of absorption of a mixture of dyes from the coloring compositions disclosed herein is predictable and accurately reproducible giving strong level shades on normal hair, on hair which has been bleached, or on hair which has been permanent-waved.
The present invention is based upon the discovery that improved semi-permanent hair coloring compositions for dyeing at room temperature and which is non-staining to the skin of the user may be achieved through the use of an organic dye carrier in combination with an anionic surface active agent which co-assists the adsorption of the dye materials onto the outer surface of the keratinic fibers to be treated and thereafter to co-assist the penetration of the dye materials into the micropores of the fibers and in further combination with an alkoxylated lanolin or fatty alcohol to yield a composition which is non-staining to the skin of the user. Briefly stated, the hair coloring compositions of the present invention comprise a major amount of water, a premetalized dye soluble in a compatible organic dye carrier and capable of penetrating keratinic fibers, a compatible organic dye carrier for co-assisting the transfer of the dye into keratinic fibers, an anionic surface active agent and a stain retarding agent selected from alkoxylated lanolins and fatty alcohols. Preferred compatible organic dye carriers for the present invention include benzyl alcohol derivatives, alkyl phenones, cyclohexane compounds, n-nonylaldehyde, 2-phenoxyethanol, and 2-methyl-1-pentanol.
In addition to the basic essential ingredients in the coloring compositions of the present invention, namely a premetallized dye, a stain-retarding agent, a dye carrier and an anionic surfactant, it is preferable to include conventional components used in hair coloring preparations, such as a cellulose ether thickening agent, a lather-forming agent, a pH buffer and perfume for their usual and intended effect. Advantageously, the coloring compositions are buffered at a pH of from 4 to 6 although a pH of from 2 to 7 is suitable for the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
A preferred formulation for the coloring compositions of this invention is listed below in Table I. (The formula below is listed in terms of parts per hundred by weight.)
TABLE I______________________________________Premetallized dye 0.1 to 10Compatible dye carrier 1 to 10Stain inhibiting agent 0.1 to 5Anionic surfactant 0.01 to 5Cellulose ether about 1(thickener)pH buffer solution about 20Lather forming agent 1 to 10Perfume (in sufficient quantity)Distilled water make to 100______________________________________
Any of the wide range of non-toxic and non-irritating premetallized dyes are suitable for the present invention to produce a wide range of desired effects. They may be chromium and/or cobalt containing dyes and their chemistry is discussed in the Journal of The Society of Dyers and Colourists, 71, pp. 705-724 (Dec. 1955). They are available commercially under such tradenames as Irgalan, Cibalan, Vialon, Ortalan and Capracyl dyes. Examples of such dyes are listed in Table II in which they have been identified by tradename and corresponding Colour Index name.
TABLE II
Cibalan Brown 2 GL (Acid Brown 224)
Irgalan Navy Blue 5RL (Acid Blue 188)
Cibalan Brown TL (Acid Brown 21)
Cibalan Bordeaux EL (Acid Red 251)
Irgalan Dark Brown 5R (Acid Brown 48)
Cibalan Bordeaux 3BL (Acid Violet 70) Cibalan Violet RL (Acid Violet 68) )
Cibalan Blue 3GL (Acid Blue 171)
Cibalan Green GL (Acid Green 43)
Cibalan Brown BL (Acid Brown 19)
Cibalan Red Brown RL (Acid Brown 226)
Cibalan Black 2BL (No C.I. name and No. yet given)
Cibalan Black 2GL (No C.I. name and No. yet given)
Cibalan Grey BL (Acid Black 60)
Preferred compatible organic dye carriers for the present invention include benzyl alcohol derivatives, alkyl phenones, cyclohexane compounds, n-nonylaldehyde and 2-methyl-1-pentanol. The most effective dye carriers for the present invention are listed below in Table III.
TABLE III
Benzyl Alcohol Derivatives
A. Alkyl Substituted Benzyl Alcohol
α,α-dimethyl benzyl alcohol
α-propyl benzyl alcohol
Dl-αmethyl benzyl alcohol
B. Benzyloxyalkanols
2-Benzyloxyethanol
2-Benzyloxypropanol
2-Benzyoxybutanol
C. Esterified benzyl alcohol of C 1 -C 4 carboxylic acids
benzyl acetate
benzyl propionate
benzyl butyrate
Alkyl Phenones
acetophenone
2,4-dimethyl acetophenone
4-ethyl acetophenone
propiophenone
Cyclohexane Compounds
cyclohexanol
2-methyl cyclohexanol
3,5-dimethyl cyclohexanone
4-methyl cychlohexanone
Equally effective are 2-phenoxyethanol, n-nonylaldehyde and 2-methyl-1-pentanol.
Any of the well-known anionic surface active agents are suitable for the present invention and such agents are listed in such sources as the annual McCutcheon's catalog "Detergents and Emulsifiers Annual." Some specific examples are sodium lauryl sulfate, triethanolamine lauryl sulfate and ethoxylated fatty alcohol sulfates. There is no criticality to the anionic surface active agent to be used.
The coloring compositions of the present invention are rendered non-staining to the skin of the user by a stain-inhibiting agent selected from polyoxyalkylene lanolins, lanolin alcohols, lanolin fatty esters, and fatty alcohols. The polyoxyalkylene lanolins should have an average degree of alkoxylation of from about 10 to 80. Examples are polyoxyethylene lanolins which are ethoxylated polymers of lanolin in which the average degree of ethoxylation ranges from 10 to 80 moles of ethylene oxide. The fatty alcohols are C 8 -C 20 fatty alcohols with C 12 -C 18 fatty alcohols being preferred. Examples of such alcohols are lauryl, myristyl, palmityl and stearyl alcohols. These agents may be used alone or in combination.
As to the cellulose ether thickening agent, any commercially available cellulose ether can be used. Examples are hydroxyethyl cellulose, carboxymethyl cellulose, hydroxypropyl cellulose, and sodium carboxymethyl cellulose.
The lather-forming agent used is preferably a mixture of lauryl diethanolamide and a dicarboxylic sodium salt derivative or coconut oil. Any lather-forming compound or composition conventionally used in hair coloring compositions can be used in the instant composition.
The pH buffers used are preferably the known phosphate, citrate and phthalate buffers suitable for the pH desired. Examples are sodium citrate; potassium acid phosphate-disodium phosphate; potassium acid phthalate-sodium hydroxide; potassium acid phosphate-sodium hydroxide; and citric acid-disodium phosphate.
The following examples illustrate the formulation and use of certain specific hair coloring compositions of the present invention. All of these compositions have the advantage of producing predictable and accurately reproducible coloring of the hair and have the important property of not staining the user's skin.
EXAMPLE 1
A hair coloring composition is formulated utilizing the constituents listed in Table IV below and the pH of the solution is adjusted by a suitable buffer to 5.0. The composition is applied to dry or wet, living human hair and left for fifteen minutes. Thereafter, the composition is shampooed out utilizing conventional soaps and the hair is found to be colored a medium brown while an examination of the scalp shows no staining. (The formula listed below is in terms of parts per hundred by weight).
TABLE IV______________________________________2-Benzyloxyethanol 4.0Cibalan brown TL (Acid Brown 21) 1.0Triethanolamine lauryl sulfate 1.0Buffer Solution 20.0Carboxymethyl cellulose 1.0Lauryl alcohol 1.0Perfume (in sufficient quantity)Distilled water make to 100______________________________________
EXAMPLE 2
A hair coloring composition is formulated utilizing the consituents listed below in Table V and the pH is adjusted to 4.0. The composition is applied to dry or wet human hair and left for 15 minutes. After the coloring composition is shampooed, the hair is found to be colored a bordeaux shade. The skin of the user is not stained. (The formula listed below is in terms of parts per hundred by weight).
TABLE V______________________________________α,α-Dimethylbenzyl alcohol 1.0Cibalan Bordeaux EL (Acid Red 251) 0.5Sodium laurylsulfate 0.1Hydroxyethyl cellulose 1.0Myristyl alcohol 1.0Buffer Solution 20.0Glycerin 5.0Perfume (in sufficient quantity)Distilled water make to 100______________________________________
EXAMPLE 3
A hair coloring composition is formulated from the constituents listed below in Table VI and the pH is adjusted to 6.0. The composition is applied to dry or wet human hair in the conventional manner and produces a dark brown coloring. The skin of the user is not stained. (The formula listed below is in terms of parts per hundred by weight).
TABLE VI______________________________________Lanolin alcohol 2.0DL-α-Methyl benzyl alcohol 2.0Dicarboxylic coconut derivative 0.5sodium saltPolyoxyethylene (40) lanolins 0.3Lauryl diethanolamide 0.3Triethanolamine lauryl sulfate 2.0Irgalan Dark Brown 5R (Acid Brown 48) 1.0Buffer solution 20.0Hydroxyethyl cellulose 1.0Perfume (in sufficient quantity)Distilled water make to 100______________________________________
EXAMPLE 4
A hair coloring composition is formulated as indicated below in Table VII and the pH adjusted to 6.0. After applying the hair coloring composition to dry or wet human hair in the conventional manner, the hair is found to have been colored a dark brown. The skin of the user is not stained. (The formula listed below is in terms of parts per hundred by weight).
TABLE VII______________________________________Lauryl alcohol 2.0Benzyl acetate 2.0Dicarboxylic coconut derivative 0.5sodium saltPolyoxy ethylene lanolin (Lanogel 41) 0.3Lauryl diethanolamide 0.3Triethanolamine lauryl sulfate 2.0Irgalan dark brown 5R (Acid 1.0Brown 48)Hydroxyethyl cellulose 2.5Buffer solution 20.0Perfume (in sufficient quantity)Distilled water make to 100______________________________________
Although the above specification describes preferred hair coloring compositions and the method of making them in accordance with the teachings of the present invention, it is to be understood that various changes may be made without departing from the scope of the invention as set forth in the following claims.
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A coloring composition for dyeing keratinous material comprising water, an organic dye carrier, a premetallized dye soluble in the carrier, a stain-inhibiting agent and an anionic surface active agent. The dyes are premetallized dyes and the composition includes dye carriers, anionic surface active agents, and stain inhibiting agents in an aqueous solution. The composition is effective as a semi-permanent hair dye that can be applied to hair without staining the skin of the user.
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RELATED APPLICATIONS
This application is a continuation application of U.S. patent application Ser. No. 12/442,347, filed on Feb. 16, 2010, which application is a U.S. National Stage Filing under 35 U.S.C. 371 from International Application No. PCT/US2007/020472, filed on Sep. 21, 2007, and published as WO 2008/036395 A1 on Mar. 27, 2008; which application claims the benefit of priority to U.S. Provisional Patent Application Ser. No. 60/826,709, filed on Sep. 22, 2006, which applications and publication are incorporated herein by reference in their entirety.
FIELD
The subject matter relates to underground formation investigation, and more particularly, apparatus and methods for formation testing and fluid sampling within a borehole.
BACKGROUND
The oil and gas industry typically conducts comprehensive evaluation of underground hydrocarbon reservoirs prior to their development. Formation evaluation procedures generally involve collection of formation fluid samples for analysis of their hydrocarbon content, estimation of the formation permeability and directional uniformity, determination of the formation fluid pressure, and many others. Measurements of such parameters of the geological formation are typically performed using many devices including downhole formation testing tools.
During drilling of a wellbore, a drilling fluid (“mud”) is used to facilitate the drilling process and to maintain a pressure in the wellbore greater than the fluid pressure in the formations surrounding the wellbore. This is particularly important when drilling into formations where the pressure is abnormally high: if the fluid pressure in the borehole drops below the formation pressure, there is a risk of blowout of the well. As a result of this pressure difference, the drilling fluid penetrates into or invades the formations for varying radial depths (referred to generally as invaded zones) depending upon the types of formation and drilling fluid used. The formation testing tools retrieve formation fluids from the desired formations or zones of interest, test the retrieved fluids to ensure that the retrieved fluid is substantially free of mud filtrates, and collect such fluids in one or more chambers associated with the tool. The collected fluids are brought to the surface and analyzed to determine properties of such fluids and to determine the condition of the zones or formations from where such fluids have been collected.
One feature that all such testers have in common is a fluid sampling probe. This may consist of a durable rubber pad that is mechanically pressed against the rock formation adjacent the borehole, the pad being pressed hard enough to form a hydraulic seal. Through the pad is extended one end of a metal tube that also makes contact with the formation. This tube is connected to a sample chamber that, in turn, is connected to a pump that operates to tower the pressure at the attached probe. When the pressure in the probe is lowered below the pressure of the formation fluids, the formation fluids are drawn through the probe into the well bore to flush the invaded fluids prior to sampling. In some prior art devices, a fluid identification sensor determines when the fluid from the probe consists substantially of formation fluids; then a system of valves, tubes, sample chambers, and pumps makes it possible to recover one or more fluid samples that can be retrieved and analyzed when the sampling device is recovered from the borehole.
It is important that only uncontaminated fluids are collected, in the same condition in which they exist in the formations. Often the retrieved fluids are contaminated by drilling fluids. This may happen as a result of a poor seal between the sampling pad and the borehole wall, allowing borehole fluid to seep into the probe. The mudcake formed by the drilling fluids may allow some mud filtrate to continue to invade and seep around the pad. Even when there is an effective seal, borehole fluid (or some components of the borehole fluid) may “invade” the formation, particularly if it is a porous formation, and be drawn into the sampling probe along with connate formation fluids.
Additional problems arise in Drilling Early Evaluation Systems (EES) where fluid sampling is carried out very shortly after drilling the formation with a bit. Inflatable packers or pads cannot be used in such a system because they are easily damaged in the drilling environment. In addition, when the packers are extended to isolate the zone of interest, they completely fill the annulus between the drilling equipment and the wellbore and prevent circulation during testing.
There is a need for an apparatus that reduces the leakage of borehole fluid into the sampling probe, and also reduces the amount of borehole fluid contaminating the fluid being withdrawn from the formation by the probe. Additionally, there is a need for an apparatus that reduces the time spent on sampling and flushing of contaminated samples.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates a system for testing and drilling operations as constructed in accordance with at least one embodiment.
FIG. 2 illustrates a wireline system for drilling operations as constructed in accordance with at least one embodiment.
FIG. 3 illustrates a probe as constructed in accordance with at least one embodiment.
FIG. 4 illustrates a probe as constructed in accordance with at least one embodiment.
FIG. 5 illustrates a probe as constructed in accordance with at least one embodiment.
FIG. 6 illustrates a side view of a probe as constructed in accordance with at least one embodiment.
FIG. 7 illustrates a side view of a probe as constructed in accordance with at least one embodiment.
FIG. 8 illustrates a side view of a probe as constructed in accordance with at least one embodiment.
FIGS. 9-16 illustrates an example of a retractable wiper for a probe as constructed in accordance with at least one embodiment.
DESCRIPTION
In the following description of some embodiments of the present invention, reference is made to the accompanying drawings which form a part hereof, and in which are shown, by way of illustration, specific embodiments of the present invention which may be practiced. In the drawings, like numerals describe substantially similar components throughout the several views. These embodiments are described in sufficient detail to enable those skilled in the art to practice the present invention. Other embodiments may be utilized and structural, logical, and electrical changes may be made without departing from the scope of the present invention. The following detailed description is not to be taken in a limiting sense, and the scope of the present invention is defined only by the appended claims, along with the full scope of equivalents to which such claims are entitled.
FIG. 1 illustrates a system 100 for drilling operations. It should be noted that the system 100 can also include a system for pumping operations, or other operations. The system 100 includes a drilling rig 102 located at a surface 104 of a well. The drilling rig 102 provides support for a down hole apparatus, including a drill string 108 . The drill string 108 penetrates a rotary table 110 for drilling a borehole 112 through subsurface formations 114 . The drill string 108 includes a Kelly 116 (in the upper portion), a drill pipe 118 and a bottom hole assembly 120 (located at the lower portion of the drill pipe 118 ). The bottom hole assembly 120 may include drill collars 122 , a downhole tool 124 and a drill bit 126 . The downhole tool 124 may be any of a number of different types of tools including measurement-while-drilling (MWD) tools, logging-while-drilling (LWD) tools, etc.
During drilling operations, the drill string 108 (including the Kelly 116 , the drill pipe 118 and the bottom hole assembly 120 ) may be rotated by the rotary table 110 . In addition or alternative to such rotation, the bottom hole assembly 120 may also be rotated by a motor that is downhole. The drill collars 122 may be used to add weight to the drill bit 126 . The drill collars 122 also optionally stiffen the bottom hole assembly 120 allowing the bottom hole assembly 120 to transfer the weight to the drill bit 126 . The weight provided by the drill collars 122 also assists the drill bit 126 in the penetration of the surface 104 and the subsurface formations 114 .
During drilling operations, a mud pump 132 optionally pumps drilling fluid, for example, drilling mud, from a mud pit 134 through a hose 136 into the drill pipe 118 down to the drill bit 126 . The drilling fluid can flow out from the drill bit 126 and return back to the surface through an annular area 140 between the drill pipe 118 and the sides of the borehole 112 . The drilling fluid may then be returned to the mud pit 134 , for example via pipe 137 , and the fluid is filtered.
The downhole tool 124 may include one to a number of different sensors 145 , which monitor different downhole parameters and generate data that is stored within one or more different storage mediums within the downhole tool 124 . The type of downhole tool 124 and the type of sensors 145 thereon may be dependent on the type of downhole parameters being measured. Such parameters may include the downhole temperature and pressure, the various characteristics of the subsurface formations (such as resistivity, radiation, density, porosity, etc.), the characteristics of the borehole (e.g., size, shape, etc.), etc.
The downhole tool 124 further includes a power source 149 , such as a battery or generator. A generator could be powered either hydraulically or by the rotary power of the drill string. The downhole tool 124 includes a formation testing tool 150 , which can be powered by power source 149 . In an embodiment, the formation testing tool 150 is mounted on a drill collar 122 . The formation testing tool 150 includes a probe that engages the wall of the borehole 112 and extracts a sample of the fluid in the adjacent formation via a flow line. The probe includes one or more inner channels and one or more outer channels, where the one or more outer channels captures more contaminated fluid than the one or more inner channels. As will be described later in greater detail, the probe samples the formation and, in an option, inserts a fluid sample in a container 155 . In an option, the tool 150 injects the carrier 155 into the return mud stream that is flowing intermediate the borehole wall 112 and the drill string 108 , shown as drill collars 122 in FIG. 1 . The container(s) 155 flow in the return mud stream to the surface and to mud pit or reservoir 134 . A carrier extraction unit 160 is provided in the reservoir 134 , in an embodiment. The carrier extraction unit 160 removes the carrier(s) 155 from the drilling mud.
FIG. 1 further illustrates an embodiment of a wireline system 170 that includes a downhole tool body 171 coupled to a base 176 by a logging cable 174 . The logging cable 174 may include, but is not limited to, a wireline (multiple power and communication lines), a mono-cable (a single conductor), and a slick-line (no conductors for power or communications). The base 176 is positioned above ground and optionally includes support devices, communication devices, and computing devices. The tool body 171 houses a formation testing tool 150 that acquires samples from the formation. In an embodiment, the power source 149 is positioned in the tool body 171 to provide power to the formation testing tool 150 . The tool body 171 may further include additional testing equipment 172 . In operation, a wireline system 170 is typically sent downhole after the completion of a portion of the drilling. More specifically, the drill string 108 creates a borehole 112 . The drill string is removed and the wireline system 170 is inserted into the borehole 112 .
FIG. 2 illustrates the formation testing tool 150 in greater detail. As mentioned above, the formation testing tool 150 can be included on the wireline system 170 or a drilling system, for example. It should be noted the formation testing tool 150 can be included on other tools, including, but not limited to tools that lower themselves into the borehole. In FIG. 2 , an example of the wireline system is shown with formation testing tool 150 .
A portion of a borehole 201 is shown in a subterranean formation 207 . The borehole wall is covered by a mudcake 205 . The formation tester body 171 is connected to a wireline system 170 leading from a rig at the surface ( FIG. 1 ). The formation tester body 171 is provided with a mechanism, denoted by 210 , to clamp the tester body at a fixed position in the borehole. In an option, the clamping mechanism 210 is at the same depth as a probe 152 . Other mechanisms for engaging the probe 152 with the borehole include, but are not limited to inflatable packers.
In an example, a clamping mechanism 210 and a fluid sampling pad 213 are extended and mechanically pressed against the borehole wall. The fluid sampling pad 213 includes a probe 152 that has one or more outer channel 156 , and one or more inner channel 154 . The inner channel(s) 15 is disposed within at least a portion of the outer channel(s) 156 . In an option, the inner channel(s) 154 is extended from the center of the pad, through the mud cake 205 , and pressed into contact with the formation. For instance, the inner channel(s) 156 is connected by a hydraulic flow line 223 a to an inner channel sample chamber 227 a . In another option, the fluid sample pad 213 is extended via extendable members 211 ( FIGS. 6 and 7 ), and the inner and outer channels 154 , 156 can contact the formation. In an option, flow lines 223 a , 223 b for the inner and/or outer channels 154 , 156 extend through the extendable members 211 , and to their respective channels. In a further option, the probe 152 is an articulating probe, where the probe can hinge at one or more locations 184 ( FIG. 8 ) to contact the surface of a formation and borehole more readily.
The outer channel(s) 156 has one or more openings 158 ( FIG. 3 ) therealong, the openings being hydraulic connected with the formation thru the channel. Optionally the outer channel(s) can be directly contacting the formation. All of the openings can be connected to one or more hydraulic lines with in the body of the tool. In an option, the outer channel(s) 154 is connected by its own hydraulic flow line, 223 b , to an outer channel sample chamber, 227 b . Because the flow line 223 a of the inner channel(s) 154 and the flow line 223 b of the outer channel(s) 156 are separate, the fluid flowing into the outer channel(s) 156 does not mix with the fluid flowing into the inner channel(s) 154 . The outer channel(s) can 156 isolate the flow into the inner channel(s) 154 from the borehole beyond the pad 213 . In a further option, the inner channel flow line 223 a and/or the outer channel flow line 223 b extend through extendable members 204 ( FIGS. 6 and 7 ).
The hydraulic flow lines 223 a and 223 b are optionally provided with pressure transducers 211 a and 211 b . In an option, the pressure maintained in the outer channel flowline 223 b is the same as, or slightly less than, the pressure in the inner channel flowline 223 a . In another option, the pressure ratio maintained in the inner channel flowline 223 a to the outer channel flowline 223 b is about 2:1 to 1:2. In another option, the flow rates of the inner channel(s) 154 and the outer channel(s) 156 are regulated. For example, the flow rate ration of the inner channel(s) 154 to the outer channel(s) 156 is about 2:1 to 1:2. With the configuration of the pad 213 and the outer channel(s) 156 , contaminated borehole fluid that flows around the edges of the pad 213 is drawn into the outer channel(s) 156 , and diverted from entry into the inner channel(s) 154 .
The flow lines 223 a and 223 b are optionally provided with pumps 221 a and 221 b , or other devices for flowing fluid within the flow lines. The pumps 221 a and 221 b are operated long enough to substantially deplete the invaded zone in the vicinity of the pad 213 and to establish an equilibrium condition in which the fluid flowing into the inner channel(s) 154 is substantially free of contaminating borehole filtrate.
The flow lines 223 a and 223 b are also provided with fluid identification sensors, 219 a and 219 b . This makes it possible to compare the composition of the fluid in the inner channel flowline 223 a with the fluid in the outer channel flowline 223 b . During initial phases of operation, the composition of the two fluid samples will be the same; typically, both will be contaminated by the borehole fluid. These initial samples are discarded. As sampling proceeds, if the borehole fluid continues to flow from the borehole towards the inner channel(s) 154 , the contaminated fluid is drawn into the outer channel(s) 156 . Pumps 221 a and 221 b discharge the sampled fluid into the borehole. At some time, an equilibrium condition is reached in which contaminated fluid is drawn into the outer channel(s) 156 and uncontaminated fluid is drawn into the inner channel(s) 154 . The fluid identification sensors 219 a and 219 b are used to determine when this equilibrium condition has been reached. At this point, the fluid in the inner channel flowline is free or nearly free of contamination by borehole fluids. Valve 225 a is opened, allowing the fluid in the inner channel flowline 223 a to be collected in the inner channel sample chamber 227 a . Similarly, by opening valve 225 b , the fluid in the outer channel flowline 223 b is collected in the outer channel sample chamber 227 b . Alternatively, the fluid gathered in the outer channel(s) can be pumped to the borehole while the fluid in the inner channel flow line 223 a is directed to the inner channel sample chamber 227 a . Sensors that identify the composition of fluid in a flowline can also be provided, in an option.
FIGS. 3-5 illustrate additional variations for the probe 152 . The probe 152 is defined by a height 180 and a width 182 . In an option, the probe has an elongate shape and the height 180 is greater than the width 182 . This allows for the probe 152 to contact a greater number of laminates. In another option, the probe 152 has an overall oval shape.
As discussed above, the probe 152 includes inner and outer channels 154 , 156 , and the inner and outer channels 145 , 156 include a number of openings 158 or ports therein, where fluid flows through the openings 158 . The number of flow ports, in an option, in the outer channel(s) 156 is different than in the inner channel(s) 154 . In an option, the outer channels 156 have an overall oval, elongate shape and/or encircle with inner channel(s) 154 . While an elongate or oval shape are discussed, it should be noted other shapes for the probe or outer channels can be used. Furthermore, the area of the outer channel(s) 156 relative to the area of the inner channel(s) 154 can be varied, for example, as seen in FIGS. 3 and 4 . In another option, the outer channel(s) 156 do not completely encircle the inner channel(s) 154 , as shown in FIG. 5 . For example, the outer channel(s) 156 are disposed on one or more sides of the inner channel(s) 154 .
In a further option, the probe 152 includes an outer sealing member such as a seal 162 that encircles the outer channel(s) 156 , as shown in FIG. 3 . In further option, the probe 152 includes a seal 164 disposed between the outer channel(s) 156 and the inner channel(s) 154 , where the seal 164 is optionally retractable within the probe 152 . The seals 162 , 164 seal against the bore hole wall to enclose a contact surface therein. The seals can be made of elastomeric material, such as rubber, compatible with the well fluids and the physical and chemical conditions expected to be encountered in an underground formation.
The probe 152 can be operated, cleansed, or kept cleansed in a number of manners. For example, the probe 152 includes one or more screens 166 over the openings 158 . In an option, the one or more screens 166 are retractable to promote flow. Although only one screen 166 is shown in FIG. 3 , the screens 166 can be disposed over one or more of the openings 158 for the inner channel(s) 154 and/or the outer channel(s) 156 . In another option, the probe further includes at least one wiper that excludes or assists in excluding mud entry into the inner or outer channels.
In another example, fluid can be pumped through the probe 152 in various manners, such as out of the inner and/or outer channels 154 , 156 or into the inner and/or outer channels 145 , 156 . For instance, fluid is pumped through the probe 152 clearing the inner channel(s) 154 including pumping fluid out of the inner channel(s) 154 while optionally pumping into the outer channel(s) 156 . In a further option, fluid is pumped through the probe 152 clearing the outer channel(s) 156 including pumping fluid out of the outer channel(s) 156 while optionally pumping into the inner channel(s) 154 . In another option, fluid pump through the probe 152 is a selected fluid, such as a fluid that is capable of dissolving material that can clog formation pores near the probe. The fluid can be stored in a collection chamber that can be prefilled, or empty.
In yet another option, mud cake can be displaced, including removed, adjacent the seals, the inner channel member, or the outer channel member. For example, a wiper assembly as shown in FIG. 9-16 can be included with the above-discussed probe 152 . The wiper assembly includes a retractable wiper. The wiper can be used to remove or exclude mud cake from the probe as the pad sets.
Advantageously, the formation samples with low levels of contamination can be collected more quickly using the formation tester. Furthermore, the probe can be self cleaning without having to remove the probe from the borehole. This can increase the efficiency of the pumping or drilling operations. Furthermore, the probe allows for a thin layer or fracture to be identified because the probe can capture a layer or fracture by spanning vertically along the well bore.
Reference in the specification to “an option,” “an embodiment,” “one embodiment,” “some embodiments,” or “other embodiments” means that a particular feature, structure, or characteristic described in connection with the options or embodiments is included in at least some embodiments, but not necessarily all embodiments, of the invention. The various appearances of “an embodiment,” “one embodiment,” or “some embodiments” are not necessarily all referring to the same embodiments.
Although specific embodiments have been described and illustrated herein, it will be appreciated by those skilled in the art, having the benefit of the present disclosure, that any arrangement which is intended to achieve the same purpose may be substituted for a specific embodiment shown. This application is intended to cover any adaptations or variations of the present invention. Therefore, it is intended that this invention be limited only by the claims and the equivalents thereof.
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Apparatus and methods for downhole formation testing including use of a probe having inner and outer channels adapted to collect or inject injecting fluids from or to a formation accessed by a borehole. The probe straddles one or more layers in laminated or fractured formations and uses the inner channels to collect fluid.
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RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application Ser. No. 60/046,015 filed May 9, 1997.
TECHNICAL FIELD OF THE INVENTION
The present invention relates to highway guardrail systems having a guardrail mounted on posts, and more particularly, to guardrail end treatments designed to meet applicable federal and state safety standards including but not limited to crash worthiness requirements.
BACKGROUND OF THE INVENTION
Along most highways there are hazards which present substantial danger to drivers and passengers of vehicles if the vehicles leave the highway. To prevent accidents from a vehicle leaving a highway, guardrail systems are often provided along the side of the highway. Experience has shown that guardrails should be installed such that the end of a guardrail facing oncoming traffic does not present another hazard more dangerous than the original hazard requiring installation of the associated guardrail systems. Early guardrail systems often had no protection at the end facing oncoming traffic. Sometimes impacting vehicles became impaled on the end of the guardrail causing extensive damage to the vehicle and severe injury to the driver and/or passengers. In some reported cases, the guardrail penetrated directly into the passenger's compartment of the vehicle fatally injuring the driver and passengers.
Various highway guardrail systems and guardrail end treatments have been developed to minimize the consequences resulting from a head-on impact between a vehicle and the extreme end of the associated guardrail. One example of such end treatments includes tapering the ends of the associated guardrail into the ground to eliminate potential impact with the extreme end of the guardrail. Other types of end treatments include breakaway cable terminals (BCT), vehicle attenuating terminals (VAT), the SENTRE end treatment, and breakaway end terminals (BET).
It is desirable for an end terminal assembly installed at one end of a guardrail facing oncoming traffic to attenuate any head-on impact with the end of the guardrail and to provide an effective anchor to redirect a vehicle back onto the associated roadway after a rail face impact with the guardrail downstream from the end terminal assembly. Examples of such end treatments are shown in U.S. Pat. No. 4,928,928 entitled Guardrail Extruder Terminal, and U.S. Pat. No. 5,078,366 entitled Guardrail Extruder Terminal.
A SENTRE end treatment often includes a series of breakaway steel guardrail support posts and frangible plastic containers filled with sandbags. An impacting vehicle is decelerated as the guardrail support posts release or shear and the plastic containers and sandbags are compacted. A cable is often included to guide an impacting vehicle away from the associated guardrail.
A head-on collision with a guardrail support post located at the end of a guardrail system may result in vaulting the impacting vehicle. Therefore, guardrail end treatments often include one or more breakaway support posts which will yield or shear upon impact by a vehicle. Examples of previously available breakaway posts are shown in U.S. Pat. No. 4,784,515 entitled Collapsible Highway Barrier and U.S. Pat. No. 4,607,824 entitled Guardrail End Terminal. Posts such as shown in the '515 and the '824 Patents include a slip base with a top plate and a bottom plate which are designed to not yield upon lateral impact. When sufficient axial impact force is applied to the upper portion of the associated post, the top plate and the bottom plate will slide relative to each other. If a vehicle contacts the upper part of the post, the associated impact forces tend to produce a bending moment which may reduce or eliminate any slipping of the top plate relative to the bottom plate. Also, improper installation of the top plate relative to the bottom plate, such as over tightening of the associated mechanical fasteners, may prevent proper functioning of the slip base. A breakaway support post is also shown in U.S. Pat. No. 5,503,495 entitled Thrie-Beam Terminal with Breakaway Post Cable Release.
Wooden breakaway support posts are frequently used to releasably anchor guardrail end treatments and portions of the associated guardrail. Such wooden breakaway support posts, when properly installed, generally perform satisfactorily to minimize damage to an impacting vehicle during either a rail face impact or a head-on impact. However, impact of a vehicle with a wooden breakaway support post may often result in substantial damage to the adjacent soil. Removing portions of a broken wooden post from the soil is often both time consuming and further damages the soil. Therefore, wooden breakaway support posts are often installed in hollow metal tubes, sometimes referred to as foundation sleeves, and/or concrete foundations. For some applications, one or more soil plates may be attached to each metal sleeve to further improve the breakaway characteristics of the associated wooden post. Such metal sleeves and/or concrete foundations are relatively expensive and time consuming to install.
Light poles, sign posts or similar items are often installed next to a roadway with a breakable or releasable connection. For some applications, a cement foundation may be provided adjacent to the roadway with three or more bolts projecting from the foundation around the circumference of the pole. Various types of frangible or breakable connections may be formed between the bolts and portions of the light pole or sign post.
SUMMARY OF THE INVENTION
In accordance with teachings of the present invention, various shortcomings of previous guardrail support posts associated with highway guardrail end treatments have been addressed. The present invention provides a breakaway support post which will buckle or yield during head-on impact by a vehicle at or near the extreme end of an associated guardrail to minimize damage to the vehicle and provide sufficient strength to direct a vehicle back onto an associated roadway during a rail face impact with the guardrail downstream from the guardrail end treatment. The use of breakaway support posts incorporating teachings of the present invention substantially reduces the time and cost associated with initial installation of a guardrail end treatment and repair of the guardrail end treatment following impact by a motor vehicle.
One aspect of the present invention includes providing a breakaway support post having one or more slots formed in the support post to allow the support post to buckle or yield in response to forces applied to the support post in a first direction by an impacting vehicle without causing excessive damage to the vehicle. The orientation and location of the slots are selected to allow the support post to effectively anchor the guardrail to direct an impacting vehicle back onto an adjacent roadway in response to forces applied to the support post in a second direction during a downstream rail face impact. For some applications, one or more plates may be attached to the breakaway support post and inserted into the soil to provide additional support during a rail face impact with the associated guardrail and to provide more reliable buckling or yielding of the breakaway support post during a head-on impact with one end of the associated guardrail. Alternatively, the length of the portion of the breakaway support post inserted into the soil may be increased to enhance these same characteristics. For some applications, the breakaway support post may have a typical I-beam cross section with slots formed in one or more flange portions of the I-beam. Alternatively, the breakaway support post may have a hollow, rectangular or square cross section with slots formed in one or more sides of the post in accordance with teachings of the present invention.
Another aspect of the present invention includes providing a breakaway support post having a first portion or an upper section and a second portion or a lower section with the first portion rotatably coupled with the second portion. A pivot pin or other suitable type of rotatable coupling preferably connects adjacent ends of the first portion and the second portion to allow rotation of the first portion relative to the second portion. The pivot pin is preferably oriented during installation of the associate breakaway support post to allow rotation of the first portion when force is applied thereto in one direction and to block rotation of the first portion when force is applied thereto in a second direction. A shear pin or other suitable releasing mechanism may be provided to releasably couple the first portion and the second portion aligned longitudinally with each other. The shear pin and pivot pin are preferably oriented such that during a head-on impact with the end of the associated guardrail facing oncoming traffic, the shear pin will fail and allow the upper section to rotate relative to the lower section and thus minimize damage to the impacting vehicle. For some applications, a release bar or push bar may be attached to the lower section to assist with disengagement of the upper section from the lower section during such rotation of the upper section. During a rail face impact with the associated guardrail, the same orientation of the shear pin and the pivot pin prevents the upper section from rotating relative to the lower section. Thus, the breakaway support post will buckle or yield during a head-on impact to minimize damage to an impacting vehicle and will remain intact to redirect an impacting vehicle back onto the associated roadway after a rail face impact.
Technical advantages of the present invention include providing breakaway support posts which are easier to initially install and to repair as compared to wooden breakaway support posts. Major portions of each breakaway support post may be fabricated from standard, commercially available steel I-beams using conventional metal bending and stamping techniques in accordance with teachings of the present invention. One or more metal soil plates may be attached to each breakaway support post to further enhance desired characteristics of yielding or buckling during head-on impact with one end of an associated guardrail to minimize damage to an impacting vehicle and to securely anchor the associated guardrail to redirect an impacting vehicle back onto the adjacent roadway after a rail face impact. Breakaway support posts incorporating teachings of the present invention may be used with a wide variety of guardrail end treatments having various types of energy absorbing assemblies located at or near the end of the associated guardrail facing oncoming traffic. For many applications, breakaway support posts may be satisfactorily installed adjacent to the edge of a roadway without the use of steel foundation tubes and/or concrete foundations typically associated with installing wooden breakaway support posts and other types of breakaway support posts.
A further aspect of the present invention includes providing guardrail support posts having a first portion or upper section attached or coupled, at least in part, by a frangible connection, to a second portion or lower section. The support post and frangible connection may be oriented in accordance with teachings of the present invention to resist impact by a motor vehicle from one direction (strong direction), and to yield to impact by a motor vehicle from another direction (weak direction). Preferably, the frangible connection allows the upper portion of the post to deflect slightly and then break off of the lower portion, thus minimizing lifting of the impacting vehicle into the air.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the present invention, and the advantages thereof, reference is now made to the following written description taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a schematic drawing showing an isometric view with portions broken away of a highway guardrail system having a breakaway support post with a guardrail mounted thereon in accordance with one embodiment of the present invention;
FIG. 2 is a schematic drawing in elevation with portions broken away showing a side view of the highway guardrail system of FIG. 1 ;
FIG. 3 is a schematic drawing in section of the breakaway support post taken along lines 3 - 3 of FIG. 2 ;
FIG. 4 is a schematic drawing showing an isometric view with portions broken away of a highway guardrail system having a breakaway support post with a guardrail mounted thereon in accordance with another embodiment of the present invention;
FIG. 5 is a schematic drawing in elevation with portions broken away showing a side view of the breakaway support post of FIG. 4 in its first position;
FIG. 6 is a schematic drawing in elevation with portions broken away showing a side view of the breakaway support post of FIG. 5 rotating from its first position to a second position in response to a force applied to the breakaway support post in one direction corresponding with an impact by a vehicle with one end of the associated guardrail;
FIG. 7 is a schematic drawing showing an isometric view with portions broken away of a highway guardrail system having a breakaway support post with a guardrail mounted thereon in accordance with a further embodiment of the present invention;
FIG. 8 is a schematic drawing in elevation with portions broken away showing a side view of the highway guardrail system of FIG. 7 ;
FIG. 9 is a schematic drawing in section of the breakaway support post taken along lines 9 - 9 of FIG. 8 ;
FIG. 10 is a schematic drawing showing an isometric view with portions broken away of a highway guardrail system having a breakaway support post with a guardrail mounted thereon in accordance with another embodiment of the present invention;
FIG. 11 is a schematic drawing in elevation with portions broken away showing a side view of a breakaway support post analogous to the breakaway support post of FIG. 10 rotating from its first position to a second position and separating in response to a force applied to the breakaway support post in one direction corresponding with an impact by a vehicle with one end of the associated guardrail;
FIG. 12 is a schematic drawing showing an exploded, isometric view with portions broken away of an alternative embodiment of breaker bars suitable for use with the guardrail system illustrated in FIGS. 10 and 11 ;
FIG. 13 is a schematic drawing in elevation with portions broken away showing a side view of the breakaway support post of FIG. 10 utilizing the breaker bars of FIG. 12 and rotating from its first position to a second position and separating in response to a force applied to the breakaway support post in one direction corresponding with an impact by a vehicle with one end of the associated guardrail;
FIG. 14A is a schematic drawing in elevation with portions broken away showing a detail side view of a breakaway support post incorporating a further embodiment of the present invention;
FIG. 14B is a schematic drawing in elevation with portions broken away showing another side view of the breakaway post of FIG. 14A ;
FIG. 15A is a schematic drawing in elevation with portions broken away showing a detail side view of a breakaway post in accordance with still another embodiment of the present invention;
FIG. 15B is a schematic drawing in elevation with portions broken away showing the upper portion and the lower portion of the breakaway support post of FIG. 15A disconnected from each other;
FIG. 15C is a schematic drawing in elevation with portions broken away showing another side view of the breakaway support post of FIG. 15B ; and
FIG. 16 is a schematic drawing in elevation with portions broken away showing a side view of the breakaway support post of FIG. 15A rotating from its first position to a second position in response to a force supplied to the breakaway support post in one direction corresponding with an impact by a vehicle with one end of an associated guardrail.
DETAILED DESCRIPTION OF THE INVENTION
The preferred embodiments of the present invention and its advantages are best understood by referring to the FIGS. 1 through 16 of the drawings, like numerals being used for like and corresponding parts of the various drawings.
Portions of highway guardrail system 20 incorporating one embodiment of the present invention are shown in FIGS. 1 , 2 and 3 . Portions of highway guardrail systems 120 , 220 , and 320 incorporating alternative embodiments of the present invention are shown in FIGS. 4 through 13 . Breakaway support posts incorporating further embodiments of the present invention are shown in FIGS. 14A through 16 . Highway guardrail systems 20 , 120 , 220 , and 320 are typically installed along the edge of a highway or roadway (not expressly shown) adjacent to a hazard (not expressly shown) to prevent a vehicle (not shown) from leaving the associated highway or roadway.
Guardrail systems 20 , 120 , 220 , and 320 are primarily designed and installed along a highway to withstand a rail face impact from a vehicle downstream from an associated end treatment. Various types of guardrail end treatments (not expressly shown) are preferably provided at the end of guardrail 22 facing oncoming traffic. Examples of guardrail end treatments satisfactory for use with the present invention are shown in U.S. Pat. No. 4,655,434 entitled Energy Absorbing Guardrail Terminal; U.S. Pat. No. 4,928,928 entitled Guardrail Extruder Terminal; and U.S. Pat. No. 5,078,366 entitled Guardrail Extruder Terminal. Such guardrail end treatments extend substantially parallel with the associated roadway. U.S. Pat. No. 4,678,166 entitled Eccentric Loader Guardrail Terminal shows a guardrail end treatment which flares away from the associated roadway. U.S. Pat. Nos. 4,655,434; 4,928,928; 5,078,366; and 4,678,166 are incorporated herein by reference. When this type of guardrail end treatment is hit by a vehicle, the guardrail will normally release from the associated support post and allow the impacting vehicle to pass behind downstream portions of the associated guardrail. However, breakaway support posts incorporating teachings of the present invention may be used with any guardrail end treatment or guardrail system having satisfactory energy-absorbing characteristics for the associated roadway and anticipated vehicle traffic.
Support posts 30 , 130 , 230 , 330 and 530 have a strong direction and a weak direction. When a post is subjected to an impact from the strong direction, the post exhibits high mechanical strength. The strong direction is typically oriented perpendicular to the guardrail. Thus, when the post is impacted by a vehicle in the strong direction (such as when the vehicle impacts the face of the guardrail), the post will remain intact and standing, and the vehicle will be redirected back onto the road. When the post is subjected to an impact from the weak direction, the post exhibits low mechanical strength. The weak direction is typically oriented parallel to the guardrail. Thus, when the post is impacted by a vehicle in the weak direction (such as when the vehicle impacts the end of the guardrail), the portion of the post that is substantially above the ground will either break off or bend over, so as to avoid presenting a substantial barrier to the vehicle. Preferably, the upper portion of the post will deflect slightly and then break off, in order to minimize lifting of the impacting vehicle into the air.
One or more support posts 30 , 130 , 230 , 330 , and 530 are preferably incorporated into the respective guardrail end treatment to substantially minimize damage to a vehicle during a head-on impact with the end of guardrail 22 facing oncoming traffic. The number of support posts 30 , 130 , 230 , 330 and 530 and the length of guardrail 22 may be varied depending upon the associated roadway, the hazard adjacent to the roadway requiring installation of highway guardrail system 20 , 120 , 220 or 320 , anticipated vehicle traffic on the associated roadway, and the selected guardrail end treatment. As discussed later in more detail, breakaway support posts 30 , 130 , 230 , 330 and 530 will securely anchor guardrail 22 during a rail face impact or side impact with guardrail 22 to redirect an impacting vehicle back onto the associated roadway. Support posts 30 , 130 , 230 , 330 and 530 will yield or buckle during a head-on impact with the end of guardrail 22 without causing excessive damage to an impacting vehicle.
Support posts 30 , 130 , 230 , 330 and 530 may be fabricated from various types of steel alloys or other materials with the desired strength and/or breakaway characteristics appropriate for the respective highway guardrail system 20 , 120 , 220 , and 320 . For some applications, a breakaway support post incorporating teachings of the present invention may be fabricated from ceramic materials or a mixture of ceramic and metal alloys which are sometimes referred to as cermets.
Portions of breakaway support posts 30 , 130 , 230 , 330 and 530 , as shown in FIGS. 1-16 , have the general configuration associated with a steel I-beam. Alternatively, the teachings of the present invention may be incorporated into a breakaway support post having a generally hollow or solid, rectangular, square or circular cross section.
Breakaway support posts 30 , 130 , 230 , 330 and 530 as shown in FIGS. 1-16 , have respective upper portions and lower portions with approximately the same general cross-section. However, for some applications, the upper portion of a breakaway support post incorporating teachings of the present invention may have a cross-section which is substantially different from the cross-section of the associated lower portion. For example, the upper portion may have the general configuration associated with an I-beam, while the associated lower portion may have a general configuration associated with either a hollow or solid cylindrical post or a hollow or solid square post.
In FIGS. 1 , 2 , 4 , 7 and 10 , highway guardrail systems 20 , 120 , 220 and 320 are shown having a typical deep W-beam twelve (12) gauge type guardrail 22 . For some applications, a thrie beam guardrail may be satisfactorily used. Other types of guardrails, both folded and non-folded, may be satisfactorily used with breakaway support posts 30 , 130 , 230 , 330 and 530 incorporating the teachings of the present invention. Breakaway support posts 30 , 130 , 230 , 330 and 530 may sometimes be described as direct drive support posts.
Various techniques which are well known in the art may be satisfactorily used to install breakaway support posts 30 , 130 , 230 , 330 and 530 depending upon the type of soil conditions and other factors associated with the roadway and the hazard requiring installation of respective highway guardrail systems 20 , 120 , 220 , and 320 . For many applications, breakaway support posts 30 , 130 , 230 , 330 and 530 may be simply driven into the soil using an appropriately sized hydraulic and/or pneumatic driver. As a result, breakaway support posts 30 , 130 , 230 , 330 and 530 may be easily removed from the soil using an appropriately sized crane or other type of pulling tool. For many applications, breakaway posts 30 , 130 , 230 , 330 and 530 may be satisfactorily used to install guardrail 22 adjacent to an associated roadway without the use of metal foundation tubes or other types of post-to-ground installation systems such as concrete with a steel slip base support. U.S. Pat. No. 5,503,495, entitled Thrie-Beam Terminal With Breakaway Post Cable Release, shows one example of a breakaway support post with this type of foundation.
As shown in FIGS. 1 , 2 and 3 , breakaway support post 30 includes elongated body 32 defined in part by web 34 with flanges 36 and 38 attached thereto. Elongated body 32 may be formed by cutting a steel I-beam (not expressly shown) into sections having the desired length for elongated body 32 . A pair of elongated slots 40 and 42 are preferably formed in flange 36 on opposite sides of web 34 . Similarly, a pair of slots 44 and 46 are preferably formed in flange 38 on opposite sides of web 34 . Slots 40 , 42 , 44 and 46 are formed intermediate first end 31 and second end 33 of breakaway support post 30 . Slots 40 , 42 , 44 and 46 define in part a frangible or yieldable connection between an upper portion and a lower portion of support post 30 .
The length of breakaway support post 30 and the location of slots 40 , 42 , 44 and 46 will depend upon various factors including soil conditions and the anticipated amount of force that will be applied to breakaway support post 30 during a rail face impact with guardrail 22 and during a head-on impact with one end of guardrail 22 . For the embodiment shown in FIGS. 1 , 2 and 3 , slots 40 , 42 , 44 and 46 are formed in breakaway post 30 at a location corresponding approximately with the anticipated ground line when breakaway support post 30 is properly installed adjacent to the associated roadway.
For one application, elongated body 32 may be formed from a standard steel I-beam with flanges 36 and 38 having a nominal width of four (4″) inches and web 34 having a nominal width of six (6″) inches. Slots 40 , 42 , 44 and 46 have a generally elongated oval configuration approximately six (6″) inches in length and one fourth (¼″) inch in width. Slots 40 , 42 , 44 , and 46 are positioned intermediate ends 31 and 33 to cause local buckling of the associated breakaway post 30 when properly installed.
For the embodiments shown in FIGS. 1 and 2 , block 48 is disposed between breakaway support post 30 and guardrail 22 . Block 48 may sometimes be referred to as a “blockout.” For other applications, guardrail 22 may be directly mounted adjacent to end 31 of breakaway support post 30 . During a rail face impact between a vehicle and guardrail 22 downstream from the associated end treatment, block 48 provides a lateral offset between breakaway support post 30 and guardrail 22 . The distance and direction of the lateral offset is selected to prevent the wheels (not shown) of an impacting vehicle from striking breakaway support post 30 during the rail face impact.
For the embodiment shown in FIGS. 1 , 2 and 3 , breakaway support post 30 includes soil plates 52 and 54 which are attached to the exterior of respective flanges 36 and 38 adjacent to the portion of breakaway support post 30 which will be inserted into the soil adjacent to the associated roadway. For this embodiment, soil plates 52 and 54 have approximately the same thickness as web 34 and are generally aligned with web 34 on opposite sides of respective flanges 36 and 38 .
Breakaway support post 30 is preferably installed with web 34 extended approximately perpendicular from guardrail 22 and flanges 36 and 38 extending generally parallel with guardrail 22 . By aligning web 34 approximately perpendicular to guardrail 22 , breakaway support post 30 will provide sufficient support to resist large forces associated with a rail face impact or rail face impact between a vehicle and guardrail 22 . As a result of forming slots 40 , 42 , 44 and 46 in respective flanges 36 and 38 and orienting flanges 36 and 38 generally parallel with guardrail 22 , a head-on impact from a vehicle with one end of guardrail 22 will result in buckling or yielding of breakaway support post 30 .
The amount of force required to buckle and/or fracture breakaway support post 30 may be decreased by increasing the size and/or the number of slots 40 , 42 , 44 and 46 formed in respective flanges 36 and 38 . Alternatively, reducing the number and/or size of slots 40 , 42 , 44 and 46 will result in a larger amount of force required to buckle or yield breakaway support post 30 .
The orientation of soil plates 52 and 54 , relative to a head-on impact with one end of guardrail 22 will prevent twisting or tilting of breakaway support post 30 during the head-on impact. The additional support provided by soil plates 52 and 54 will increase the reliability of breakaway support post 30 yielding or buckling at the general location of slots 40 , 42 , 44 and 46 in response to a selected amount of force applied adjacent to end 31 of post 30 in a first direction corresponding to the direction of a head-on impact with one end of guardrail 22 . Soil plate 52 includes a generally triangular portion 56 which extends above elongated slots 40 , 42 , 44 and 46 to provide additional support for breakaway support post 30 and guardrail 22 during a rail face impact.
For some applications, the length of elongated body 32 may be increased such that soil plates 52 and 54 are no longer required to provide additional support for the resulting breakaway support post 30 . Eliminating soil plates 52 and 54 will allow a hydraulic or pneumatic hammer to more quickly install the associated breakaway support post 30 and a crane or hydraulic/pneumatic pulling tool to more easily remove a damaged breakaway support post 30 . Alternatively, breakaway support post 30 could be inserted into an appropriately sized concrete foundation and/or metal sleeve. Soil plates, concrete foundation, sleeves and other anchoring devices can be used in any of the posts of the present invention.
For some applications, it may be preferable to form a breakaway support post in accordance with teachings of the present invention from an elongated body having a generally hollow, rectangular or square configuration (not shown). Slots 40 , 42 , 44 and 46 may then be formed in opposite sides of the resulting breakaway support post which are aligned generally parallel with the associated guardrail similar to flanges 36 and 38 . The other pair of opposite sides preferably extend approximately normal from the associated guardrail similar to web 34 .
When force is applied adjacent to end 31 of breakaway support post 30 in a second direction corresponding with a rail face impact between a vehicle and guardrail 22 , web 34 will resist buckling of breakaway support post 30 and provide sufficient support to redirect the impacting vehicle back onto the roadway.
Breakaway support post 130 , as shown in FIGS. 4 , 5 and 6 , includes elongated body 132 having an upper portion 142 and a lower portion 144 which are rotatably coupled with each other. For the embodiment of the present invention shown in FIGS. 4 , 5 and 6 , rotatable coupling assembly 140 is preferably installed intermediate ends 131 and 133 of elongated body 132 .
Upper portion 142 and lower portion 144 each have a general configuration of an I-beam defined in part by respective webs 134 and flanges 136 and 138 . Upper portion 142 and lower portion 144 may be formed from a conventional steel I-beam in the same manner as previously described.
For the embodiment of the present invention as shown in FIGS. 4 , 5 and 6 , rotatable coupling assembly 140 includes a first generally U-shaped bracket 150 attached to one end of upper portion 142 , opposite end 131 and a second U-shaped bracket 152 attached to the end of lower portion 144 opposite from end 133 . Brackets 150 and 152 each have a generally open, U-shaped configuration with extensions substantially parallel to the flanges and protruding beyond the respective webs. A portion of bracket 150 is preferably sized to fit within a corresponding portion of bracket 152 . Pivot pin 154 extends laterally through adjacent portions of bracket 150 and 152 in a direction which is generally parallel with webs 134 . The resulting breakaway support post 130 is preferably installed with webs 134 and pivot pin 154 extending generally normal from the associated guardrail 22 . As a result of this orientation, webs 134 and rotatable coupling assembly 140 including pivot pin 154 allow breakaway support post 130 to sufficiently support guardrail 22 during a rail face impact to redirect an impacting vehicle back onto the associated roadway.
In FIGS. 4 , 5 and 6 , respective webs 134 of upper portion 142 and lower portion 144 are shown generally aligned parallel with each other. For some applications, the orientation of lower portion 144 may be varied with respect to upper portion 142 such that web 134 of lower portion 144 extends approximately parallel with guardrail 22 . The attachment of brackets 150 and 152 with their respective upper portion 142 and lower portion 144 may be modified to accommodate various orientations of lower portion 144 relative to upper portion 142 .
Depending upon the length of lower portion 144 and the type of soil conditions, soil plates 162 and 164 may be attached to lower portion 144 extending from respective flanges 136 and 138 . For some applications, lower portion 144 may be substantially longer than upper portion 142 . As a result of increasing the length of lower portion 144 , the use of soil plates 162 and 164 may not be required.
Shear pin 156 is laterally inserted through adjacent portions of brackets 150 and 152 offset from pivot pin 154 . Shear pin 156 preferably has a relatively small cross-section as compared to pivot pin 154 . As a result, when a vehicle impacts with one end of guardrail 22 , shear pin 156 will break and allow upper portion 142 to rotate relative to lower portion 144 as shown in FIG. 6 . Shear pin 156 maintains upper portion 142 and lower portion 144 generally aligned with each other during installation of the associated breakaway support post 30 .
The amount of force required to fracture or break shear pin 156 may be determined by a variety of parameters such as the diameter of shear pin 156 , the type of material used to fabricate shear pin 156 , the number of locations (either along a single pin or with plural pins) that must be sheared, and the distance between shear pin 156 and pivot pin 154 . As discussed later in more detail with respect to breakaway support post 530 , as shown in FIGS. 15A through 16 , rotatable coupling 540 may be modified to allow upper portion 542 to disconnect and separate from lower portion 544 .
Various types of releasing mechanisms other than shear pin 156 may be satisfactorily used to maintain upper portion 142 and lower portion 144 generally aligned with each other during normal installation and use of the associated breakaway support post 130 . A wide variety of shear bolts, shear screws and/or breakaway clamps may be used to releasably attach first bracket 150 with second bracket 152 .
When a vehicle impacts with one end of guardrail 22 , force is applied in a first direction to upper portion 142 and will break shear pin 156 . As a result, upper portion 142 will then rotate relative to lower portion 144 as shown in FIG. 6 .
FIGS. 7 , 8 and 9 show portions of highway guardrail system 220 which includes breakaway support post 230 and guardrail 22 . Breakaway support post 230 includes elongated body 32 and is similar in both design and function with breakaway support post 30 . One difference between breakaway support posts 30 and 230 is the replacement of soil plates 52 and 54 by soil plates 254 and 256 . As best shown in FIGS. 8 and 9 , fastener assembly 160 may be used to attach soil plate 254 with elongated body 32 . Fastener assembly 160 includes threaded bolt 163 , hollow sleeve or spacer 168 and nut 165 . The use of soil plate 254 and fastener assembly 160 eliminates some of the welding steps associated with attaching soil plates 52 and 54 to breakaway support post 30 .
Soil plate 254 has a generally rectangular configuration. The length, width and thickness of soil plates 254 may be varied depending upon the intended application for the associated breakaway post 230 and the anticipated soil conditions adjacent to the associated roadway. An appropriately sized hole is preferably formed in the mid-point of soil plate 254 and bolt 163 inserted therethrough. The head 166 of bolt 162 is disposed on the exterior of soil plate 254 . Spacer or hollow sleeve 168 is then fitted over the threaded portion of bolt 163 extending from soil plate 254 opposite from head 166 . A corresponding hole is preferably formed in web 34 at the desired location for soil plate 254 . Bolt 163 is inserted through the hole in web 34 and nut 165 attached thereto.
For some applications, a smaller soil plate 256 may be attached to the exterior of flange 36 adjacent to web 34 . The dimensions and location of soil plate 256 may be varied depending upon the anticipated application including soil conditions, associated with highway guardrail system 220 .
FIGS. 10 and 11 illustrate portions of highway guardrail system 320 , which includes breakaway support post 330 and guardrail 22 . FIG. 11 illustrates an embodiment of support post 330 having narrower breaker bars 350 and 352 than those illustrated in FIG. 10 . Support post 330 includes an elongated body 332 having an upper portion 342 and a lower portion 344 . Upper portion 342 and lower portion 344 each have the general configuration of a steel I-beam similar to elongated body 32 of breakaway support post 30 .
Upper portion 342 and lower portion 344 are defined in part by respective webs 334 and flanges 336 and 338 . Upper portion 342 and lower portion 344 may be formed from a conventional steel I-beam in the same manner as previously described. Lower portion 344 may be positioned substantially within the ground. Alternatively, lower portion 344 could be inserted into a concrete foundation and/or a metal sleeve which have been previously installed at the desired roadside location.
Upper portion 342 and lower portion 344 are provided with breaker bars 350 and 352 . In the embodiment shown in FIG. 10 , flanges 336 and 338 in upper portion 342 are connected to breaker bar 350 , by for example, welds. Flanges 336 and 338 in lower portion 344 may be connected to breaker bar 352 in an analogous fashion. Other suitable connection techniques may be used to couple flanges 336 and 338 of upper and lower portions 342 and 344 to breaker bars 350 and 352 , respectively. For example, as illustrated in FIG. 11 , tie straps 362 and 364 may be used, particularly in an embodiment where breaker bars 350 and 352 are narrower than flanges 336 and 338 , as is the case in FIG. 11 . For some applications, breaker bar 352 may be directly attached to a concrete foundation to eliminate the use of lower portion 344 .
Breaker bars 350 and 352 are connected to each other by fasteners 358 , which is illustrated by a simple nut and bolt; however, other suitable fasteners may be used with this aspect of the invention. Breaker bars 350 and 352 are preferably formed with chamfered or tapered surfaces 354 . Chamfered surfaces 354 cooperate with each other to define in part a notch or gap between adjacent portions of breaker bars 350 and 352 . Chamfered surfaces 354 extend generally parallel with each other in a direction generally normal to guardrail 22 . An imaginary line 359 can also be drawn through fasteners 358 in the same general direction parallel with chamfered surfaces 354 and normal to guardrail 22 . Imaginary line 359 corresponds with a strong direction for breakaway support posts 330 in which breakaway support post 330 exhibits high mechanical strength. There is a notch or gap on each side of the imaginary line 359 .
Chamfered surfaces 354 cooperate with each other to allow upper portion 342 to pivot relative to lower portion 344 during a head-on impact, as illustrated in FIG. 11 . Such pivoting may cause fasteners 358 to break, separating upper portion 342 from lower portion 344 and may therefore substantially minimize damage to a vehicle during a head-on impact with the end of guardrail 22 facing oncoming traffic. The orientation of chamfered surfaces 354 and fasteners 358 relative to each other further define a weak direction for breakaway support post 330 in which support post 330 exhibits low mechanical strength. However, chamfered surfaces 354 do not reduce the ability of guardrail 320 to redirect an impacting vehicle back onto the associated roadway during a rail face impact with guardrail 22 .
FIG. 12 is a schematic drawing showing an exploded isometric view with portions broken away of an alternative embodiment of breaker bars suitable for use in guardrail system 320 . Breaker bars 450 and 452 perform similar functions as breaker bars 350 and 352 . Breaker bar 450 includes a flat plate 453 having a protruding member or projection 454 . Breaker bar 452 includes a flat plate 455 having a protruding member or projection 456 . Flat plates 453 and 455 are each formed with two or more apertures 458 for receiving a connecting member, such as mechanical fastener 358 , for attaching breaker bars 450 and 452 with each other. The use of protruding members or projections 454 and 456 allows upper portion 342 to pivot relative to lower portion 344 during a head-on impact, as illustrated in FIG. 13 . Impact from the weak direction for support post 330 will result in bending and preferably failure of connecting members 358 . Failure of connecting members 358 separates upper portion 342 from lower portion 344 and may, therefore, substantially minimize damage to a vehicle during a head-on impact with the end of guardrail 22 facing oncoming traffic. However, protruding members or projections 454 and 456 do not reduce the ability of guardrail 22 to redirect an impacting vehicle back onto the associated roadway during a rail face impact.
FIGS. 14A and 14B are schematic drawings with portions broken away showing an alternative embodiment of a frangible or yieldable connection satisfactory for releasably coupling upper portion 342 with lower portion 344 of support post 330 . For this embodiment, breaker bars 450 and 452 are substantially the same as previously described with respect to the embodiment shown in FIG. 13 , except for the elimination of protruding members or projections 454 and 456 . A pair of elongated connecting members 458 and a plurality of nuts 460 are preferably provided to maintain a desired gap or spacing between breaker bars 450 and 452 . For the embodiment shown in FIGS. 14A and 14B , elongated connecting members 458 and nuts 460 have matching threads. However, various types of mechanical fasteners and connecting members may be satisfactorily used to position upper portion 332 of support post 330 relative to lower portion 344 .
As a result of incorporated teachings of the present invention, support post 330 has relatively low mechanical strength with respect to impact from a direction generally normal to an imaginary line 359 (see FIG. 10 ) extending through connecting members 358 or 458 as appropriate. This direction may be referred to as the “weak direction.” Connecting members 358 and 458 are preferably formed from materials which will yield and preferably fracture or break to allow upper portion 342 to separate from lower portion 344 . Since there is a gap between the breaker bars 350 and 352 or breaker bars 450 and 452 to either side of line 359 in the weak direction, connecting members 358 or 458 as appropriate will carry substantially all of the force or load from an impact in the weak direction.
When support post 330 is impacted from another direction, the resulting force, or at least a component of the resulting force, will tend to place one of the associated connecting members 358 or 458 as appropriate in tension, and will tend to place the other connecting member 358 or 458 as appropriate in compression. Therefore, the mechanical strength of the frangible connection between upper portion 342 and lower portion 344 is substantially greater in the strong direction as compared with an impact from the weak direction. The strongest direction for an impact with support post 330 is from a direction substantially perpendicular to the surface of flanges 338 and 336 and parallel with web 334 (the strong direction). The weakest direction for an impact with support post 330 is in a direction which is substantially perpendicular to web 334 and parallel with flanges 336 and 338 .
Spacers with various forms and configurations may be used to separate breaker bars 350 and 352 or 450 and 452 from each other as desired. For the embodiment shown in FIGS. 10 and 11 , tapered surfaces or chamfered surfaces 354 form the necessary spacers as integral components of breaker bars 350 and 352 . For the embodiment shown in FIGS. 12 and 13 , protruding members or projections 454 and 456 function as spacers to form the desired gap. For the embodiment shown in FIGS. 14A and 14B , nuts 460 cooperate with connecting members 458 to function as spacers to form the desired gap. Nuts 460 that are between breaker bars 450 and 452 may also be referred to as “stops.”
For some applications, upper portion 342 and lower portion 344 of support post 330 may be coupled with each other by only one connecting member 358 or 458 . Alternatively, more than two connecting members 358 or 458 may be used depending upon the anticipated application for the associated support post 330 . For some applications, one connecting member 358 or 458 may be provided on the side of support post 330 which is immediately adjacent to guardrail 22 . The associated breaker bars 350 and 352 or 450 and 452 will contact each other on the opposite side of the post, whereby the single connecting member 358 or 458 as appropriate will provide sufficient strength for support post 330 to withstand rail face or side impact with the associated guard rail 22 .
Support post 530 , as shown in FIGS. 15A through 16 , is substantially similar to previously described support post 130 , except rotatable coupling assembly 140 has been replaced by rotatable coupling assembly or releasable hinge 540 . The embodiment shown in FIGS. 15A , 15 B, 15 C and 16 provides for the separation of upper portion 142 from lower portion 144 . Thus, upper portion 142 will not lift an impacting vehicle. Support post 530 may be formed in part by upper portion 142 and lower portion 144 as previously described with respect to support post 130 . Coupling assembly or releasable hinge 540 preferably includes a first generally U-shaped bracket 550 attached to one end of upper portion 142 , and a second U-shaped bracket 552 attached to an adjacent end of lower portion 144 . Brackets 550 and 552 each have a generally open, U-shaped configuration. A portion of bracket 550 is preferably sized to fit over a corresponding portion of bracket 552 .
Pivot pin 554 preferably extends through adjacent portions of brackets 552 in a direction which is generally parallel with webs 134 . Alternatively, pivot pin 554 may be replaced by generally round projections extending from opposite sides of bracket 552 . Bracket 550 preferably includes a pair of slots 572 formed in opposite sides thereof. Slots 572 are preferably sized to releasably engage respective portions of pin 554 which extend from bracket 552 . Slots 572 cooperate with pivot pin 554 to allow rotation of upper portion 142 relative to lower portion 144 , and to allow disengagement of upper portion 142 from lower portion 144 .
The resulting breakaway support post 530 is preferably installed with webs 134 and pivot pin 554 extending generally normal from the associated guardrail 22 . As a result of this orientation, webs 134 and releasable hinge 540 , including pivot pin 554 , allow support post 530 to adequately support guardrail 22 during a rail face impact to redirect an impacting vehicle back onto the associated roadway.
Shear pin 556 is preferably inserted through adjacent portions of brackets 550 and 552 offset from pivot pin 554 . Shear pin 556 maintains upper portion 142 and lower portion 144 generally aligned with each other during installation of the associated breakaway support post 530 . Shear pin 556 preferably has a relatively small cross-section as compared to pivot pin 554 . As a result, when a vehicle impacts with one end of guardrail 22 , shear pin 556 will break and allow upper portion 142 to rotate relative to lower portion 144 as shown in FIG. 16 . For some applications, push bar 580 is preferably attached to and extends between opposite sides of bracket 552 . The location of push bar 580 on bracket 552 is selected to assist disengagement of slot 572 from pivot pin 554 as upper portion 142 rotates relative to lower portion 144 . See FIG. 16 .
The amount of force required to fracture or break shear pin 556 may be determined by a variety of parameters such as the diameter of shear pin 556 , the type of material used to fabricate shear pin 556 , the number of locations (either along a single pin or with plural pins) that must be sheared, and the distance between shear pin 556 and pivot pin 554 .
Various types of releasing mechanisms other than shear pin 556 may be satisfactorily used to maintain upper portion 142 and lower portion 144 generally aligned with each other during normal installation and use of the associated breakaway support 530 . A wide variety of shear bolts, shear screws, frangible disks, and/or breakaway clamps may be used to releasably attach first bracket 550 with second bracket 552 .
When a vehicle impacts with one end of guardrail 22 , force is applied in a first direction (weak direction) to upper portion 142 and will break shear pin 556 . As a result, upper portion 142 will then rotate relative to lower portion 144 as shown in FIG. 16 . When portions of bracket 550 contact push bar 580 , slots 572 will disengage from pivot pin 554 and release upper portion 142 from lower portion 144 .
Although the present invention and its advantages have been described in detail it should be understood that various changes, substitutions, and alterations can be made hereto without departing from the spirit and scope of the invention as defined by the following claims.
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A support post for a guardrail has a strong axis and a weak axis which is substantially perpendicular to the strong axis. The support post is adapted to receive a guardrail such that the rail face of the guardrail runs generally perpendicular to the strong axis such that the support post resists an impact on the face of the guardrail and yields to an impact force on the end of the guardrail.
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FIELD
[0001] The shredder apparatus and method for shredding disclosed herein relate generally to the shredding of wet chip materials that are subsequently separated into dry chips and fluid, and, more specifically, to a shredder apparatus having a shaftless shredder ring component and a shredder comb member component that cooperate to shred wet chip materials.
BACKGROUND
[0002] Wet chip materials are generated in the course of machining operations. Often the wet chip material, which can vary in size and configuration, is passed through a shredder apparatus that serves to shred the material prior to its passing on to other work stations, e.g., filtering or centrifugal separation stations.
[0003] Shredder apparatuses for shredding wet chip materials are well known in the art. Conventional shredder apparatuses include systems that utilize a plurality of spaced shredder members that are disposed upon a rotatable rotor. One example is the shredder apparatus shown and disclosed in my co-pending U.S. patent application Ser. No. 10/611,526, filed Jul. 1, 2003, the disclosure, drawings and claims of which are incorporated by reference in their entirety herein. Upon actuation of such a shredder apparatus, the rotor rotates, and the shredder members fixed to the rotor rotate and cooperate with shredder comb members to shred material entering the apparatus.
[0004] In some instances, however, it has been found that, because of the nature of the material to be shredded, the shredder apparatus experiences difficulty in properly transporting the material to be shredded to the shredder components, such that appropriate shredding does not occur. For example, certain wet chip material, e.g., ball bearing-type scrap material or scrap rings formed in the manufacture of pistons, sometimes fail to shred properly with conventional shredding apparatuses. It has been found that this type of material, once it enters the shredder apparatus, is not properly carried to the shredder components within the shredder apparatus.
[0005] What is desired is to have a shredder apparatus that allows for the appropriate shredding of material whereby material to be shredded is properly transported to and within the shredder apparatus.
[0006] It is also desired to have a shredder apparatus where the shredder elements that cooperate to shred material are positioned principally orthogonal to the primary flow direction of the material to be shredded.
[0007] It is further desired to have a shredder apparatus located at least partially in a coolant flow path so that coolant flowing along the flow path and through the shredder apparatus assists in moving material through the shredder.
[0008] Finally, it is desired to have a shredder apparatus where, if desired, the shredding can occur without the requirement of having rotating shredding elements located on a rotating shaft-like member.
SUMMARY
[0009] A shredder apparatus may include a shaftless shredder ring component attached to an apparatus frame. The shredder ring component may be a cylindrically-shaped member that includes a plurality of spaced shredder rings. Spacer bars serve to join and space the shredder rings from each other. The shredder ring component is positioned within the frame to be substantially in-line with wet chip or other material entering the shredder apparatus to be shredded.
[0010] A secondary shredder component includes a plurality of spaced comb members attached to the frame. Upon rotation of the shredder ring component relative to the comb members, the shredder rings and comb members cooperate to shred material in the shredder apparatus into more discrete wet chips.
[0011] Wet chip material enters the shredder apparatus through an opening in a frame wall and passes through one end of the shredder ring component. While in the shredder ring component, the material is shredded due to the cooperation of the comb members and shredder rings. Following a shredding operation, the shredded material passes out of the remaining end of the shredder ring component.
[0012] Other advantages of such a shredder apparatus will become apparent from the drawings and the following detailed description of the shredder apparatus and method of shredding.
DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 shows a frontal perspective view of the shredder apparatus;
[0014] FIG. 2 shows a front view of shredder apparatus of FIG. 1 ;
[0015] FIG. 3 shows a left side view of the shredder apparatus of FIG. 1 ;
[0016] FIG. 4 shows a perspective rear view of the shredder apparatus of FIG. 1 with the drive assembly and top plate removed;
[0017] FIG. 5A shows a perspective view of a shredder ring having a first shredder portion;
[0018] FIG. 5B shows a perspective view of a shredder ring having a second shredder portion;
[0019] FIG. 6 shows an exploded view of a sprocket ring assembly;
[0020] FIG. 7 shows a perspective view of a shredder comb member;
[0021] FIG. 8 shows a perspective view of a shredder ring spacer bar having a plurality of grooves located therein;
[0022] FIG. 9 shows a rear, or discharge end, perspective view of the shredder rings and spacer bars, as assembled;
[0023] FIG. 10 shows a frontal perspective view of the shredder rings and spacer bars, as assembled;
[0024] FIG. 11 shows an enlarged, partial perspective view of a plurality of cam followers contacting a surface of a shredder ring;
[0025] FIG. 12 shows a frontal perspective view of spaced shredder rings and comb members positioned relative to one another;
[0026] FIG. 13 shows a schematic diagram of a drive assembly employed in the shredder apparatus of FIG. 1 ;
[0027] FIG. 14 shows a schematic diagram of a shredder assembly, wherein the shredder ring component is tapered and the secondary shredder component comprises comb members having shredder portions of different lengths; and
[0028] FIG. 15 shows a frontal perspective of the shredder apparatus of FIG. 1 disposed at least partially in a fluid flow path (e.g., a flume).
DETAILED DESCRIPTION
[0029] An exemplary shredder apparatus 10 comprises frame assembly 11 that, as illustrated in FIGS. 1, 2 , and 4 , includes base 12 , front (end) wall 13 , back or rear (end) wall 14 and side walls 15 , 16 . Top plate 17 is fixed at plate ends 18 , 19 and sides 20 , 21 to the frame assembly front, back and side walls 13 , 14 , 15 , 16 . Top plate 17 has an opening therein. A second top plate 22 , which, if desired, can be hinged, is disposed on top of top plate 17 and covers the opening in plate 17 . A conventional locking assembly 23 , as illustrated in FIG. 2 , holds plate 22 in place relative to plate 17 . A first threaded boss 24 extends upwardly from plate 17 and a second threaded boss 25 extends upwardly from top plate 22 . Bolt 26 extends through the two bosses and is held in place by nut 27 .
[0030] Shredder assembly 30 is disposed within frame assembly 11 . Shredder assembly 30 comprises a first, cylindrically-shaped shredder ring component 31 and a second shredder component 32 (see FIGS. 2, 3 , and 12 ). Shredder ring and shredder components 31 , 32 cooperate to shred material entering shredder apparatus 10 through an opening in front wall 13 .
[0031] The shredder ring component 31 is a shaftless rotatable member made up of plurality of shredder rings 33 , 34 (see FIGS. 9 and 11 ). As illustrated in FIGS. 5A and 5B , rings 33 , 34 include an annular portion 35 bounded by a radially outer surface and a radially inner surface and having a thickness. The radially inner surface also defines a ring opening 36 . Each ring 33 , 34 includes a plurality of equally spaced projections 37 extending inwardly from portion 35 into ring opening 36 . A recess 38 is located in ring portion 35 adjacent each projection 37 .
[0032] Rings 33 have a plurality of spaced tapered shredder portions 39 (see FIGS. 2 and 5 A), each having a first desired length “x”. Rings 34 have a plurality of shredder portions 40 (see FIGS. 2 and 5 B) each having a second desired length “y”. The shredder portions 39 , 40 are, as shown, formed integrally with or defined by the radially inner surfaces of the rings 33 , 34 .
[0033] Turning to FIGS. 2, 4 and 8 , the rings 33 , 34 are spaced from each other by means of a plurality of spacer bars 41 . As shown in FIG. 8 , each spacer bar 41 includes a plurality of projections 42 along the length of one side of bar 41 to define a plurality of spaced grooves 43 . As shown in FIGS. 2 and 4 , each spacer bar 41 is positioned in one of the recesses 38 of each shredder ring 33 , 34 and abuts one of the projections 37 . Specifically, one of the spacer bar projections 42 will be disposed in one of the shredder ring recesses 38 . Once the bar 41 is positioned relative to the plurality of cutter rings 33 , 34 , the bar 41 is fixed in place, for example, by welding.
[0034] It will be appreciated that while four, equally-spaced spacer bars are employed in this illustrative embodiment, other spacer bar arrangements could be employed to space and align the rings 33 , 34 with respect to the shredder component 32 described below. Further, while, in the shredder ring component embodiment shown, a pair of spaced shredder rings 33 is shown positioned adjacent a pair of spaced shredder rings 34 , other arrangements could be utilized. For instance, a single ring 33 could be positioned adjacent a single ring 34 .
[0035] As shown in FIG. 7 , for example, the secondary shredder component 32 comprises a plurality of spaced comb members 44 . Each comb member 44 includes an opening 45 and a shredder portion 46 . A bar 47 extends through each opening 45 to provide a plurality of aligned, spaced comb members 44 .
[0036] The bar 47 is fixed to the frame assembly front and rear walls 13 , 14 in any suitable manner, e.g., welding or a release bolt fastener such as illustrated in FIGS. 1, 2 . Each comb member 44 is positioned on bar 47 so that it can cooperate with a shredder portion 39 , 40 on shredder rings 33 , 34 . The comb members 44 are positioned on bar 47 so that they extend into and pass through the spacer bar grooves 43 during operation of shredder apparatus 10 . The comb members 44 may move relative to the bar 47 , although it is preferred to limit the movement of the comb members 44 relative to the bar 47 , for example, through the cooperation of the cross-section of the bar 47 (which is square as shown) and the shape of the opening 45 (which is also square as shown) so that the component 32 is substantially stationary.
[0037] Shredder ring component 31 is positioned within frame assembly 11 so that the cylindrically-shaped structure extends from front wall 13 to rear wall 14 . FIGS. 4 and 12 , for example, illustrate a system for mounting shredder ring component 31 to frame assembly 11 . A plurality of cam follower assemblies 50 are disposed on each end wall 13 , 14 . The assemblies 50 surround an opening in the end walls 13 , 14 . As shown in FIG. 3 , cam follower assemblies 50 each include a bolt 5 1 , washer 52 , nut 53 and cam follower 54 in the form of a roller. Cam followers 54 position shredder ring component 31 in position within the frame assembly 11 while allowing for rotation of ring component 31 . Rollers or cam followers 54 , as illustrated in FIG. 11 , contact the outer face 56 of each outboard shredder ring located contiguous to a respective frame assembly end wall 13 , 14 .
[0038] Shredder ring component 31 also includes a sprocket ring assembly 58 that, as illustrated in FIGS. 3 and 6 , includes shredder sprocket ring 59 having a sprocket 60 , two spacer or shield rings 61 , 62 and a modified shredder ring 63 having a recess 64 formed in the outer circular ring portion 65 . Shredder ring 63 , in this particular embodiment, is the same as shredder ring 34 save for recess 64 formed in annular portion 65 . Sprocket ring 59 can be fixed in place in recess 64 of shredder ring 63 by any suitable means, such as, for example, welding.
[0039] FIG. 3 shows sprocket ring assembly 58 located on shredder ring component 31 . The sprocket ring assembly 58 is disposed inwardly from the end of component 31 located contiguous to rear end wall 14 . Spacer or shield ring 61 is located adjacent one side of shredder ring 63 and spacer or shield ring 62 is located adjacent the opposite side of shredder ring 63 . Spacer or shield rings 61 , 62 sandwich sprocket ring 59 between them. These spacer or shield rings 61 , 62 shield the chain from contacting the adjacent shredder rings 63 .
[0040] As shown in FIG. 13 , drive assembly 70 includes motor 71 having a drive shaft that is connected by belt drive to a conventional gear reducer 72 . A drive sprocket 73 is attached to drive shaft 74 extending from reducer 72 . Sprocket chain 75 connects drive sprocket 73 and sprocket ring 59 . As shown in FIG. 3 , for example, a cover 76 encloses the belt drive between motor 71 and reducer 72 , and a cover 77 encloses the sprocket chain 75 .
[0041] In operation, material to be shredded is directed to an inlet opening 81 in front end wall 13 . Upon actuation of motor 71 of drive assembly 70 , shredder ring component 31 rotates about its longitudinal axis which is substantially in-line with the incoming material to be shredded, as opposed to traversing the material. Shredder rings 33 , 34 rotate whereby shredder portions 39 , 40 cooperate with comb members 44 to shred the material passing through the openings 36 defined by the radially inner surfaces of the rings 33 , 34 . The shredded material continues on through shredder assembly 30 and discharges out of opening 82 in rear end wall 14 . It has been found that having shredder portions 39 , 40 of different lengths “x” and “y” assist in transporting the material to be shredded and shredded material along the length of shredder assembly 30 .
[0042] In some instances, where a shredder apparatus 10 is disposed at least partially in a fluid flow path 100 (as shown in FIG. 15 ), fluid and material to be shredded (e.g., wet chips) flow along the flow path 100 and through the shredder assembly 30 (as illustrated by the arrow marked “F”). In such a case, the fluid may also assist in directing or moving material to be shredded, being shredded or having been shredded through shredder assembly 30 . For example, as shown in FIG. 15 , the shredder apparatus 10 , and in particular shredder assembly 30 , is disposed at least partially in a fluid flow path 100 , in this case defined, at least in part, by a flume. In other embodiments, the shredder apparatus 10 and/or shredder assembly 30 may be totally or almost totally disposed or submerged in the fluid flow path. The fluid (including coolant) flowing along the flume also passes through the shredder assembly 30 and directs the material (including wet chips and shredded wet chips) through the shredder assembly 30 . Eventually, the fluid and shredded material passes out of the shredder assembly 30 and shredder apparatus 10 along the fluid flow path 100 .
[0043] While shredder rings 33 , 34 have been shown as having the same outer diameter, it is appreciated that, if desired, the shredder rings could be formed of varying diameters traveling from one end of the cylindrically-shaped shredder ring component 31 to the remaining end. In this embodiment, the cylindrically-shaped ring component would resemble somewhat of a cone-like or tapered shape, with the larger opening preferably contiguous the material feed end of apparatus 10 .
[0044] FIG. 14 illustrates such an embodiment in which shredder ring component 90 has a tapered or cone-like shape. In this embodiment, the shredder ring 92 closest to the material feed end of component 90 would have the largest diameter, “D”, in the component 90 , whereas the shredder ring 93 nearest the exit end would have the smallest diameter, “d”. Similarly, secondary shredder component 94 would also employ comb members having shredder portions of varying sizes, but in the lengths of the comb members would vary inversely to the diameters of the shredder rings. That is, the comb member 95 contiguous to the ring 93 would preferably have a greater length, “L”, than the length, “1”, of the comb member 96 located contiguous to ring 92 .
[0045] Similarly, if desired, the tapered shredder portions of shredder rings 33 , 34 could be arranged to form a helical shaped shearing path progressing from the feed end of shredder ring component 31 to the material discharge end. This could be accomplished by varying the length dimensions of “x” and “y” of the shredder portions to form a helical path.
[0046] Utilizing the embodiment shown and disclosed herein allows material to be shredded to enter a shredder assembly wherein the shredder assembly is substantially in-line with the material to be shredded. Moreover, the rotatable component comprises a shaftless ring component, as opposed to being mounted on a shaft.
[0047] Further, it may be desired to have the shredder rotation reverse in the event that a large piece of material to be shredded interferes with the shredder operation. The drive assembly 70 can be actuated to reverse the direction of shredder ring component 31 to allow the unwanted material to be cleared. A drive assembly utilizing this type of reversible drive assembly is disclosed in my heretofore-referenced pending U.S. patent application Ser. No. 10/611,526, filed Jul. 1, 2003, which has been incorporated by reference herein in its entirety.
[0048] While one or more embodiments have been illustrated and described in detail herein, it will be understood that modifications and variations thereof may be effected without departing from the spirit of the invention and the appended claims.
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A shredder apparatus has a moveable, shaftless ring component and a secondary comb member component. The ring component and the secondary component cooperate to shred material. The shredder mechanism may be positioned so as to be substantially in-line with the material entering the shredder. The shredder apparatus may be used in a method for shredding materials.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a service communication system for directing a service attendant to an automated, user operated device requiring service attention, and more particularly to a communications system for coordinating the assignments of a pool of service personnel.
2. Description of the Prior Art
In current casino settings the use of a large number of automated gaming devices, including slot machines, is an arrangement of substantial commercial preference. Automated devices allow for more varied selection of games, the comfort of impersonal interchange, along with all the other well-known advantages associated with automation, cybernetics and/or robotics. The automated gaming device and its most basic form, the slot machine, are therefore found in large numbers throughout commercial establishments devoted to gambling.
While the servile, untiring obedience of an automated device is well known, in a casino there still remains a substantial need for personal service. Most frequently the attention required in the course of use of a slot machine or automated gaming device is that associated with the demands of the patron. Typically the playing patron may not understand the mechanics of the use of the machine, may require some credit accommodation, or may simply be out of change. Less frequently, but nonetheless with some regularity, the automated device itself may require service, a function somewhat more technically complex entailing different skills and proficiency.
Both instances, however, evoke the same response from the patron, the response of pushing a summoning button to turn on a light on the machine. Since personal attention needs to be provided promptly to maintain customer satisfaction and loyalty, work duplication is inherent in this current practice. Moreover the number of illuminated summoning lights can become quite large on a busy day, to a point where perception is rendered difficult when displayed against a background of jackpot bells and other flashing lights, a background in which the attending staff encounters some difficulty in perceiving the requesting signal. Confusion is therefore inherent.
In the past various mechanisms have been devised which in one manner or another produce some kind of a remote signal indicating, or even anticipating, a troubling state of an automatic machine. For example: U.S. Pat. No. 5,954,576 to Coulter et al appears to teach a signaling system for a low coin level in a slot machine, allowing for a preemptive replenishment; U.S. Pat. No. 4,614,342 to Takashima appears to teach a multiple player automatic gaming system which is implemented with an indicator useful to indicate operational problems perceived by a player; and U.S. Pat. No. 5,919,091 to Bell et al appears to teach a plurality of casino gaming machines tied together in a computer network which includes servicing requests sent to a central station. Each of the foregoing, while suitable for the purposes intended, fails to attend to the noisy work setting of the attending personnel, and particularly the confusing mix of machine service and patron demand signals that is so prevalent in the current setting.
Those in the art will appreciate that a signal from a gaming casino patron sometimes coincides with one or another failure in the operation of the gaming machine. Simply, the latter precipitates the former. Thus patron attention requests that immediately follow or are contemporaneous with a machine failure are usually reporting the failure, and if both the service attendant and the patron assistant respond duplication is inherent. Accordingly, a logical process is required to detect these coinciding signals in order to direct only the service attendant to provide the response.
Moreover, some machine service requirements are less complex than others and can therefore be sequenced in the service assignment. Thus the service attendant may be assigned to replenish some coin hoppers on his path to the site of a major machine failure, again a logical sequencing process susceptible of programmed implementation. There are therefore numerous instances in a casino setting where coherent, logical communications will both simplify the process while also reducing the stress level of the employees.
Along with these requests summoning personal assistance or machine service are also the occasional signals indicating a jackpot payout that may exceed the coin storage capacity of the machine. These jackpots are usually accompanied by all sorts of light and sound displays which add to the already noisy background of a gambling establishment. Thus machine failure, an imminent need for intervention in the automatic operation thereof (e.g., running out of currency or coin) or any other condition that may be sensed by the diagnostic system of the machine are cumulative with the high stress events of a payout that is often competing with a patron's request for assistance now expressed by a single signal, a light on the machine requesting change.
In the past these concerns have been only sporadically considered, most often in the setting of a particular machine failure or servicing requirement. For example U.S. Pat. No. 5,919,091 to Bell et al appears to teach a communication system between a plurality of slot machines provided with some fault protection and a central control, while U.S. Pat. No. 5,954,583 to Green describes in portions thereof an automatic summoning process for calling a service operator. Once again, each of the foregoing, while suitable for the purposes intended, fails to describe or suggest a summoning system which logically selects the correct responding skill level, while conserving all others to their proper tasks.
Thus, mixed in with the requests summoning personal assistance, are also the occasional signals indicating a jackpot, a machine failure, an imminent need for intervention in the automatic operation thereof (e.g., running out of currency or coin) or any other condition that may be sensed by the diagnostic system of the machine. Clearly, this intense environment is prone to breed patron irritation.
A logical system that optimizes the response patterns and assignments of a large group of attending personnel is therefore extensively sought, and it is one such system that is disclosed herein.
SUMMARY OF THE INVENTION
Accordingly, it is the general purpose and object of the present invention to provide a central processing system for logical management of assisting and servicing personnel assignments.
Other objects of the present invention are to provide a wireless communication system for directing the assignments of servicing casino gaming machines and for assisting casino patrons.
Yet further objects of the invention are to provide a communication system for use in a casino for communicating various requests for personal assistance and sequencing machine servicing requests to a central processing facility for retransmission in a logical arrangement to individual ones of servicing and assisting personnel.
Briefly, these and other objects are accomplished within the present invention by providing a communication link between the various slot machines, automatic gaming machines and other automated devices in the casino that interface with a patron, and a central processing station. The communication link may be hard wired, by radio frequency (RF), infrared or even optical carrier and may convey separate codes for at least the following events at a gaming machine:
1. The patron has depressed the change button, causing a light to go on on top of the machine;
2. The player has caused the statistical combination of a jackpot and there is a large payment due;
3. The gaming machine is out of coins;
4. The machine is simply jammed; and
5. The machine is in some other failure state.
Of course, the first condition will often occur in parallel with items 2 through 5, as a patron will typically reach for the sole communication mechanism once any difficulty arises. Accordingly, within the central processing station the signals that carry diagnostic information are compared in their time relationship with the corresponding patron's personal service request signal, and if a coincidence is found a logical deduction is made that the former caused the latter. In this manner one primary source of confusion is reduced.
Moreover, the logical process does not need to differentiate between the machine service requests 2 through 5. In each instance the response required is one provided by a skilled machine service attendant and not by the personal patron assistant that heretofore was primarily devoted to providing change. In this manner the number of dispatching messages is reduced, optimizing the use of personnel.
Accordingly, upon receipt of the several signals 1 through 5 from a particular gaming machine the central station performs the above logical operation determining if the response is to be made by a service attendant, and if so a summoning signal is transmitted which identifies (a) the attendant selected, (b) the machine location from which the service signal was received, and (c) the type of service request, i.e., a code corresponding to one of the requests 2 through 5. If, on the other hand, the personal service (the light) signal is unrelated to a concurrent machine service request then the central station processor issues a personal service request, now directed to a particular patron assistant. Thus the central processing station selects the type of employee that is sent to cure the problem and the particular one of the employees within each class. This last selection is based on geometric proximity of the assigned employee pool, a pool continuously reduced by those summoned earlier that are still on assignment and increased by those that have completed their task, grouped by grid mapping of the casino wherein each grid coordinate is associated with a specific personnel roster. Once the assigned employee completes the task he or she then sends a completion signal to the central station and is returned back to the pool of available employees.
Concurrently the central station may also maintain a transaction log corresponding to each employee, each machine and each coordinate group. This transaction data may be used to develop assignment profiles, work load predictions and even redistribution of the whole employee roster in the various coordinate groups. This available data base is therefore not just useful in meeting customer demands but is also useful in casino management, to optimize staffing levels.
Accordingly, each casino service employee is provided with a communication device, e.g., a transceiver, by which the employee is summoned, directed to a particular machine and with which the employee then responds once the assignment is completed. These communication devices may take the form of general purpose pagers, or preferably a dedicated form useful with a single channel or narrow frequency, low wattage, local carrier or transmission medium. In each instance the information is transmitted in the form of data bursts or packets, including the identification code of the receiving device (destination address), the identification code of the sender (originating address) and the message (e.g., the coordinate of the machine to be serviced and the type of service).
Of course, the data packet may also include one or more error detection schemes to insure data integrity, (e.g., odd parity bit) which may automatically invoke a ‘repeat’ request back to the sender. The receiving instrument is thus assured of receiving the correct message which includes the location of the service request and the type of assignment (e.g., reload coin hopper). Similarly, the task completion response includes the identification code of the sender, the address of the recipient device and some code indicating completion of the assignment, together with error checking signals to invoke a similar ‘repeat’ response from the receiving device if a transmission error is detected.
Those in the art will appreciate that the foregoing transmission ‘packets’ are quite limited in their content or bit length and are therefore well suited for single channel transmission like that generally known under the mark or symbol “Ethernet” adopted by the Xerox Corporation, Stamford, Conn., and described in U.S. Pat. No. 4,063,220 to Metcalfe et al. More importantly, the several types of response to a summoning signal are particularly useful in rank ordering the interval between the various devices competing for the channel. Thus the central station will be accorded a higher priority, and therefore a shorter inactive interval following data collision, while the personal service transceivers are assigned the lowest priority and consequently the longest interval.
The foregoing single channel system is particularly suited for multiple network arrangement according to ‘zones’ in a single gaming establishment. Simply, the use of a single channel allows for very narrow carrier tuning, low power levels and therefore several communication systems may co-reside in a single facility without causing mutual interference or bandwidth crowding.
While the acknowledgment signal protocol and error checking substantially increase system reliability and convenience of use, further benefits may be derived from two-way communication. For example, a reassuring message like “an assistant is on the way” or “an assistant will be here shortly”, depending on the current depth of previous assignments, may be communicated back to be displayed on the summoning device. The inventive communication system, therefore, both organizes the labor pool and also assists in the maintenance of patrons' tranquility and enjoyment.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic illustration of an inventive casino communication system in accordance with a first implementation thereof;
FIG. 2 is a logic diagram of a transceiver useful with the inventive communication system generally illustrated in FIG. 1;
FIG. 3 is a logic diagram of a communication adaptor for slot machines or other gaming machines useful with the invention herein;
FIG. 4 is a pulse diagram of a pulse sequence useful in the transmission of signals in the inventive communication system shown in FIG. 1; and
FIG. 5 is a flow chart illustrating the sequence of steps effected by the logical processes of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
As shown in FIGS. 1 through 4, the inventive communication system generally designated by the numeral 10 comprises a first communication zone Z 1 and a second communication zone Z 2 where the signals between the zones may overlap. Zone Z 1 comprises a central station generally at 11 including a transceiver stage 12 tied to a data processing system 14 . Transceiver 12 then communicates by way of a narrow frequency band radio signal ff 1 to a plurality of portable communication units 21 - 1 through 21 - n , each of the units again including its own transceiver 22 tied to a logic stage 24 .
Similarly, zone Z 2 includes its own central station 111 also provided with a transceiver 112 and a processor 114 communicating by way of rf signal ff 2 with a further plurality of communication units 121 - 1 through 121 - n . Each of these-portable units, like those earlier described, includes a transceiver stage 122 tuned to the frequency ff 2 and communicating with a logic stage 124 .
Each of the zones Z 1 and Z 2 may be geometrically segmented into a set of grid coordinates G 1 - 11 through G 1 - mn and G 2 - 11 through G 2 - pq where the suffix defines the particular area within which one or more slot machines or other gaming devices are located, illustrated herein as machines M 1 - 1 through M 1 - r for those located in zone Z 1 and as machines M 2 - 1 through M 2 - s for those in zone Z 2 . In a manner described below each of the foregoing machines M 1 - 1 through M 1 - r and M 2 - 1 through M 2 - s may be connected to the corresponding central station 11 and 111 either by way of the rf links ff 1 and ff 2 or even by hard wire (not shown). It is this communication path that transmits to the central station the earlier summarized conditions 1 through 5.
By particular reference to FIG. 2 each of the communication units 21 - 1 - 21 - n and 121 - 1 - 121 - n take the form of a portable device contained in a housing 20 and including a message display. Except for the carrier frequency ff 1 and ff 2 the operation of transceivers 22 and 122 are functionally alike and their corresponding logic units 24 and 124 are also substantially alike excepting, of course, the unit's designation or address. Accordingly the description following refers by like numbered parts logical units that operate in like manner, it being understood that while one manner of implementation is disclosed the individual ones of the logical operations are well known and various levels of integration thereof are now commercially available.
Thus the transceiver 22 (and 122 ) may be any commercially available receiving-transmitting system tuned tightly to the frequency ff 1 (or ff 2 ) including means for phase, frequency or amplitude modulation and/or demodulation of a logical signal 25 . Signal 25 is passed along one branch through a gate 26 to an address filter 27 , which could be variously implemented and may take the form of a shift register read by a decoder (not shown), and when the code sequence corresponding to the designation of one of the communication units. If the address of the particular unit is decoded in the received bit stream of signal 25 , address decoder 27 then enables an AND gate 29 . The other input to gate 29 is then the same signal 25 . Thus a signal path is opened following an address decode for transferring the succeeding bit burst to a message decoder 30 tied to a display 31 , e.g., a 7 -segment display. In this manner the central station can communicate to the portable unit the address of the machine requiring service, and perhaps the type of service 2 - 5 , or personal attention.
Along the other branch of signal 25 a bidirectional gate configuration is provided comprising gates 36 and 37 , respectively in the transmitting and receiving directions. The receiving gate 37 then passes its output to the input of an EXCLUSIVE OR gate 38 . The selection between gate 26 and gates 36 and 37 is effected by a manual switch 41 on the unit exterior which sets a latch 39 , the Q and Qnot ouputs of the latch then respectively enabling gates 26 and 36 - 37 . Thus the employee assigned the portable unit issues the task completion signal by depressing switch 41 to reconfigured the unit to a data burst transmitter. This data packet, as previously described, may be generated in a data generator 42 and will include the destination address of the central station 11 or 111 , the address of the sending unit and the code corresponding to a completed task. This same data stream is also fed to the other input of gate 38 for comparison, to detect any data collisions or interference, in a manner similar to that earlier described in the patents first disclosing the Ethernet implementation. If a collision is detected, gate 38 enables a clock driven random number generator 44 which delays the retransmission attempt.
By particular reference to FIG. 3, each of the slot or gaming machines M 1 - 1 -M 1 - r and M 2 - 1 -M 2 - s is provided with a transceiver stage 50 tied to a logic unit 60 by way of a data signal. As before, transceiver 50 is tuned tightly to either of the carrier frequencies ff 1 or ff 2 which are separated from each other for optimal rejection of the other by well known techniques associated with tuned circuits. Again like numbered parts functioning in like manner the signal 25 from the transceiver is fed to the EXCLUSIVE OR gate 38 which compares the signal against the output of an encoding stage 242 which collects the outputs of a plurality of photo couplers 251 through 255 corresponding to the earlier described conditions 1 through 5. Within encoder 242 this signal combination is combined with the output of a register 243 in which the destination address (corresponding central station) and the sending address (the numerical designation of the machine) are then side loaded to a shift register 244 for transmission. The output of register 244 is then tied to signal 25 and also to the input of gate 38 to detect data collisions. These are then resolved in a manner earlier described by reference to the clock driven random number generator 44 .
Since each machine is essentially a passive device for the purposes of the instant invention no local need exists for any display or task assignment. Accordingly those functions earlier ascribed to logic operations at gate 29 , encoder 30 and display 31 are not required, nor is there a requirement for any latching function.
By reference to FIG. 4, the first signal in any requesting process is that emitted by transceiver 50 , shown as signal S 50 and comprising a bit sequence for the destination and sending address S 50 A, followed by the fault code 1 - 5 , shown as sequence S 50 D and thereafter the error checking bits S 50 E. As this signal sequence is in the carrier ff 1 (or ff 2 ) all other transceivers defer in response to the suppression signal from the corresponding gates 38 . On completion the carrier is once again idle and each of the gates 38 will then allow its own transmission. As will be shown below, the typical sequence will be from the central station transceiver 12 (or 112 ), shown as signal S 12 , again comprising the address sequence S 12 A, the data sequence S 12 D and error sequence S 12 E. It is this signal that selects a particular portable unit and delivers a data message thereto. Once the task assigned is completed the employee depresses the task completion switch 41 to issue its response signal stream S 41 comprising sequences S 41 A, S 41 D and S 41 E. In each instance the channel is monitored for the presence of other data in the manner earlier described.
This same signal sequence is logically developed in the course of operation of the data processing system 14 (or 114 ), in a logical sequence illustrated in FIG. 5 . In this sequence the slot machine or device M 1 - 1 (or any other machine) issues the service requesting signal S 50 received in step 501 indicating the source of the request and the type of problem. Concurrent therewith the patron may also be making a request shown as a signal sequence PS, received in step 502 . The timing between the signals is then compared in step 503 and if signal PS lags signal S 50 by a selected time increment or less then the sequence is returned to the main branch at step 504 . Otherwise, signal PS returns to the initial step 501 as a separate, unrelated process.
In step 504 the request is identified and a service assignment is then communicated in step 505 , as signal S 12 , to the employee at the bottom of a first-in, first-out stack (FIFO) 511 - 1 - 511 - n , assigned to each grid coordinate. On the completion of the task the employee sends the completion signal S 41 reconciled in step 506 . Then in step 507 a record is made of the service, including the length thereof, and in step 508 the employee is returned back to those available in FIFO stack 511 - 1 - 511 - n . Thereafter the system remains in an idle do-loop shown at step 509 , waiting for the next request signal.
In this manner a single, very narrow bandwidth communication carrier can be used to service contiguous zones which because of its narrow nature is relatively immune to cross-talk or other interference. The same attributes render this system particularly useful for low power, multiple area application.
While the foregoing description illustrates the various data reception and transmission paths by way of holding registers, shift registers and the like, such is illustrative only. Those in the art will appreciate that various serial data transmission and reception devices, at various levels of integration and capacity, are currently available, as for example devices commonly known as U niversal A synchronous R eceiver and T ransmitters [UARTs].
In all the forms illustrated herein the inventive system allows for higher employee productivity, better management information and, most importantly, better customer response. Moreover, good data is available for analysis on the reliability of the various machine types, assisting in the task of quality control.
Since the foregoing system communicates into a single channel, the same task assignment signal directing the employee to a particular casino machine location may also be utilized to display a re-assuring message like “Your request will be serviced in just a few minutes.” In this manner optimal employee use is effected while also maintaining good customer relations.
Obviously, many modifications and variations can be effected without departing from the spirit of the invention disclosed herein. It is therefore intended that the scope of the invention be determined solely by the claims appended hereto.
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A computer assisted process useful in managing the task assignments of a pool of casino employees in accordance with the service requests issued by automated gaming machines either indicating the state of machine operation or the patron's request for attention issued at the machine is enabled with intra-casino communication devices. In accordance with the process the employee pool is fractioned by the type of service skill required, i.e., machine service or patron's requirement for attention, and each employee is assigned a uniquely addressed communication device to which the task assignment is communicated and by which the employee indicates task completion. The employee pool is decremented on each task assignment and incremented on each task completion in a first-in, first-out arrangement in each skill group. In the instances of a large casino facility further division into zones can be made with each zone having its own pool assigned.
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TECHNICAL FIELD
This invention relates generally to capacitance sensitive and proximity responsive electro-mechanical systems and apparatus and more particularly to a body capacitance responsive system and method for protecting the operators of potentially dangerous equipment, such as electrical power saws.
BACKGROUND ART
In the past, certain types of electrical and electro-mechanical equipment have been provided with proximity detectors for controlling the movement of potentially injurious moving parts in response to the approach of a portion of a human body such as a hand or arm. An example of such a proximity detector is disclosed in U.S. Pat. No. 4,453,112 issued to Saver et al, and this proximity detector is operative to stop the motion of automatic automobile windows in response to human body capacitance reaching a predetermined critical distance from a moving window glass. U.S. Pat. No. 4,453,112 is incorporated herein by reference.
However, as presently known, hazardous electrical equipment requiring the presence of an operator in relatively close proximity to potentially dangerous moving parts, such as saw blades, has not been equipped with protective devices for rapidly shutting down the equipment when the operator's hands or arms reach a critically dangerous distance from the moving parts. Where body capacitance-operated proximity sensitive devices have been utilized to control certain types of electrical and electro-mechanical equipment, problems have developed with the inability of these devices to discriminate between human body motion on the one hand and the motion of inanimate objects on the other hand. Thus, the desirability of providing a highly sensitive and discriminating proximity safety device and system for the protection of operators of dangerous equipment is manifest.
DISCLOSURE OF INVENTION
The general purpose and principal object of the present invention is to provide a highly sensitive and discriminating proximity system and method for use with certain types of electro-mechanical equipment, such as electrical power saws. This new and improved body or human capacitance responsive system and method utilizes certain novel circuitry described below which is readily adaptable for use with both fixed blade and movable blade power saw equipment. This object and purpose are accomplished by, among other things:
a. providing an antenna connected to a moving or movable part to be controlled,
b. coupling a tuned circuit to the antenna so that the antenna provides a lumped capacitance parameter within the tuned circuit which is variable in response to an increase in body or human capacitance in close proximity to the antenna,
c applying an RF signal to the tuned circuit, and
d. varying the tuning of the circuit in response to a variation in the lumped capacitance produced by a human being coming within a predetermined critical distance from the moving or movable part.
In this manner, the tuning of the circuit to or near resonance at a certain known point on its transfer gain characteristic in response to a human being coming within a predetermined proximity of the moving or movable part allows a detectable level of RF signal to pass through the tuned circuit. This signal is then processed to in turn activate safety equipment for controlling the motion of the moving part substantially instantaneously.
Another object of this invention is to provide a new and improved method, system, and associated circuitry of the type described which is reliable in operation and readily adaptable for use with fixed blade and moving blade power saw equipment.
Another object of this invention is to provide a new and improved system of the type described which may be economically constructed using existing off-the-shelf electronic components which may be connected by those skilled in the art in a reliable circuit arrangement and variably tuned for different applications.
A further object of this invention is to provide a new and improved method and system of the type described which may be modified for use with various types of potentially dangerous electro-mechanical equipment wherein mechanically moving parts could possibly crush, cut, or otherwise injure a human being.
A further object of this invention is to provide a novel method and system of the type described which may be readily adapted to widely diverse applications such as the proximity sensing of persons entering within a predetermined range of automobile doors and the like. This type of operation could be used, for example, to alert the driver of an automobile of pedestrians entering in close proximity to the automobile and out of the line-of-sight of the driver.
A further object of this invention is to provide a new and improved method and system of the type described which may be modified for use and control of non-dangerous mechanical or electro-mechanical equipment such as door openers, home appliances, robotic equipment, automobile safety equipment and the like.
The above objects, features, and various advantages of this invention will become more fully apparent from the following description of the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a hybrid functional block and schematic electrical diagram of a preferred embodiment for implementing the method and system described herein.
FIG. 2 is a functional block diagram of one implementation of the envelope detector, signal processor and level detector electronics shown in FIG. 1.
FIG. 3 is a graph showing the envelope detector output voltage in FIGS. 1 and 2 versus the equivalent antenna shunt capacitance in picofarads.
FIG. 4 is a schematic circuit diagram for the RF signal source shown functionally in FIGS. 1 and 2.
FIG. 5 is a schematic circuit diagram of part of the signal processing and level detection electronics shown functionally in FIGS. 1 and 2.
FIG. 6 is a schematic circuit diagram of the interlock controller which responds to output signal from the level detection electronics in FIG. 5 to initiate shut down operation for the power saw.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to FIG. 1, there is shown a band pass resistance-inductance-capacitance (RLC) tunable filter circuit 10 which is connected to receive a driving signal from an RF signal source 12 and is further connected as shown through a coaxial cable 14 and an antenna 16 to a saw blade 18. The connection of the coaxial cable 14 to the saw blade 16 may be made either by the use of a slip ring or by the use of parallel plate capacitance coupling using large parallel plates, preferably adjustable in separation distance. The RLC circuit 10 is a 3 pole pi network consisting of a resistance R, and inductance L, a fixed capacitor C 1 and a variable trimming capacitor C 2 connected in the manner indicated to an envelope detector stage 20. The trimming capacitor C 2 together with the shunt capacitance of the coaxial cable 14 and the capacitance of the antenna 16 form a lumped shunt capacitance indicated as C 3 . As described below, this lumped shunt capacitance C 3 also includes and is controlled by the body capacitance of an operator coming within the electromagnetic field of the antenna 16. This body capacitance can be up to ten (10) times greater than wood or other inanimate objects coming within this electromagnetic field. Although the term "electromagnetic field" properly describes the physical coupling of body capacitance to the antenna 16, it is the electrical or "E-field" component of coupling to the parallel plate capacitance of the antenna 16 which has the predominant effect of changing the dynamic capacitance input to the antenna 16 and antenna coupling to the slope tuned network 10 which the present system responds in the manner described below to control shut-off of a saw blade motor or the like.
The envelope detector 20 has its output signal connected by way of line 22 to signal processing electronics 24 described in more detail below, and the output signal from the signal processing electronics stage 24 is connected by way of its output line 26 to a signal level detector stage 28. The output signal from the level detector stage 28 is connected by way of its output line 30 to break and motor control electronics 32 which are described in more detail below with reference to FIG. 2. The break and motor control electronics and the associated breaking mechanism (not shown) to which they are coupled are operative to stop the rotation of the saw blade 18 substantially instantaneously upon receipt of an output detection signal on line 30 from the level detector stage 28.
The trimming capacitor C 2 in the RLC circuit 10 is used to tune this band pass filter network slightly below its point of resonance, and the surface area of the antenna 16 must be sufficient to add the effect of "body capacitance", which is the capacitance added by the presence of the human body within the field of the antenna 16, to the lumped capacitance C 3 . The RLC network 10 is thus alternatively referred to herein as a "slope" tuned network, since it is tuned on the slope of the transfer gain characteristic of this band pass filter network. The RLC network 10 component values are selected to make the transfer gain of the network highly critical to the value of C 3 and thus highly critical to small changes in the field capacitance of the antenna 16. The input resistor R in the RLC network 10 determines the overall linearity in shape of the frequency response curve of this RLC network 10, and larger values of R serve to steepen the slope of the transfer gain characteristic of this network as described below with reference to FIG. 3. Thus, by steepening the slope of this transfer gain characteristic, the network sensitivity to dynamic changes in C 3 is increased.
A careful analysis of the transfer function in FIG. 3 will show that a value of about 680 ohms for resistor R provides a good compromise between RLC network linearity and RLC network sensitivity. This value of resistor R has been used with an inductor L of four (4) microHenrys (μH), a first capacitor C 1 of 360 picofarads (pF) and a second capacitor C 2 of 50 picofarads in the actual reduction to practice of this invention.
The fixed capacitor C 1 serves to control the maximum transfer gain of the RLC filter network 10 at resonance, and has been selected to produce an arbitrary gain of seven (7). Higher gains may be achieved by increasing the value of C 1 and by retuning the trimming capacitor C 2 . However, transfer gains greater than ten (10) can cause the RLC filter network 10 to be too sensitive and thus become unstable. The value of the inductor L is selected to resonate with the lumped capacitance C 3 slightly below the oscillation frequency of the RF source 12, thereby slope tuning the RLC network 10. The lumped capacitance C 3 thus becomes the RLC network parameter for effectively controlling the transfer gain of the network 10, since R, L, and C are fixed in value. Since the RF signal source 12 directly feeds the RLC network 10, the output signal from this network is an amplitude modulated carrier signal which varies in amplitude in response to body capacitance-produced dynamic changes in the capacitance dynamically coupled to the antenna 16.
Generally speaking, the changes in dynamic capacitance at the antenna 16 are proportional to changes which occur at parallel plate capacitors wherein the antenna 16 functions as one capacitor plate and the moving body part serves as the other capacitor plate. The amplitude of the dynamic capacitance signal coupled to the antenna 16 is proportional to A/d, where A is the effective parallel plate area and d is the effective parallel plate separation distance.
Referring now to both FIG. 1 and FIG. 2 wherein like reference numerals indicate identical electronic stages in these two figures, the RF signal source 12 consists of a crystal oscillator 34 and a low pass filter stage and a driver stage 36. The output signal from the driver stage 36 is applied directly to the slope tuned network 10, and the crystal oscillator within stage 34 will typically be tuned to generate a 12 mHz signal. The oscillator in stage 34 is slightly overdriven to generate peak clipping for improved amplitude and frequency stability, and unwanted harmonics are removed from the oscillator signal by the low pass filter connected thereto before being applied to the driver stage 36. The driver stage 36 will typically be a wide band amplifier having low signal distortion, a stable gain, and a sufficiently low output impedance necessary to handle the dynamic load of the RLC network 10. The exact oscillator frequency of the RF source 12 is not critical to the performance of the system and circuitry shown in FIGS. 1 through 6 herein. However, the Federal Communications Commission (FCC) does restrict the electric field intensity at a given distance from a radiating source, which in this instance is the antenna 16 and the saw blade 18 to which it is connected.
The envelope detector 20 is a typical AM detector stage consisting of a half-wave diode detector 38 and a low-pass filter 40 as shown in FIG. 2. The diode detector 38 rectifies the carrier signal applied thereto, and the low-pass filter 40 removes the carrier signal, leaving only the modulation components at its output connection 22. The low-pass filter 40 is typically a pi network of third order Butterworth filtering with an upper frequency cut-off of 10 kHz. The modulation components which pass through the low-pass filter 40 range from DC to a few hundred cycles, and the DC components of the detected envelope result from the "proximity effect" of non-moving objects which are placed near the sensor antenna 16. This effect can be reduced by limiting the low frequency response in the signal processing stage 24, thus allowing minor set-up changes on the power tool 18. Frequency components above DC result from motion of objects in the field of the antenna 16, and all of these components will be negative going with respect to increasing antenna capacitance. This is because the RLC network 10 is tuned on the lower slope of its transfer gain characteristic. The modulation components which are passed through the low-pass filter stage 40 must be positive going for positive level triggering, and as a result of this requirement an inverter stage (not shown) is required in the signal processing electronics 24.
The signal processor 24 includes a DC amplifier 42 and a voltage amplifier 44 of variable gain, and modulation components from the envelope detector 20 are processed in these two stages of gain 42 and 44. The DC amplifier 42 is a difference amplifier which is referenced to 6 volts DC and provides a 10 dB gain and the required signal inversion. By referencing the DC amplifier 42 to 6 volts, this allows a linear operation of the RLC network 10 and also provides an output signal therefrom which is referenced to zero volts DC. By correctly centering the lumped capacitance C 2 with respect to the point of resonance of the RLC circuit 10 and by optimum slope tuning of the RLC network 10, a zero DC offset voltage for the DC amplifier 42 may be obtained. Effects of various objects in the field of the antenna 16 can be determined by measuring the output voltage of the DC amplifier 42.
The second voltage amplifier stage 44 provides an adjustable signal gain up to 40 dB, thereby giving the proximity sensor according to the present invention a pick-up of range up to 12 inches for a human hand approaching the saw blade 18. The second stage 44 of voltage gain limits the low frequency response of the system to about 0.5 Hz, thereby reducing the "proximity effect" described above and allowing a fixed object to be placed near the antenna 16 without triggering the system operation. To maintain full sensitivity in the presence of an object being suddenly removed from the field of the antenna 16, the second stage 44 of voltage gain will track negative DC shifts in the system to thereby maintain an output positive voltage swing only with respect to zero volts DC.
The level detector 28, which is also alternatively identified herein as a comparator in FIG. 2, is a non-inverting operational amplifier using 0.5 volts of hystresis for noise immunity and for setting the trigger point of this detector at about 2.5 volts. The absolute discrimination of materials cannot be achieved through level detection, since the sensitivity of the RLC filter network 10 is also a function of distance of these materials from the antenna 16.
Referring now to FIG. 3, there is shown a graph of the envelope detector output voltage versus the equivalent antenna shunt capacitance in picofarads. This plot was obtained using the above stated values for the various components in the RLC network 10. The transfer gain corresponding to this detector output voltage peaked at about 7dB for a value of C 3 slightly greater than 50 picofarads and then began to taper off gradually as indicated to a gain of between 1 and 2 dB for a value of C 3 of about 52 picofarads. As an example, if the input signal to the slope tuned network 10 is ten (10) volts peak and the network 10 has a gain of eight (8), then a peak voltage of about eighty (80) volts may be chosen as the desired detectable output voltage from the following envelope detector stage 20 as threshold for producing sawblade shutdown in the manner described below. However, in the preferred mode of operation, as objects move into the field of the antenna 16, the network 10 is moved away from resonance, so this action in turn will produce a decrease in voltage output from the network 10. The reason for this is to establish an existing high level threshold voltage above which spurious signals cannot cause the system to function improperly.
The following TABLE A lists the effects of various materials on antenna 16 capacitance and provides a reference for the normalized modulation of human body capacitance versus modulation by the movement of inanimate objects within the field of the antenna 16.
TABLE A______________________________________Effects of Materials on Antenna CapacitanceVarious materials were cut into 4 inch by 6 inch sections toapproximate the dimensions of the human hand. All materialswere .75 inches thick with the exception of the 6062 aluminumwhich was .062 inches thick. Each item was placed one inchfrom the sensing antenna (4 inch face dimension parallel tothe antenna) while the shift in DC voltage at TP-1(wideband test) was measured. NormalizedMaterial Volts Modulation (%)______________________________________Human Hand 5.5 100.0Common WoodsAlder 0.38 6.9Oak 0.38 6.9Particle Board 0.31 5.6Pine 0.34 6.2Redwood 0.32 5.8MetalsAluminum (6062 alloy) 0.89 16.0Other MaterialsStyrofoam 0.02 0.36Plexiglass 0.20 3.6______________________________________
Referring now in sequence to FIGS. 4, 5, and 6, the conventional active and passive component notation is used in these three figures wherein resistors are identified R1, R2, R3, etc., capacitors are identified as C1, C2, C3, etc., inductors are identified as L1, L2, L3, etc., transistors are identified as Q1, Q2, Q3, etc., diodes are identified as D1, D2, D3, etc. Zener diodes are identified as Z1, Z2, etc. and standard off-the-shelf amplifiers are identified as U1, U2, U3, etc. In addition, passive component values for the circuits shown in FIGS. 4, 5, and 6 are listed in TABLE B below, and therefore it is not necessary for those skilled in the art to call out each and every circuit connection in FIGS. 4, 5, and 6 in detail. These circuits are connected exactly as shown in these figures. Instead, the discussion to follow will focus on the more significant functions of the various stages in these figures as they have a bearing on signal processing, signal modification, signal amplifying, signal filtering and other like functions which are all related to providing a detectable level of output signal at the output 30 of the level detector stage 28 in FIGS. 1 and 2 and useful for providing a break and motor control signal to the output break and motor control stage 32.
Returning again to FIG. 4, the oscillator and low pass filter stage 34 includes a 12 megahertz crystal controlled oscillator and transistor stage Q1 connected as shown to a tuned resonant tank circuit including inductor L1 and capacitors C2 and C3. The capacitors C2 and C3 serve as a voltage divider from which an output signal may be derived and applied to base of a buffer amplifier Q2. The output of the buffer amplifier Q2 is connected as shown to the input of a low pass filter stage 35 including the series and parallel connected passive components shown therein. The low pass filter network 35 consist of resistor R9, capacitor C8, inductor L2, and capacitor C5. Since the Pierce oscillator circuit including the transistor Q1 connected as shown is slightly overdriven during normal operation, the low pass filter network 35 serves to remove the harmonics from this signal so that the output signal provided on line 50 is a relatively clean sinewave signal.
The oscillator signal indicator stage 37 is not shown in the functional block diagrams in FIGS. 1 and 2 above and is used merely for the purpose of providing an operation indication at the light emitting diode (LED) 52 which is connected as shown to the output of the transistor Q3. The LED 52 merely gives an indication that the Pierce oscillator circuit in stage 34 is operating properly. Additionally, the LED 52 can be used in tuning the Pierce oscillator circuit of stage 34 including the tunable inductor L1, and the tunable capacitor C3 therein. This is done by varying the intensity of the output of the LED 52 in accordance with the resonant point of the tank circuit consisting of inductor L1 and capacitors C2 and C3.
The output driver stage 36 includes transistors Q4, Q5, and Q6 connected as shown in FIG. 4. The driver stage 36 is connected essentially as a wide band amplifier having a bandwidth of approximately 20 megahertz which may be controlled by varying the value of the inductor L3. The driver stage 36 thus provides a low impedance driving source for the sloped tuned network 10 in FIGS. 1 and 2. Since the impedance of the sloped tuned network 10 is dynamic, it is important that the low output impedance of the driver stage 36 remains substantially constant. This is accomplished using the push pull connection of transistors Q5 and Q6 connected as shown which are driven by the collector output of the input transistor Q4. The diodes D2 and D3 provide the necessary DC offsets within the driver stage 36 so as to minimize the distortion of the output signal appearing on line 56 and applied as an input signal to the sloped tuned network 10. The driver circuit 36 is further stabilized by the DC feedback connection including resistors R13 and R14 connected as shown between the diodes D2 and D3 and the input transistor Q4. The RF output signal on line 56 is typically about eight (8), volts peak, and this signal is applied to the input of the sloped tuned network 10.
Referring now to FIG. 5, the sloped tuned network 10 includes capacitor C10, inductor L4, and capacitor C11. The resistor R21 in FIG. 5 corresponds to the resistor identified as R, of 680 ohms, in FIG. 1; the capacitor C10 corresponds to capacitor C 1 in FIG. 1; the inductor L4 corresponds to the inductor identified as L in FIG. 1; and the variable capacitor C11 corresponds to the variable capacitor C 3 in FIG. 1. The sloped tuned network 10 further includes a varactor diode D6 which is connected to a variable potentiometer 58 to provide the necessary critical tuning of the network 10 in addition to that provided by the variable capacitor C11. The tuning of capacitor C11 is very critical to proper sloped tuned network operation.
The sloped tuned network 10 provides an input signal to the following stage 20 which is the envelope detector stage previously identified functionally in FIGS. 1 and 2 above. The envelope detector 20 includes a diode detector components consisting of D4 and R22 which develops the amplitude detected carrier signal which is applied to the low pass filter 40, and the low pass filter 40 serves to remove the carrier components of the rectified signal. As previously indicated, the low pass filter network 40 consisting of capacitor C12, inductor L5 and capacitor C13 and is a third order Butterworth filter which has a rolloff gain characteristic so that it is about 3 dB down at about 10 kilohertz and thus provides the desired level of input signal to the DC amplifier stage 42.
The signal applied to the DC amplifier stage 42 is coupled through resistor R24 to the operational amplifier U1 which is referenced to approximately 6 volts and provides a zero volt output signal on line 60 when the sloped tuned network 10 is properly tuned to resonance. The output voltage on line 58 from the DC amplifier stage 42 is then applied to the meter amplifier and meter stage 43 including a voltage follower amplifier U1A, which is a unity gain voltage follower amplifier connected as shown to apply signals to a meter 62. The diodes D6, D7 and D8 connected as shown across the meter 62 are for the purpose of protecting the meter 62 from over-voltage when the system starts up. The input signal to the meter amplifier and meter stage 43 is taken from a tunable potentiometer 2 which is used to control the trigger point for the DC amplifier stage 42 and thereby cause triggering to occur, for example, at about a 12 inch separation distance between a human hand or other body part and the sawblade, and down to a much closer separation distance if desired in the range of three to four inches.
The DC amplifier stage 42, which has about 20 dB of gain, feeds its output signal by way of line 64 to the voltage amplifier stage 44. The voltage amplifier stage 44 has a clamping diode D5 connected as shown therein to capacitor C16 and is used for the purpose of stabilizing the voltage across the capacitor C16 when inanimate objects are moved rapidly into an out of the field of the antenna 16 and would thus otherwise tend to cause the capacitor C16 to be driven negatively quite rapidly and thus de-stabilize the voltage amplifier stage 44. If the output signal on line 64 goes negative, then the voltage across capacitor C16 will tend to track this negative going signal, so that when inanimate objects are moved rapidly into and out of the field of the antenna 16 and might otherwise cause undesirable voltage swings across capacitor C16, the clamping diode D5 will clamp this voltage level at a desirable and stable point.
The output signal from the voltage amplifier 44 is connected by way of line 66 and resistor R38 to the positive input terminal of the operational amplifier U3, which is a standard National Semiconductor LM311 type operational amplifier. This amplifier U3 is referenced at its negative terminal to a DC voltage such that the amplifier U3 will trigger on an output signal on line 66 in the range of 2 to 3 volts and thereby generate an output signal on line 68 which is then applied to both the alarm indicator stage 33 and by way of previously identified line 30 to the break and motor control circuitry and electronics 32 previously identified, and including the interlock controller stage shown in FIG. 6.
Referring now to the interlock controller stage shown in FIG. 6, this circuitry consists of an RS flip-flop stage 70 connected to drive brake and motor control logic circuitry 72. The input level detected signal on line 30 is applied as shown to an input transistor Q8 in the RS flip-flop stage 70, and the toggle action of this flip-flop stage 70 is provided by the cross coupled amplifiers U4A and U4B as shown. The transistor Q8 is a logic inverter whose collector output signal is applied to one input of the amplifier U4A. When the RS flip-flop comprising amplifiers U4A and U4B toggles to provide a switching signal on the output conductor 74, the transistor Q9 is switched to conduction to energize the alarm 76 and also to generate an output motor shut down signal on line 78. This signal is applied to the motor relay coil 80 to turn off the motor (not shown) which drives the sawblade 18. Simultaneously, an output signal on line 82 is applied to transistor Q10 and is further coupled through capacitor C23 to the integrated circuit NE555 type timer identified as U5. When the U5 timer is activated, a signal on its output conductor 84 is applied to the base of transistor Q11 to in turn activate the motor brake relay coil 86, thereby activating the brake relay 86 for the time out period of the timer U5.
TABLE B______________________________________Listed herein are the passive component values for thecircuits shown in FIGS. 4, 5, and 6 described above, butthese values are given by way of illustration only and imposeno limitation on the scope of the appended claims. A resistoris designated by "R", capacitor by "C", and inductor by "L". Component Value______________________________________ R1 27K Ω R2 3.3K Ω R3 47 Ω R4 220 Ω R5 10K Ω R6 100 Ω R7 390 Ω R8 1000 Ω R9 68 Ω R10 100K Ω R11 1200 Ω R12 820 Ω R13 24K Ω R14 4.7K Ω R15 5.6K Ω R16 200 Ω R17 180 Ω R18 1500 Ω R19 10 Ω R20 10 Ω R21 680 Ω R22 100K Ω R23 1200 Ω R24 10K Ω R25 10K Ω R26 100K Ω R27 100K Ω R28 5K Ω R29 1000 Ω R30 100K Ω R31 1000 Ω R32 16K Ω R33 56K Ω R34 10K Ω R35 1000 Ω R36 22K Ω R37 7K Ω R38 4.7K Ω R39 820 Ω R41 220 Ω R42 2200 Ω R43 2200 Ω R44 1000 Ω R45 1000 Ω R46 4.7K Ω R47 6.8K Ω R48 1000 Ω R49 91K Ω C1 150 pF C2 150 pF C3 10-40 pF C4 .01 μF C5 82 pF C6 .01 μF C7 .01 μF C8 .01 μF C9 .01 μF C10 36 pF C11 4-20 pF C12 .012 μF C13 .033 μF C15 .001 uF C16 220 μF C17 10 μF C18 47 μF C19 47 μF C20 10 μF C21 .01 μF C22 47 μF C23 5 μF L1 7-14 μH L2 10 μH L3 10 μH L4 3-5 μH L5 15 mH______________________________________
Various modifications may be made in and to the above described embodiment without departing from the spirit and scope of this invention. For example, the various electrical values given above may be varied in accordance with a particular equipment control application, and the operational power and threshold levels and antenna size, shape and connection may also be changed and modified where the operating distance between the operator and equipment under control is increased or decreased. Thus, if for example the system described above were to be adapted for the opening of doors in response to a person approaching a door, the antenna field would have to be greatly increased in order for the RLC circuit 10 to properly respond to a person coming within, for example, three to six feet of the door.
In addition, the present invention may be used in combination with and control for other systems such as those used in meat chopping, metal buffing, and other heavy duty construction applications by the judicious selection of component values and tuning in accordance with the teachings provided herein. Also, as previously indicated, if the above described system is to be adapted for use with control systems for controlling equipment located twenty to thirty feet or more from an approaching human being, then the output power from the RF source 12 must be increased substantially and the effective "parallel plate" area of coupling to the antenna 16 must also be increased substantially. In addition, materials selection for parallel plate antenna materials will become important in these types of long range dynamic capacitance operations, and it may in some instances be desirable to use a plurality of directionally oriented antennas to give varying sensitivities to persons entering, say, from angular or side directions to an apparatus being controlled as opposed to a person entering head-on through a capacitance sensitive door or the like.
Accordingly, the above circuit, system and method variations which are within the skill of this art are clearly within the scope of my following appended claims.
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A method and system and associated circuitry for controlling and stopping the motion of dangerous moving parts such as power saw blades substantially instantaneously in response to body or human capacitance produced by an operator coming with a predetermined critical distance from the moving part. This method includes, and this system provides for, among other things, connecting an antenna to the moving part and then coupling a tunable circuit to the antenna so that the antenna provides a variable lumped capacitance parameter (dependent upon human body capacitance) within the tunable circuit. This lumped capacitance parameter is variable in response to body or human capacitance produced when an operator comes within a predetermined critical proximity to the moving part. This variation in lumped capacitance serves to tune the circuit at or near a point of resonance to thereby enable an RF signal to pass through the tunable circuit at a detectable level which is subsequently processed to activate safety equipment for controlling and stopping the motion of the moving part substantially instantaneously. This invention is also adaptable for use with non-dangerous mechanical apparatus such as automatic door openers, automatic robot equipment, and capacitance-sensitive lighting appliances, and the like. It is also adaptable for use on automobile safety equipment, such as the proximity sensing of persons approaching an automobile out of the normal line-of-sight vision angles of the driver.
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[0001] This is a Continuation-in-Part Application of International Application No. PCT/JP02/00986 filed Feb. 6, 2002, incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to crystalline forms of a pyrimidine nucleoside derivative which exhibit excellent anti-tumour activity; to a pharmaceutical composition (preferably an anti-tumour agent) containing said crystalline form as an active ingredient; to the use of said crystalline form in the preparation of said pharmaceutical composition; and to a method for prevention or treatment of disease (preferably tumour) which comprises administering to a warm blooded animal (preferably a human) in need of such prevention or treatment a pharmacologically effective amount of said crystalline form.
[0003] [Background of the Invention]
[0004] The pyrimidine nucleoside derivative of formula (I) (hereinafter referred to as Compound (I)) has been disclosed in Japanese Patent No. 2569251 and U.S. Pat. No. 5,691,319. As described therein, compound (I) exhibits excellent anti-tumour activity and is expected to become an agent for treatment or prevention of tumours. To make Compound (I) more practical for use as a medicament, better storage stability, ease of handling and the like is required.
BRIEF DESCRIPTIONS OF THE INVENTION
[0005] The inventors have studied the stability and the like of Compound (I) and have succeeded in obtaining crystals of Compound (I). These crystals have remarkably better storage stability and ease of handling than a powder of Compound (I) as obtained in example 1 disclosed in Japanese Patent No. 2569251 and U.S. Pat. No. 5,691,319. These crystals exhibit an excellent pharmacokinetic profile such as oral absorption and the like and are, therefore, practically useful medicaments as described in U.S. Pat. No. 5,691,319 (incorporated herein by reference).
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] [0006]FIG. 1 is a powder X ray diffraction pattern of the crystalline product prepared in Example 1, the diffraction pattern of which is obtained by irradiation of the crystalline product using the copper Kα ray (wavelength λ=1.54 angstrom).
[0007] [0007]FIG. 2 is a powder X ray diffraction pattern of the crystalline product prepared in Example 2, the diffraction pattern of which is obtained by irradiation of the crystalline product using the copper Kα ray (wavelength λ=1.54 angstrom).
[0008] [0008]FIG. 3 is a powder X ray diffraction pattern of the crystalline product prepared in Example 3, the diffraction pattern of which is obtained by irradiation of the crystalline product using the copper Kα ray (wavelength λ=1.54 angstrom).
[0009] [0009]FIG. 4 is a powder X ray diffraction pattern of the crystalline product prepared in Example 4, the diffraction pattern of which is obtained by irradiation of the crystalline product using the copper Kα ray (wavelength λ=1.54 angstrom).
[0010] In addition, in these figures the vertical axis of each powder X ray diffraction pattern indicates the diffraction intensity in units of counts/second (cps) and the horizontal axis indicates the diffraction angle as the value 20.
DETAILED DESCRIPTION OF THE INVENTION
[0011] According to the invention there is provided:
[0012] (1) a crystalline form of a compound of formula (I),
[0013] (2) a crystalline form according to (1) wherein the compound of formula (I) is a hydrate,
[0014] (3) a crystalline form according to (1) or (2) wherein said crystalline form has main peaks at lattice distances of 19.53, 13.03, 9.75, 4.17, 4.00, 3.82, 3.68 and 3.41 angstroms determined by X-ray diffraction by the powder method using the copper Kα ray (wavelength λ=1.54 angstroms),
[0015] (4) a crystalline form according to (1) or (2) wherein said crystalline form has main peaks at lattice distances of 19.36, 12.87, 9.63, 4.70, 4.64, 4.28, 4.10, 3.92, 3.77 and 3.48 angstroms determined by X-ray diffraction by the powder method using the copper Kα ray (wavelength λ=1.54 angstroms),
[0016] (5) a crystalline form according to (1) or (2) wherein said crystalline form has main peaks at lattice distances of 19.62, 13.06, 9.82, 4.72, 4.63, 4.56, 4.15, 3.98, 3.93, 3.82, 3.45 and 3.40 angstroms determined by X-ray diffraction by the powder method using the copper Kα ray (wavelength λ=1.54 angstroms),
[0017] (6) a crystalline form according to (1) or (2) wherein said crystalline form has peaks at lattice distances of 22.52, 5.17, 4.60, 4.28, and 3.87 angstroms determined by X-ray diffraction by the powder method using the copper Kα ray (wavelength λ=1.54 angstroms),
[0018] (7) a pharmaceutical composition containing a crystalline form according to any one of (1) to (6) as an active ingredient,
[0019] (8) a pharmaceutical composition according to (7) for prevention or treatment of tumours,
[0020] (9) the use of a crystalline form according to any one of (1) to (6) in the preparation of a pharmaceutical composition,
[0021] (10) the use according to (9) wherein the pharmaceutical composition is for the prevention or treatment of tumours,
[0022] (11) a method for the prevention or treatment of disease comprising administering a pharmacologically effective amount of a crystalline form according to any one of (1) to (6) to a warm blooded animal in need of such prevention or treatment,
[0023] (12) a method according to (11) wherein the disease is a tumour,
[0024] (13) a method according to (11) or (12) wherein the warm blooded animal is a human.
[0025] The crystalline form of Compound (I) in the present invention is a solid which has a regular repeated arrangement of atoms (or groups of atoms) in a three-dimensional structure. The crystal is different from an amorphous solid that has no regular arrangement of atoms in a three-dimensional structure.
[0026] In general, different plural crystalline forms (polymorphism) of the same compound can be produced depending upon the crystallization conditions used. These different crystalline forms have different three-dimensional structures and have different physicochemical properties.
[0027] The present invention encompasses individual crystalline forms and mixtures of two or more of said crystalline forms.
[0028] Crystalline forms of Compound (I) include, for example:
[0029] a crystal having main peaks at lattice distances of d=19.53, 13.03, 9.75, 4.17, 4.00, 3.82, 3.68 and 3.41 angstrom determined by X-ray diffraction by the powder method using the copper Kα a ray (wavelength λ=1.54 angstrom) wherein the main peaks have relative diffraction intensities greater than 36 based on the relative intensity 100 of the peak at lattice distance d=9.75 angstrom;
[0030] (In addition, the lattice distance d can be calculated on the basis of the equation of 2d sin θ=nλ (n=1).)
[0031] a crystal having main peaks at lattice distances of d=19.36, 12.87, 9.63, 4.70, 4.64, 4.28, 4.10, 3.92, 3.77 and 3.48 angstrom determined by X-ray diffraction by the powder method using the copper Kα ray (wavelength λ=1.54 angstrom) wherein the main peaks have relative diffraction intensities greater than 53 based on the relative intensity 100 of the peak at lattice distance d=3.92 angstrom;
[0032] a crystal having main peaks at lattice distances of d=19.62, 13.06, 9.82, 4.72, 4.63, 4.56, 4.15, 3.98, 3.93, 3.82, 3.45 and 3.40 angstrom determined by X-ray diffraction by the powder method using the copper Kα ray (wavelength λ=1.54 angstrom) wherein the main peaks have relative diffraction intensities greater than 30 based on the relative intensity 100 of the peak at lattice distance d=4.56 angstrom; and
[0033] a crystal having peaks at lattice distances of d=22.52, 5.17, 4.60, 4.28, and 3.87 angstrom determined by X-ray diffraction by the powder method using the copper Kα ray (wavelength λ=1.54 angstrom) wherein the main peaks have relative diffraction intensities greater than 36 based on the relative intensity 100 of the peak at lattice distance d=22.52 angstrom.
[0034] When the crystalline forms of Compound (I) are allowed to stand so that they are open to the atmosphere or are mixed with water or a solvent, they may absorb water or a solvent to form a hydrate or solvate. The present invention encompasses these hydrates and solvates
[0035] The compound (I) can be prepared according to a similar procedure to that described in the specification of Japanese Patent No. 2569251 and in U.S. Pat. No. 5,691,319.
[0036] The crystalline forms of Compound (I) can be obtained from a supersaturated solution. The supersaturated solution can be prepared through dissolution of Compound (I) in an appropriate solvent, pH adjustment of said solution, concentration of said solution, cooling said solution, addition of a solvent in which Compound (I) is slightly soluble to a solution of Compound (I) in a solvent in which Compound (I) is readily soluble, or the like.
[0037] A suspension of a crystal or amorphous solid of Compound (I) in an appropriate solvent is converted into a slurry and then is stirred to transform alternate crystal (solvent-mediated transformation).
[0038] In addition, precipitation of the crystals takes place spontaneously in the reaction vessel or it can be started or accelerated by addition of a crystalline seed, by mechanical stimulation such as through use of ultrasonic waves or by stretching the inside of the reaction vessel.
[0039] The temperature for crystallization of Compound (I) or a pharmacologically acceptable salt thereof is usually in the range between 0 and 60° C., preferably between 5 and 45° C.
[0040] Precipitated crystals can be collected by filtration, centrifugation or decantation methods. Isolated crystals may be washed with an appropriate solvent. The washing solvent can include, for example, water; an alcohol such as ethanol, isopropanol; a ketone such as acetone; an ester such as methyl formate, ethyl formate, methyl acetate, ethyl acetate; an aromatic hydrocarbon such as toluene, xylene; a nitrile such as acetonitrile; an ether such as diethyl ether, tetrahydrofuran, or a mixture thereof. Preferably methyl acetate which contains water or is anhydrous is used.
[0041] Isolated crystals can be dried between 10 and 100° C., preferably between 30 and 50° C. until the weight of said crystals becomes constant, if necessary, in the presence of a drying agent such as silica gel or calcium chloride and under reduced pressure.
[0042] Dried crystals may absorb water under condition of 20 to 90% relative humidity and between 10 and 30° C., preferably 50 to 80% relative humidity and between 20 and 30° C. until the weight of said crystals becomes constant.
[0043] Crystals thus obtained can be further purified by recrystallization or slurry-purification.
[0044] The recrystallization is accomplished by techniques known to those skilled in the art such as (1) cooling method: Compound (I) or a pharmacologically acceptable salt is dissolved in a hot solvent and then the resulting solution is cooled, (2) concentration method: a solution of Compound (I) or a pharmacologically acceptable salt thereof is concentrated, (3) precipitation method: a solvent in which Compound (I) or a pharmacologically acceptable salt thereof is slightly soluble is added to a solution of Compound (I) or a pharmacologically acceptable salt thereof in a solvent in which Compound (I) or a pharmacologically acceptable salt is readily soluble.
[0045] The slurry-purification comprises collection of crystals which are obtained by stirring a suspension of a certain compound in an appropriate solvent.
[0046] The solvent employed in slurry-purification of Compound (I) includes, for example, a ketone such as acetone, methyl ethyl ketone; an ester such as methyl acetate, ethyl acetate; a nitrile such as acetonitrile; a halogenated hydrocarbon such as methylene chloride, chloroform; an aromatic hydrocarbon such as toluene, xylene; an alcohol such as ethanol, isopropanol; an ether such as diethyl ether, tetrahydrofuran; an amide such as N,N-dimethylformamide; water; an aliphatic hydrocarbon such as hexane; an ether such as diisopropyl ether, diethyl ether; or the like and a mixture thereof. Preferably a ketone such as acetone, methyl ethyl ketone; an ester such as methyl formate, ethyl formate, methyl acetate, ethyl acetate; a nitrile such as acetonitrile; an alcohol such as ethanol, isopropanol and these solvents containing water is used, and more preferably methyl acetate which contains water or is anhydrous.
[0047] Crystals obtained by recrystallization and slurry-purification are also isolated by similar techniques to those described hereinbefore.
[0048] When crystalline forms of Compound (I) are used as a medicament preferably as an agent for treatment or prevention of tumours (as described in U.S. Pat. No. 5,691,319), said crystalline forms can be administered alone or as a mixture of said crystalline form with an appropriate pharmacologically acceptable excipient(s), and/or diluent(s). Compositions according to the present invention can be in unit dosage form such as tablets, capsules, granules, powders, syrups, injections, ointments, solutions, suspensions, aerosols, troches or the like for oral or parenteral administration.
[0049] The pharmaceutical compositions can be prepared in a known manner by using additives such as excipients, binding agents, disintegrating agents, lubricating agents, stabilizing agents, corrigents, suspending agents, diluents and solvents.
[0050] An example of an excipient includes a sugar derivative such as lactose, sucrose, glucose, mannitol, or sorbitol; a starch derivative such as corn starch, potato starch, α-starch, dextrin, carboxy methylstarch; a cellulose derivative such as crystalline cellulose, low-substituted hydroxypropylcellulose, hydroxypropylmethylcellulose, carboxymethylcellulose, calcium carboxymethylcellulose, internal-cross-linked sodium carboxymethylcellulose; acacia; dextran; pullulan; a silicate derivative such as light silicic acid anhydride, synthetic aluminum silicate, magnesium aluminate metasilicate; a phosphate derivative such as calcium phosphate; a carbonate derivative such as calcium carbonate; a sulfate derivative such as calcium sulfate; or the like.
[0051] An example of a binding agent includes an excipient described hereinbefore; gelatin; polyvinylpyrrolidone; macrogol; or the like.
[0052] An example of a disintegrating agent includes an excipient described hereinbefore, a chemically modified starch or cellulose derivative such as sodium cross-carmellose, sodium carboxymethylstarch, cross-linked polyvinylpyrrolidone or the like.
[0053] An example of a lubricating agent includes talc; stearic acid; a metal stearate derivative such as calcium stearate, magnesium stearate; colloidal silica; veegum; a wax such as beeswax or spermaceti; boric acid; a glycol; a carboxy acid derivative such as fumaric acid, adipic acid; a sodium carboxylate such as sodium benzoate; a sulfate such as sodium sulfate; leucine; a lauryl sulfate such as sodium lauryl sulfate, or magnesium lauryl sulfate; a silicic acid derivative such as silicic acid anhydride, silicic acid hydrate; a starch derivative described above as an excipient; or the like.
[0054] An example of a stabilizing agent includes a para-hydroxybenzoic acid ester derivative such as methylparabene, propylparabene; an alcohol derivative such as chlorobutanol, benzyl alcohol, phenethyl alcohol; benzalkonium chloride; a phenol derivative such as phenol, cresol; thimerosal; acetic anhydride; sorbic acid; or the like.
[0055] An example of a corrigent includes a sweetening, souring, and flavoring agents or the like all of which are ordinarily used.
[0056] An example of a solvent includes water, ethanol, glycerin or the like.
[0057] The dose of the crystalline form of compound (I) will depend on such factors as symptom, body weight and age of the patient. A suitable dosage level for an adult human patient is 0.1 mg (preferably 1 mg) per day to 100 mg (preferably 50 mg) per day. The crystalline form of the compound of formula (I) can be administered as either a single unit dosage, or if desired, the dosage may be divided into convenient subunits administered at one to several times throughout the day depending on the symptoms of the patient.
EXAMPLES
[0058] The present invention is further described by Examples. Test examples and Formulation examples.
Example 1
[0059] Crystal B
[0060] (a) To 2′-cyano-2′-deoxy-N 4 -palmitoyl-1-β-D-arabinofuranosylcytosine (30 g), which is the compound described in Example 1 (1d) of the Japanese Patent No. 2569251 (or U.S. Pat. No. 5,691,319), was added methyl acetate containing water at 2.5 vol % (300 ml), and the resulting mixture was heated up to approximately 55° C. to prepare a clear solution. Subsequently, the solution was cooled to 5° C. at a rate of approximately 0.5° C. per minute. Upon cooling to about 45° C. in the course of the cooling, plate crystals were separated out of solution. After stirring furthermore at 5° C. for 20 min, the separated crystals were collected by filtration and washed with methyl acetate containing water at 2.5 vol % (30 ml) to afford the desired crystal B (28.78 g, purity 97.9%) in a 96.0% [N/N] yield.
[0061] (b) To 2′-cyano-2′-deoxy-N 4 -palmitoyl-1-β-D-arabinofuranosylcytosine (8.7 kg), which is the compound described in Example 1 (1d) of the Japanese Patent No. 2569251 (or U.S. Pat. No. 5,691,319), was added methyl acetate containing water at 1.9 vol % (80 L), and the resulting mixture was stirred at approximately 23° C. for 1.5 hr. The separated crystals were collected by filtration, washed with methyl acetate containing water at 1.9 vol % (20 L) and dried to afford the desired crystal B (7.7 kg, purity 97.3%) in a 90.1% [N/N] yield.
Example 2
[0062] Crystal C
[0063] (a) To 2′-cyano-2′-deoxy-N 4 -palmitoyl-1-β-D-arabinofuranosylcytosine (30 g), which is the compound described in Example 1 (1d) of the Japanese Patent No. 2569251 (or U.S. Pat. No. 5,691,319), was added methyl acetate containing water at 4 vol % (600 ml), and the resulting mixture was heated up to approximately 50° C. to prepare a clear solution. Subsequently, the solution was cooled to 40° C. at a rate of approximately 0.5° C. per minute and stirred. In the course of the stirring, crystal B was first separated out of solution and then transformed gradually into needle-like crystals. After stirring furthermore at 40° C. for 60 min, the solution was cooled to 25° C. at a rate of approximately 0.5° C. per minute. After stirring at 25° C. for 60 min, the separated crystals were collected by filtration and washed with methyl acetate containing water at 4 vol % (30 ml) to afford the desired crystal C (23.74 g, purity 98.5%) in a 79.7% [N/N] yield.
[0064] (b) To 2′-cyano-2′-deoxy-N 4 -palmitoyl-1-β-D-arabinofuranosylcytosine (60 g), which is the compound described in Example 1 (1d) of the Japanese Patent No. 2569251 (or U.S. Pat. No. 5,691,319), was added methyl acetate containing water at 2.5 vol %(600 ml), and the resulting mixture was stirred at about 23° C. for 2 hr and then cooled to 12° C. at a rate of approximately 0.5° C. per minute. After stirring at 12° C. for 1 hr, the separated crystals were collected by filtration, washed with methyl acetate containing water at 2.5 vol % (180 ml) and dried to afford the desired crystal C (55.1 g, purity 94.5%) in a 89.6% [N/N] yield.
Example 3
[0065] Crystal C(I)
[0066] 1) The dried crystal C was kept standing for about 20 min under an atmosphere moistened to more than 45% humidity to afford the desired crystal C(I).
[0067] 2) To the dried crystal C was added water to an amount which corresponds to about 33 wt % of the used crystal, and the resulting mixture was kneaded for 3 min to afford the desired crystal C(I).
Example 4
[0068] Crystal D
[0069] (a) To 2′-cyano-2′-deoxy-N 4 -palmitoyl-1-β-D-arabinofuranosylcytosine (10.0 g), which is the compound described in Example 1 (1d) of the Japanese Patent No. 2569251 (or U.S. Pat. No. 5,691,319), was added anhydrous methyl acetate (400 ml), and the resulting mixture was heated up to approximately 60° C. to prepare a clear solution. Subsequently, the solution was cooled to 25° C. at a rate of approximately 0.5° C. per minute. Upon cooling to about 43° C. in the course of the cooling, crystals were separated out of solution. After cooling to 25° C., the separated crystals were collected by filtration to afford the desired crystal D (8.8 g, 88.4% yield).
[0070] (b) To 2′-cyano-2′-deoxy-N 4 -palmitoyl-1-β-D-arabinofuranosylcytosine (50 g), which is the compound described in Example 1 (1d) of the Japanese Patent No. 2569251 (or U.S. Pat. No. 5,691,319), was added methyl acetate (1500 ml), and the resulting mixture was heated up to approximately 50° C. and stirred at about 50° C. for 1 hr. Subsequently, the solution was cooled to 40° C. at a rate of approximately 0.5° C. per minute. After stirring at 40° C. for 30 min, the separated crystals were collected by filtration and dried to afford the desired crystal D (37.0 g, purity 99.2%) in a 74.2% [N/N] yield.
Test Example 1
Stability Test
[0071] In the stability test, crystals B, C and D of the present invention prepared in Examples 1, 2 and 4, respectively and the amorphous powder (Amorphous A) of compound of general formula (I) described in Example 1 (1d) of the Japanese Patent No. 2569251 were used as reference. These compounds were placed in stoppered vessels separately and stored at 60° C. under a nitrogen atmosphere for 17 days, and the content of these compounds was measured on 5, 10 and 17 days after the initiation of the storage.
[0072] The content of these compounds was determined quantitatively with high performance liquid chromatography (HPLC), and the rate of the remaining compounds (%) was calculated by the content of Compound (I) determined at each sampling point based on the initial content (100%) determined immediately before the storage.
[0073] The operating conditions of HPLC were as follows:
Column: L-column ODS (4.6 mm × 250 mm) (Chemicals Inspection and Testing Institute) Mobile Acetonitrile:water:acetic acid = 750:250:1 phase: Flow rate: 1.0 ml/min Detection 249 nm wavelength: Column 40° C. temperature:
[0074] [0074] TABLE 1 Stability of each compound at 60° C, under a nitrogen atmosphere (Residual rate) Days after the initiation of stability test Compound 5 days 10 days 17 days Amorphous A 92.7% 78.6% 62.5% Crystal B prepared in 101.0% 100.3% 100.4% Example 1 Crystal C prepared in 101.0% 100.4% 100.1% Example 2 Crystal D prepared in 99.9% 98.3% 98.4% Example 4
[0075] Based on the results summarized in Table 1, the stability of the amorphous powder (amorphous A) of compound (I) at 60° C. under a nitrogen atmosphere was extremely low, and the residual rate decreased to 62.5% after storage for 17 days. By contrast, the residual rates of crystals B and C prepared in Example 1 and 2, respectively, under the same storage conditions were 100% each and that of the crystal D prepared in Example 4 was 98.4%, demonstrating that the stability of crystals of the present invention is extremely high.
Formulation Example 1
Solution 1
[0076] A solution is prepared so that said solution contains the compound prepared in Example 1 (10%(w/W)), benzalkonium chloride (0.04%(W/W)), phenethyl alcohol (0.04%(W/W)) and purified water (89.56%(W/W)).
Formulation Example 2
Solution 2
[0077] A solution is prepared so that said solution contains the compound prepared in Example 1 (10%(W/W)), benzalkonium chloride (0.04%(W/W)), propylene glycol (30%(W/W)) and purified water (39.96%(W/W)).
Formulation Example 3
Powder
[0078] A powder is prepared so that said powder contains the compound prepared in Example 1 (40%(W/W)) and lactose (60%(W/W)).
Formulation Example 4
Aerosol
[0079] An aerosol is prepared so that said aerosol contains the compound prepared in Example 1 (10%(W/W)), lecithin (0.5%(W/W)), fulon 11 (34.5%(W/W)) and fulon 12 (55%(W/W)).
[0080] The crystalline forms of this invention have remarkably better storage stability and ease of handling than the amorphous powder of Compound (I). Said crystalline forms exhibit excellent metabolic disposition such as oral absorption and the like and are, therefore, useful medicaments (preferably as agents for treatment or prevention of tumours).
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The present invention provides crystalline forms and compositions thereof, of a pyrimidine nucleoside derivative of formula (I) having anti-tumour activity, wherein formula (I) is:
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FIELD OF THE INVENTION
The present invention relates to tapes or narrow fabrics used for gasketing, insulating, padding, sealing, and the like, and has particular application to fabrics made of fiberglass and similar filamentary material which has properties particularly suited to the desired end use.
BACKGROUND OF THE INVENTION
In the past, asbestos has been the principal material used for heat insulation and sealing where the material is subjected to elevated temperatures. Asbestos fibers are plentiful and are readily combined into laps, roving, and yarn for various end uses by conventional textile apparatus. Asbestos materials tend to flake or slough off fibers unless specially treated, but such tendency has not been a significant deterrent to the use of asbestos because of its abundant supply and relative ease of handling in manufacturing.
In recent years, fiberglass has been developed as a substitute for asbestos where the coarseness of the asbestos material is unsuitable for the end use and where the fine filamentary characteristics of fiberglass provide properties which justify the normally higher cost of substituting fiberglass for asbestos.
A significant advantage of fiberglass is that it has considerable tensile strength in comparison to asbestos and in continuous-filament fiberglass products, the fiberglass tensile strength is relatively independent of the degree of twist in the fiberglass strands so that fiberglass may be fabricated with a looser or less compact fibrous structure.
SUMMARY OF THE INVENTION
With the foregoing in mind, the present invention provides an improved fabric which is produced in a highly efficient operation and yet which has characteristics which are comparable to or are improvements over the characteristics of fabrics formed with less expensive material by conventional techniques.
More specifically, the present invention provides an improved narrow fabric in which the fabric has high widthwise dimensional stability with a reasonable degree of lengthwise extensibility which permits the fabric to be formed around corners without sacrificing its flat characteristics.
The fabric of the present invention exhibits substantial heat-insulating characteristics which enables it to be used as a spacer element between components having different temperatures.
The present invention also provides a fabric element which has a degree of porosity which inhibits direct airflow through the fabric yet which permits limited breathing to avoid explosive containment.
The present invention provides a highly economical and effective procedure for fabricating fiberglass material into composite fabrics having substantial bulk and high density to enhance the utility of such fabrics in gasketing, insulating, padding, sealing and similar uses.
More specifically, the present invention provides a composite fabric consisting of a plurality of tubular-knitted components which are joined in side-by-side juxtaposed relation by seams, the dimensions of the components being such as to provide dimensional stability to the fabric in a widthwise direction while affording limited extensibility lengthwise.
DESCRIPTION OF THE DRAWING
All of the objects of the invention are more fully set forth hereinafter with reference to the accompanying drawing, wherein:
FIG. 1 is a diagrammatic illustration of a composite fabric embodying the present invention;
FIG. 2 is a diagrammatic transverse section view taken through the fabric of FIG. 1;
FIG. 3 is a schematic illustration of the stitch pattern embodied in the tubular fabric components of the present invention, the tubular fabric being split and opened out to facilitate the illustration of the stitch pattern;
FIG. 4 is a diagrammatic view similar to FIG. 1 illustrating another embodiment of the present invention;
FIG. 5 is a diagrammatic transverse sectional view taken through the fabric of FIG. 4; and
FIG. 6 is a schematic block diagram illustrating the method embodied in the production of a composite fabric in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawing, FIG. 1 diagrams a composite fabric made in accordance with the present invention. In the embodiment of FIG. 1, the composite fabric 10 is made up of four individual fabric components designated 11, 12, 13 and 14 respectively in FIG. 1. The components are positioned side-by-side and are interconnected by seams 15, 16 and 17 extending along the line of junction between the juxtaposed components. The components are of indeterminate lengths so that the illustration in FIG. 1 represents a typical segment of a continuous length of composite fabric. As shown, the width of the composite fabric 10 is equal to the sum of the width of the individual components 11, 12, 13 and 14.
In accordance with the present invention, each of the components is a tubular knit fabric and as shown in FIG. 2, the flattened fabric has an ovate cross section which closes the interior bore of the tubular fabric so that the interior surface at one side of the tubular component is in engagement with the interior surface at the opposite side. As indicated in FIGS. 1 and 2, each of the seams 15, 16 and 17 consists of a zigzag line of stitching which, in the present instance, is made by a chain-stitch sewing machine which produces a double line of stitching at the looper side of the fabric and a single line of thread at the needle side of the fabric. The zigzag sewing machine operates in a fashion that the needle alternately penetrates the edge portions of the juxtaposed fabric components as they travel past the needle in side-by-side relation thereby causing the stitch segments of the seam to be disposed diagonally alternately in opposite directions along the length of the junction line between the two components. The seams not only provide a secure interconnection between the components, but also permit the components to extend longitudinally while sewn together.
The use of tubular knit fabric components provides a firm self-edge when the components are flattened which enhances the interconnection of the components by the stitches of the seams. Furthermore, the outer edges of the composite fabric 10 are also provided with a firm self-edge. The self-edge formed by the flattened tubular knit fabric components is formed without the extra threads or different warp manipulation which is required in the selvage of woven fabrics. In the present instance, the self-edge is obtained by the simple expedient of flattening the tubular knit fabric.
A desirable characteristic of tubular knit fabric for the present purpose is its inherent characteristic of having limited widthwise extensibility while exhibiting substantial lengthwise extensibility. The lengthwise extension of the fabric tends to contract it widthwise but the close-knitted stitch formation in the tubular knit fabric of the present invention inhibits the lateral extension of the fabric component.
In accordance with another feature of the present invention, the knitted tubular components of the composite fabric are knitted compactly with a non-run stitch which enhances the dimensional stability and durability of the knitted product. To this end, the fabric components are each knitted on a knitter-braider manufactured by the Lamb Knitting Machine Corporation of Chicapee, Mass. This knitter-braider is a circular warp knitter having a circle of knitting needles mounted in a cylinder for vertical displacement between a stitch feed and a stitch draw position. Each needle has associated with it a feeder which is capable of feeding strand material to the needles from a creel or other fixed supply source. The needle cylinder is hollow to permit withdrawal of the knitted tube from the machine downwardly through the center of the cylinder, the needles being positioned externally of the cylinder so that the top of the cylinder serves to cast the previously-knitted loop from the needle as it is pressed downwardly to the stitch-draw level.
The yarn feeders reciprocate transversely between two needle stations in timed relation to the vertical reciprocation of the needles so that each feeder deposits a strand into the hook of the needle in the yarn feed position, on one needle at the first station in a first course and then on the other needle at the other station in the subsequent course. As the needle draws a stitch, it casts the stitch formed previously from an alternate yarn. In this fashion, the stitches in any given needle wale alternate between two feeds, the loops of the one strand alternating with the loops of the other strand. The strand forming the alternate loops form loops on the needles in a wale on one side of the given needle wale, while the intermediate loops are being formed on the needle in the given wale. Likewise, when the alternate loops are being formed on the needle in the given wale, the strand forming the intermediate loops are forming loops in a wale on the other side of the given wale.
FIG. 3 diagrams the stitch pattern produced by the knitter-braider when the feeder reciprocates between adjacent wales. In the illustration, four needle wales are illustrated, designated 21, 22, 23 and 24, respectively. With reference to the needle wale 22, it is noted that the strand 25 forms alternate needle loops 26 in the wale 22 and also forms intermediate needle loops 27 in the wale 21. A second strand 28 forms intermediate needle loops 29 in the wale 22 as the strand 25 forms the loops 27 in the wale 21. When the strand 25 forms the loops 26 in wale 22, the strand 28 forms loops 30 in the wale 23 on the opposite side of the wale 22 from the wale 21. The bight of the needle loops is shown in double lines in FIG. 3 to indicate that they appear on the same surface of the fabric as the stitch connectors extending diagonally between the needle loops, which are also shown in double lines. The single line portions of the needle loops shown in FIG. 3 appear on the reverse face of the fabric. In the preferred embodiment of the invention, the Lamb knitter-braider is a four-needle machine which forms four needle wales spaced circumferentially about the tubular fabric. With reference to FIG. 3, the tubular fabric produced by the knitter-braider has only four wales 21, 22, 23 and 24, the wale 24 being formed adjacent the wale 21 to make a continuous tubular fabric.
On the knitting machine, the non-run stitch pattern is obscured because of the tension applied to the strand during the knitting operation. The tension on the strand causes the knitted loops to assume angular positions in which the bases of the loops 26 and 30 are canted toward the left relative to the bights thereof and the bases of the loops 27 and 29 are canted toward the right relative to their bights. The overall effect of this structure is to produce a tubular knit fabric having an appearance of a braid. The alternation of the strands between the adjacent wales provides a non-run stitch pattern similar to the standard tricot stitch of the flat tricot machine.
The knitter-braider may also be adjusted to reciprocate the feeder between spaced-apart wales. For example in a machine with four needle stations, one feeder may reciprocate between stations 1 and 3, a second feeder may reciprocate between stations 2 and 4, a third between stations 3 and 1, and a fourth between stations 4 and 2. With this adjustment, the machine produces a tubular fabric having an appearance more like a knitted tube than like a braid, and the stitch connectors extend across the core of the fabric and tend to fill it up.
With either adjustment, the knitter-braider apparatus is particularly effective for use in the present invention since the machine is capable of knitting a wide variety of strand material which may vary in bulk from a fine thread to a bulky sliver or roving. Fiberglass roving is a bundle of fiberglass filaments which are assembled into a strand of considerable tensile strength without substantial twisting. For the purpose of the present invention where a bulky fabric is desired, it has been found that a fiberglass roving is particularly effective to provide the desired bulk. Since each feed mechanism of the knitter-braider operates in association with only two needle stations by arcuate oscillation between the two stations, the feeder may be fed from a stationary source without entanglement from strands being fed to other feed stations in the machine. Thus, the stationary supplies for each feeder may provide positive feeding or controlled feed of the strand material thereby insuring the desired geometry in the fabric produced by the knitter-braider.
The components are then assembled by a zigzag sewing machine as diagrammed in FIG. 6. Preferably, the sewing machine is a chain stitch machine having a reciprocating needle on one side the work which cooperates with an oscillatory looper on the opposite side of the work. Following the schematic diagram of FIG. 6, the rovings which are employed to fabricate the individual components of the tape 10 are knitted in groups of four to form tubular knitted fabric components 11 through 14 of any desired length. These components are then fed through feed rollers which flatten the tubes and position them side-by-side so that a sewing machine may provide a seam such as indicated at 15, 16 and 17 in FIGS. 2 and 3. The tubular components may be all sewn together at the same time or they may be connected two at a time as desired, or as required by the capability of the sewing machine.
In the embodiment shown in FIGS. 1 and 2, the composite fabric produces a tape having a width corresponding to the accumulated with of the individual components which are connected to form the composite fabric. The longitudinal extensibility of the individual component and the use of a zigzag stitch seam to interconnect the juxtaposed components is particularly effective to provide longitudinal extensibility in the composite fabric. By reason of the stitch formation and the strand tension in the components, the lateral extensibility of the fabric is restricted so that the composite fabric has good lateral dimensional stability and provides a tape structure which is capable of withstanding harsh handling during use.
A preferred application for the tape of FIGS. 1 and 2 is for use as a framing gasket where it is desired to position the tape around the periphery of a frame to separate or insulate the frame from the underlying structure. The longitudinal extensibility of the composite fabric provides an ability for the fabric to lay flat as it is displaced into a curvilinear path at the corners of the frame element without bunching or creasing, which in conventional gasketing material provides open passageways which render the seal ineffective in the corners. With conventional inextensible gasket material, the bunching of the material in the corners is avoided by mitering the corners of the gasketing material and relying on the abutment of the mitered edges of the material in the corners of the frame. Obviously, inaccuracies in mitering the corners of the inextensible gasketing material enables the formation of gaps which destroy the effectiveness of the seal. By providing extensibility without creasing or bunching, the need for mitering is obviated in the present invention.
The invention is also effective to provide a tadpole tape of the character shown at 40 in FIGS. 4 and 5 in which one marginal portion of the tape is of substantially greater thickness than the other marginal portion. Such a tape is frequently used as a sealing gasket wherein the tail portion, i.e., the marginal portion of lesser thickness is used to mount the tape between a pair of confronting clamping elements. The body portion, i.e., the marginal portion of greater thickness, is left free to serve as a resilient sealing portion which may conform to irregularities in the surfaces between which it is positioned.
A tadpole tape of this character is formed in the same fashion as the tape of FIGS. 1 and 2 but instead of having all of the fabric components of the tape formed identically, one of the components 41 is formed with substantially greater bulk than the other components 42, 43 and 44 so that the component 41 may serve as the body portion of the tadpole tape while the remaining components 42, 43 and 44 combine to serve as the tail portion. Depending upon the degree of difference between the bulk of the body portion and the tail portion, the tape components may be fabricated on the same machines with simply the substitution of a bulkier strand in the component 41 forming the body portion in comparison to the less bulky strands in the components 42, 43 and 44 forming the tail portion.
In this embodiment of the invention, the tape may be assembled in the same fashion as that set forth above in connection with FIGS. 1 and 2, following the schematic diagram of FIG. 6.
Thus, the tapes of the present invention are manufactured using the most economical fabrication techniques, namely circular knitting and sewing by sewing machine. The production rate of circular knitters is substantially greater than the production rate of braiding machines and by the use of the tubular knitting technique, the separate components of the fabrics are produced with substantial thickness caused by the doubling and overlapping effect achieved in the knitting operation.
In order to obtain fabrics of comparable thickness prior to the present invention, it was necessary to use multi-ply weaving techniques which in themselves are slow and provide problems in the fabrication operation, or to use braiding which is likewise slow and expensive. Furthermore, in the braiding apparatus, the strand material must be provided in a form which may be accommodated in the carriers of the braiding machine. The conventional bobbins of a braiding machine render it impractical to use yarns of any substantial bulk.
In the preferred embodiment of the invention the individual components of the composite fabric are tubular knit with only four needle wales and through selection of a fabric of this character, it has been found that each component itself provides a highly compact structure in which the strand material, in this case the four individual strands, are capable of completely filling the central portion of the tubular material so as to provide a dense fabric of substantial thickness and wherein the density of the fibrous material and the strands is effective to eliminate any voids or open spaces within the body of the fabric. The knitted structure provides a compact bundle of knitted loops having a large number of air spaces in it but which provides substantial impediment to direct airflow through the material so that the material may serve as an effective sealing element. The fibrous nature of the structure, on the other hand, does permit breathing of the fabric and permits escape of air through the seal when subjected to a substantial increase in pressure.
The zigzag stitching provided by the seams between the juxtaposed components tends to maintain the components in the flattened state which they assume during the stitching operation, but the fibrous nature of the components permits them to have sufficient resilience to serve as an effective sealing element which may conform to variations in surfaces between which the sealing element is positioned.
It has been found that the lengthwise extensibility and widthwise inextensibility of the composite fabric permits the tape to be laid flat around a corner. For the purpose of providing maximum tape effectiveness, it has been found that the width of the composite tape should be less than one-third of the radius of curvature of the sharpest curve to which the tape is subjected.
The tape of the present invention is also highly effective for wrap-around framing for glass inserts and the like, wherein the tape is wrapped around the edge of the glass insert prior to its insertion into the frame. The same tape thereby serves as a framing gasket for both surfaces of the glass insert. The lengthwise extensibility of the tape of the present invention enables the tape to be wrapped continuously around the perimeter of a glass insert without bunching and to thereby provide a firm seat for the insert in its frame.
The following are examples of composite fabric construction which have been found preferred for certain end uses.
EXAMPLE I
To produce a framing gasket for mounting a glass insert within a frame, for example mounting an oven inspection window within the door of the oven, the following procedure may be used. Starting with one strand per needle composed of 2 ends of 45 count-US (approximately 110 TEX) fiberglass roving as the feed supply, knit 12 lengths of tubular knitted fabric components on an 18 ga Lamb knitter-braider having an approximately one-half inch cylinder with four needles and four feeders. Knit the fiberglass roving into the tubular component at 12 courses per inch with a fabric takeoff at the rate of two feet per minute. The product from two knitters are fed side-by-side in pairs through a sewing machine having a zigzag chain stitch positioned to provide a lateral throw of 1/8-inch and a stitch length of 5/32-inch to thereby interconnect the pair of tubular components side-by-side. These pairs are then fed through a similar sewing machine to interconnect the pairs side-by-side repeatedly until six of such pairs are interconnected to thereby produce a composite fabric composed of 12 tubular knit interconnected juxtaposed components. A predetermined length of this composite fabric is produced so that it may be cut to a length corresponding to the perimeter of the window which is to be mounted in the frame within the door of the oven.
The tape of this Example has a width of 21/4 inches and a thickness of approximately 3/16 inch and is capable of laying flat with around a radius of seven inches. When folded over the edge of the window glass inserted into the oven, it follows a curvilinear path having a radius of approximately four inches without generating any substantial creases or wrinkles in the turn.
EXAMPLE II
To produce a tadpole tape for sealing the perimeter of an oven door, one strand per needle consisting of 2 ends of 45 count-US fiberglass roving is fed to four knitting machines of the type set forth in Example I and the machines are adjusted in the same manner as set forth in Example I. In addition, one strand per needle composed of 4 ends of 45 count-US fiberglass roving is fed to a second knitting machine of the aforedescribed type and the knitting machine is adjusted to knit the fiberglass roving into the tubular component at 8 courses per inch with a fabric takeoff at the rate of 3 feet per minute.
The four tubular fabrics having the strand with 2 ends are interconnected by zigzag sewing as set forth above, and the composite fabric produced by these four fabrics are then juxtaposed with the tubular knit fabric from the single knitting machine producing tubular fabrics from strands with 4 ends per needle. The components are juxtaposed and interconnected by a seam produced in the sewing machine with the same settings as before to produce a tadpole tape.
The tadpole tape of this example has a keyhole shaped cross section with a width of 1/2-inch, the body portion occupying approximately 3/8-inch and the tail portion occupying approximately 1/2-inch. The thickness of the tail portion is approximately 1/8-inch, whereas the thickness of the body portion when flattened is approximately 1/4-inch.
The foregoing examples are only two of the wide number of variations that are effective within the scope of the present invention. It has been found that the 18 ga cylinder knitter-braider is effective to knit bundles of fiberglass filaments, including yarns and rovings ranging in size from approximately 45 count to 10 count and a 2.5 ga knitter-braider having 4 needles in the circumference of a 1-1/8-inch cylinder with 4 feeders can knit strands ranging in size from approximately 45 count-US to 1.1 count-US. The latter machine may also knit strands which in themselves are tubular knit strands from the smaller diameter machine where it is desirable to obtain a high-density component of substantial bulk.
While particular embodiments of the present invention have been herein illustrated and described, it is not intended to limit the invention to these specific embodiments. Changes and modifications may be made therein and thereto within the scope of the appended claims.
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A composite bulky fabric of narrow width having lengthwise extensibility and widthwise dimensional stability in which the fabric is made up of a plurality of flattened tubular-knit components disposed in edge-to-edge juxtaposed position and interconnected by seams extending along the junction and formed of a zigzag line of stitching, the knitted tubular components being formed of a non-run stitch comparable to a tricot stitch formation. The tubular knit components are preferably knit on a small diameter knitting machine having a reciprocating feed for each of the needles so that the feed reciprocates between a pair of adjacent needles, and is supplied from a creel or other stationary supply.
The products made in accordance with the invention are useful for thermal and electrical insulating, gasketing, padding, sealing and similar purposes.
The novel method for producing the fabric is diagrammed in FIG. 6.
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BACKGROUND OF THE INVENTION
a. Field of the Invention
The present invention relates to a method of working steel machine parts including machining during quench cooling, and more particularly it relates to a composite tequnique consisting of machining and heat-treatment.
B. Description of the Prior Art
In general, the cutting of quench hardened steel machine parts is very difficult because of their high hardness. In some cases, turning of steel machine parts is performed by using cemented carbide cutting tools or ceramic tools, but the very low machinability of the parts results in the generation of heat, which, undesirably, often changes part of the steel structure. As a measure for avoiding this adverse effect, grinding, electrolytic working or spark-pressure working is employed. However, these working processes are low in working quality and requre a long period of time for a given working operation with a fixed amount to be cut, thus being inefficient. In order to increase productivity, the usual method adopted by manufacturers, though a roundabout way, is to effect cutting, such as turning, prior to quenching, and then effect quench hardening, which is followed by working such as grinding.
On the other hand, when the quenching process of steel is considered, it is seen that, as shown in FIGS. 1 and 2, it is within a relatively low-temperature region below the Ms point that quench hardening commences. In a higher-temperature region, the structure of steel is in a supercooled austenite state and its hardness is considerably low as compared with that when it is in a martensite state. Therefore, it is conceivable that its machinability in this temperature region is naturally improved. A known example of working in this supercooled austenite state is ausforming (plastic working). Since it serves for the strengthening of steels, it has been substantially studied, both scholarlily and technically, and is increasingly used.
SUMMARY OF THE INVENTION
A first form of the present invention has been developed in the course of researches about the above described prior art, and particularly it relates to a composite technique consisting of heat-treatment and machining, intended for machining steel machine parts in the supercooled austenite region during quench cooling. Thus, we have found through tests for machining of various steels that the machining of steels in the supercooled austenite region is possible even if they are not high-carbon steels generally known as ausforming-oriented steels but are low-carbon steels, such as shaft bearing steels, and we have estabished technical facts supporting this technique. In addition, the machining as mentioned herein includes cutting and plastic working. Further, the cutting includes turning and grinding, while the plastic working includes forging and rolling.
A second form of the present invention relates to a composite technique consisting of heat-treatment and cutting, performed in a line subsequent to forge quenching, wherein a steel machine part after being plastic worked is subjected to isothermal retention at 700°-850° C for spheroidigation of cementite on the way of continuous cooling and then to uniform heating to 800°-900° C, which is regarded as the quenching temperature, and cutting is performed in the supercooled austenite region in the course of quench cooling.
A third form of the present invention relates to a composite technique consisting of heat-treatment, plastic working (ausforming) and cutting (auscutting), wherein the plastic working and cutting of steel machine parts are performed in the course of quench cooling, thereby achieving precision finish.
FEATURES OF THE INVENTION
According to the present invention, a steel machine part uniformly heated to the predetermined quenching temperature in accord with the kind of steel, i.e, the quenching temperature in the austenite region above the A1 transformation point is quickly cooled in a cooling medium to a temperature in the vicinity of or above the Ms point, and cutting is performed with the structure of the steel maintained in the supercooled austenite state or a portion thereof undergoing martensite transformation or beinite transformation, and finally the machine part is cooled to room temperature to complete hardening. Therefore, the invention is highly advantageous in materials saving, energy saving and labor saving. Further, descaling by shot blast is no longer necessary, and the large-scale equipment, such as a quenching furnace and annealing furnace and the costly equipment, such as a quenching press, can be dispensed with. Further, the process can be line-sy systemized to achieve high economic advantages, including the reduction of the quantity of half-finished parts, office work costs and transportation costs.
Further, according to the present invention, a steel blank heated to 950°-1,300° C is formed into a steel machine part by forging, rolling or other plastic working process, and in the course of continuous cooling thereof from the forging or rolling temperature, where necessary, it is subjected to isothermal retention at 700°-850° C for spheroidization of cementite, then to uniform heating to the predetermined quenching temperature in accord with the kind of steel, and when it is quench cooled in a cooling medium for the quenching temperature, the cooling is interrupted in the vicinity of the Ms temperature and cutting is performing while effecting air cooling or warmth retention, and finally it is either cooled to room temperature or allowed to undergo beinite transformation and then cooled to room temperature. Thus, in quench cooling, the cooling is interrupted at a temperature preceding the temperature at which hardening takes place, and then cutting is performed. As a result, by only applying heating necessary for hot forging or rolling, it is possible to continuously carry out spheroidization annealing in the course of cooling from this temperature, cutting, quench hardening and aging treatment, while achieving the same merits as those of the first form of the invention.
Further, subsequent to the so-called ausforming wherein a steel blank uniformly heated to the predetermined quenching temperature in accord with the kind of steel is quickly cooled in a cooling medium from this quenching temperature and is then subjected to forming by plastic working before quench hardening commences, cutting is performed in the supercooled austenite state and finally the machine part is either cooled to room temperature or subjected to isothermal retention for a suitable period of time and then cooled to room temperature to complete hardening. As a result, there is obtained a steel machine part with a minimum amount to be ground. Thus, the invention increases productivity and is also highly advantageous from the standpoint of economics, while achieving the same merits as those of the first form of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an isothermal transformation diagram for quenching of SKD-6 steel regarded as suitable for plastic working in the supercooled austenite region;
FIG. 2 is an isothermal transformation diagram for quenching of shaft bearing steel Class 3 (SUJ-3);
FIGS. 3 through 7 are views for explanation of a first form of the present invention; FIG. 3 shows a thermal handling process conventionally employed with respect to shaft bearing steel, in terms of relationship between temperature and time; FIG. 4 shows a thermal handling process according to the present invention, in terms of relationship between temperature and time; FIGS. 5 through 7 show results obtained when shaft bearing steel Class 3 is turned in the supercooled austenite region and an annealed material (raw material) of shaft bearing steel Class 3 is turned at room temperature and under the same cutting conditions, these Figures depicting the principal component force, feed component force and back component force acting on a tool, for different depths of cut;
FIGS. 8 and 9 are views for explanation of another embodiment of said first form of the present invention; FIG. 8 shows the result of measurement by X-rays of the residual stress in the surface layer of a quenched steel ground article according to the present invention, while FIG. 9 shows the result of measurement by X-rays of the residual stress in the surface layer of a conventional quenched steel ground article;
FIGS. 10 and 11 are views for explanation of a second form of the present invention; FIG. 10 shows a thermal handling process conventionally employed with respect to shaft bearing steel, in terms of relationship between temperature and time, while FIG. 11 shows a thermal handling process according to the invention, in terms of relationship between temperature and time;
FIGS. 12 and 13 are views for explanation of a third form of the present invention; FIG. 12 shows a thermal handling process conventionally employed with respect to shaft bearing steel, in terms of relationship between temperature and time, while FIG. 13 shows a thermal handling process according to the present invention, in terms of relationship between temperature and time.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
First Form of The Invention
Cooling in the course of quenching of a steel machine part made of shaft bearing steel Class 3 (SUJ-3) was interrupted and cutting was performed in the supercooled austenite region. As a result of this cutting experiment, this steel machine part exhibited machinability which compared well with that of an annealed material. When it was further cooled to room temperature, a high hardness of above Rockwell C 60 was obtained. In addition, since the cutting is performed in the austenite region, it is hereinafter referred to as auscutting.
The conventional process requires heating and cooling processes many times as follows: (steel machine part) → (annealing) → (turning) → (quenching) → (tempering) → (turning) or (steel machine part) → (annealing) → (turning) → (cold forging) → (annealing) → (turning) → (quenching) → (tempering) → (turning).
In contrast, in the auscutting method according to the present invention, the required processes are: (steel machine part) → (quick cooling after uniform heating) → (auscutting) → (tempering) → (turning). This provides remarkable improvements as seen in FIGS. 3 and 4 in which the conventional and present methods are depicted in terms of temperature cycles.
In the conventional temperature cycle shown in FIG. 3, the steel machine part is uniformly heated to 750°-800° C taking 4-5 hours, retained at this temperature for 4-5 hours, annealed by being gradually cooled for 15-16 hours at a rate of 15°-20° C per hour, shot turned, quenched at 800°-850° C for about 1-2 hours, allowed to cool, and tempered at 150°-200° C for 3-5 hours. In contrast, in the temperature cycle according to the present invention shown in FIG. 4, the steel machine part is uniformly heated to a quenching temperature of 800°-900° C in the austenite region above the A1 transformation point, quickly cooled in a cooling medium to a temperature of 100°-300° C in the vicinity of or above the Ms point, turned (auscut) at this temperature which is retained for about 30 minutes, allowed to cool, and tempered at 150°-200° C for 3-5 hours. In addition, it goes without saying that instead of reheating for tempering subsequent to cooling to room temperature, as shown in FIG. 4, the auscutting may be followed by isothermal transformation for obtaining a beinitic structure.
A concrete experimental example of the above will now be described with reference to an instance of turning.
A hollow cylindrical workpiece (steel SUJ-3) measuring 40 mm in outer diameter, 20 mm in inner diameter and 100 mm in length was heated 850° C × 30 minutes, quenched in a salt bath at 200° C and isothermally retained (for about 2 minutes) to assume a supercooled austenite state. The temperature at which the workpiece was withdrawn was about 220° C. Immediately thereafter, it was chucked on a lathe where its outer diameter surface was then turned (auscut). In order to know the machinability, the tool was set on a power tool meter to measure the cutting resistance. For comparison purposes, an annealed material (raw material) of SUJ-3 was turned at room temperature under the same conditions to measure the machining resistance. Throwaway tips were used for the tools, the front rake being +5°. The results, as shown in FIGS. 5 through 7, indicated that when the depth of cut was 0.5 mm and the feed was 0.2 mm/rev, the auscutting was superior to the turning of the raw material for any of the turning rates in that the principal component force, feed component force and back component force were all lower and hence the machinability was satisfactory. Even when the depth of cut was increased to 1 mm and then to 1.5 mm, the machinability was still better than that of the raw material for a range of turning rate between 50 m/min and 110 m/min. The foregoing refers to turning at temperatures (from 220° C to 180° C) above the Ms point in the completely supercooled austenite state. In order to know what would happen at temperatures just below the Ms point, a magnetic transformation detector was placed in contact with the workpiece to measure the transformation to martensite while turning the workpiece. It was found that when several % transformation to martensite took place, the turning resistance was more or less high and yet satisfactory turning was possible but that when 20% or more transformation took place (the corresponding temperature being 120° C), the turning resistance was extremely high and turning was impossible under the same turning conditions. Further, the hardness of the workpiece as allowed to cool to room temperature subsequent to auscutting was HRC 65-64, indicating that the workpiece had been fully quench hardened. The surface roughness of the workpiece as auscut was better than that of the raw material.
The worked surface roughness obtained by the above described turning operation is 10-30 μ, so that when it is desired to have a better worked surface, finishing by grinding becomes necessary. However, the technical concept of the present invention may be further developed to carry out a series of operations ending in grinding concurrently with heat-treatment to thereby efficiently provide a steel machine part of good quality.
The temperature cycle is substantially the same as those shown in FIGS. 3 and 4 and a detailed description thereof is omitted, but a concrete experimental example thereof is given below with reference to FIGS. 8 and 9 and photomicrographs A and B showing metal structures.
A hollow cylindrical workpiece (steel SUJ-3) measuring 40 mm in outer diameter, 20 mm in inner diameter and 100 mm in length was heated 850° C × 30 minutes, quenched in a salt bath at 230° C and isothermally retained (for about 2 minutes) to assume a supercooled austenite state. The temperature at which the workpiece was withdrawn was about 250° C. Immediately thereafter, it was set on a grinder where it was then subjected to traverse grinding (ausgrinding). When the amount to be ground was set at 0.5 mm in terms of diameter and the amount of feed was placed under a constant pressure by means of hydraulic pressure and the workpiece was axially fed, it was possible to grind a length of 100 mm in 7-8 seconds. In contrast, it took 10 seconds to grind a quenched steel (hardness HRC 64) of the same shape under the same conditions, and it may be said that the ausgrinding is superior in that the grindability is high. Further, when the workpiece was allowed to cool to room temperature after ausgrinding, its hardness was HRC 64-65, indicating that it had been fully quench hardened. The residual stress in the surface layer at that time was measured by X-rays. As a result, as shown in FIG. 8 and Photomicrograph, it was found that the residual stress was a compressive one and there was observed no abnormal structure in the surface layer. In contrast, in the case of the conventional quenched steel ground article, as shown in FIG. 9 and Photomicrograph B, there was observed a tensile residual stress of about 20 Kg/mm 2 in the surface layer and there was also observed an abnormal structure of the order of about 10 μ (white layer).
As described above, the grinding of conventional quenched steels has a limit in efficiency and continued grinding beyond that limit would cause grinding burn, resulting in a tensile residual stress and abnormal structure, which are undesirable from the standpoint of quality. On the other hand, in the case of the ausgrinding according to the present invention, even if continued grinding is performed, no abnormal structure is created and a compressive residual stress is produced, thus providing increased efficiency and improved quality. Further, since heat-treatment and grinding can be performed at the same time, the merits regarding materials saving, energy saving and labor saving are high. Further, a method is possible in which ausgrinding is performed subsequent to ausforming in the course of quench cooling, and another method is possible in which grinding is performed in the course of quench cooling subsequent to rolling. Therefore, the invention is very useful for use as a method of working precision parts of high tenacity steel.
Second Form of the Invention
Bearing steel Class 3 (SUJ-3) was hot forged to form a steel machine part, the heat of forging was utilized to spheroidize the steel structure in the course of quench cooling and cutting was performed in the supercooled austenite region, such experiment being repeatedly conducted. The steel machine parts thus obtained exhibited machinability which compared well with that of annealed materials. When they were further cooled to room temperature, there was obtained a high hardness of above Rockwell C 60. In addition, the cutting is performed in the austenite region, it is hereinafter referred to as auscutting.
The conventional process requires heating and cooling processes many times as follows: (steel blank) → (forge rolling) gradual cooling almost to room temperature (annealing) gradual cooling to room temperature (turning) → (quenching) → (tempering) → (grinding). In contrast, in the auscutting method according to the present invention, the required processes are as follows: ##STR1## This provides remarkable improvements as seen in FIGS. 10 and 11 in which the conventional and present methods are depicted in terms of temperature cycles.
Thus, in the conventional temperature cycle shown in FIG. 10, the steel machine part is first heated to 1,100°-1,200° C and then forged or rolled to form an intermediate blank. This intermediate steel machine part is then heated to 750°-800° C taking 4-5 hours, gradually cooled for 15-16 hours at a rate of 15°-20° C per hour for annealing, shot turned after cooling, quenched again at 800°-850° C for about 1-2 hours, allowed to cool and tempered at 150°-200° C for 3-5 hours. In contrast, in the temperature cycle shown in FIG. 11 according to the present invention, the steel machine part is heated to 950°-1,300° C, formed by forging or rolling, and, without being cooled once to ordinary temperature, it is isothermally retained at 700°-850° C, where necessary, for spheroidization of cementite, whereupon it is uniformly heated to the quenching temperature in the austenite region above the A1 transformation point, quickly cooled in a cooling medium to a temperature of 100°-300° C in the vicinity of or above the Ms point, cut (auscut) in an isothermally retained or air cooled condition within an ensuing period of about 30 minutes, allowed to cool, and tempered at 150°-200° C for 3-5 hours. In addition, the cooling process may be varied in accord with the kind of steel and the intended object. Further, it goes without saying that instead of reheating for tempering subsequent to cooling to room temperature, as shown in FIG. 11, the auscutting may be followed by isothermal transformation for obtaining a beinitic structure.
A concrete experimental example will now be described. A steel blank was heated to 1,100° C and formed by a forging machine into an intermediate workpiece (steel SUJ-3) measuring 40 mm in outer diameter, 20 mm in inner diameter and 100 mm in length. It was isothermally retained at 800° C, heated to 850° C and quenched in a salt bath at 200° C and isothermally retained (for about 2 minutes) to assume a supercooled austenite state. The temperature at which the article was withdrawn was about 220° C. Immediately thereafter, it was chucked on a lathe where its outer diameter surface was then turned (auscut). In order to know the machinability, the tool was set on a power tool meter to measure the cutting resistance. The results were the same as those in the case of the first form of the invention (shown in FIGS. 5 and 7).
Third Form of the Invention
Using a steel machine part in process of working, made of bearing steel Class 3 (SUJ-3), having a large amount of material to be removed, cooling was interrupted in the course of quench cooling and as a result of an experiment of cutting subsequent to plastic working, this steel machine part exhibited workability and machinability which were not less high than those of annealed materials. In addition, plastic working in the austenite region is referred to as ausforming and cutting in the austenite region auscutting.
The conventional process is carried out in the following sequence: (steel machine part) -- (quenching) -- (ausforming) -- (spark-pressure working or turning) -- (tempering) -- (grinding). The product which had undergone quenching was very difficult to spark-pressure work or turn. On the other hand, in the ausforming or auscutting method according to the present invention, the sequence is as follows: (steel machine part) -- (quenching) -- (ausforming) -- (auscutting) -- (tempering) -- (grinding), wherein the workpiece is precision worked almost to the degree of a finished product in the step of ausforming or auscutting, so that the final amount of material to be removed by grinding is very small. This provides remarkable merits as shown in FIGS. 12 and 13 in which the conventional and present invention are depicted in terms of temperature cycles.
Thus, in the conventional temperature cycle shown in FIG. 12, a steel machine part subjected to primary rough working is heated to a quenching temperature of 800°-900° C, whereupon it is quickly cooled in a cooling medium and then plastic worked (ausformed) in the supercooled austenite state at 100°-300° C to go through secondary rough working. Thereafter, it is once allowed to cool. It is then subjected to spark-pressure working or turning, tempering at 150°-200° C and grinding for finish.
In contrast, in the temperature cycle according to the present invention shown in FIG. 13, the steel machine part is uniformly heated to a quenching temperature of 800°-900° C in the austenite region above the A1 transformation point, whereupon it is quickly cooled in a cooling medium to a temperature in the vicinity of or above the Ms point or plastic worked (ausformed) and cut (auscut) and then allowed to cool, thereby completing quench hardening. Thereafter, it is tempered at 150°-200° C for 3-5 hours. In addition, it goes without saying that instead of tempering by reheating subsequent to cooling to room temperature, auscutting may be followed by isothermal transformation for obtaining a beinitic structure. A concrete experimental example of said cutting (auscutting) is given. A hollow cylindrical workpiece (steel Class SUJ-3) measuring 40 mm in outer diameter, 20 mm in inner diameter and 100 mm in length was heated 850° C × 30 minutes and quenched in a salt bath at 200° C and isothermally retained (for 2 minutes) to assume a supercooled austenite state. The temperature at which the article was withdrawn was about 220° C. Immediately thereafter, it was chucked on a lathe where its outer diameter surface was then turned (auscut), while in order to know the machinability, the tool was set on a power tool meter to measure the cutting resistance. The results were the same as those in the case of the first form of the invention shown in FIGS. 5 through 7.
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The invention provides a method of working steel machine parts, and it relates to a composite technique consisting of machining and heat-treatment, which makes use of the fact that at temperatures in the vicinity of or above the Ms point during quench cooling, the structure of steel assumes a state of supercooled austenite or a portion thereof assumes a state of martensite transformation or beinite transformation, suitable for machining, and in such state desired machining is applied to steel machine parts, which are then cooled to room temperature for hardening. Other merits and details will be made clear.
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BACKGROUND OF THE INVENTION
The present invention relates to a disc cartridge, for example, a magnetic disc cartridge or an optical disc cartridge, which rotatably accommodates a disc for recording information therein in a cartridge case, and more specifically, to an apparatus for producing a disc cartridge provided with a shutter, made of a synthetic resin, for opening and closing a aperture formed in the cartridge case for inserting a head there through.
A disc cartridge of this kind is already known, an example of which is shown in FIG. 5 in the form of a disassembled perspective view of the cartridge.
FIG. 5 shows a magnetic disc cartridge, in which a flexible magnetic disc 2 is rotatably accommodated in a cartridge case 1 constructed by connecting an upper case 1a and a lower case 1b both made of a synthetic resin. The magnetic disc 2 is formed with a hub 3 at the central portion thereof, which is exposed to the outside through a hole 4 formed at the center of the cartridge case 1. Through this hub 3, the magnetic disc 2 is rotated at a predetermined speed by a driving device.
The above-mentioned cartridge case 1 is formed with rectangular apertures 5, for allowing access of a magnetic head to the disk 2, on the upper and lower surfaces thereof at predetermined positions. About the peripheral region of each of the apertures 5 is formed a shallow recess 6 of a rectangular shape, to which a shutter 7 having a U-shaped cross-section is slidably fitted.
The shutter 7 comprises two flat plate portions 9a, 9b opposing each other and an end plate portion 10 connecting the flat plate portions 9a, 9b with each other at respective edges thereof, and is formed with rectangular windows 8 having almost the same size and shape as the apertures 5. The shutter 7 when mounted on the cartridge can is kept elastically urged by means of a built-in spring (not shown) towards a position such that the apertures 5 are closed. When the shutter 7 is moved against the elastic force of the spring, and is stopped by the stepped portion of the recess 6, the apertures 5 and the windows 8 are registered or aligned with each other and the apertures 5 are opened, thereby making it possible to insert a magnetic head for access to the disk 2.
The shutter 7 is made from metal or a synthetic resin. In the case of metal, the sliding surface of the recess 6 may be scratched by the edges of the shutter 7 when the shutter slides over the surface of the recess 6, and there may be produced scratched chips of synthetic resin which may be deposited on or adhered to the magnetic disc and which are apt to cause errors in recording or in reproducing. When, for preventing this trouble, a large clearance is arranged between the cartridge case 1 and the shutter 7, dust may easily intrude from the outer circumference through the peripheral region of the shutter 7 and may adhere to or be deposited on the magnetic disc 2, thereby also causing errors in recording and reproducing.
On the other hand, in the case when the shutter is made from synthetic resin, there is no problem relating to the scratching of the surface of the recess 6, in contrast to the case when the shutter is made from metal. Therefore, the shutter 7 can be elastically pressed so as to be in close contact with the surface of the cartridge case 1 (recess 6), and the intrusion of dust from the peripheral region of the shutter 7 can be effectively prevented. However, there is still another problem.
The motion of the shutter 7 is limited by stepped portions of the recess 6 of the cartridge case 1. However, when the shutter 7 is shaped such that the flat plate portions 9a, 9b extend as diverging outwards, as shown in FIG. 6A showing a side view of the shutter 7, the end A is widely opened, and the flat plate portions 9a, 9b may ride over the stepped portions, thus allowing the shutter 7 to be moved beyond the limited movable range thereof. As a result, there occurs a problem that a positional deviation is produced between the opening portion or aperture 5 and the window 8, and it become impossible to insert a magnetic head in a suitable manner.
The same problem occurs when the flat plate portions 9a, 9b, which were parallel to each other at the time of fabrication, suffer deformations due to repeated use, and the open end A opens even wider, as shown in FIG. 6A.
Further, when the shutter is so shaped that the flat plate portions 9a, 9b converge towards the open end a as shown in FIG. 6B showing a side view of the shutter 7, there occurs a problem that the open end A become extremely narrow, and the sliding resistance between the shutter 7 and the recess 6 of the cartridge case 1 undesirably increases.
Therefore, it is desirable from a point of view relating to the functional features of the shutter such as movable range-controllability or slide resistance that the flat plate portions of the shutter slightly contact or are convergent to be close to each other with a slight gap therebetween at the free ends, i.e. open end A of the shutter 7.
However, it is not easy to fit the shutter 7 having a contacting open end A as mentioned above to the recess 6 of the cartridge case 1.
Therefore, there is required a fitting process. In one of the conventional processes, opening jigs are inserted through the open lateral sides B and moved towards the open end a relative to the shutter 7, to open the end A and then the shutter 7 fitted to the recess 6 of the cartridge case 1 with the open end A maintained in a relatively widely opened condition. In another conventional process, the flat plate portions 9a, 9b are both pulled outwards by sucking forces of a vacuum suction device, and the shutter 7 fitted to the recess 6 of the cartridge case 1 with the shutter maintained in a relatively widely opened condition.
In the above-mentioned conventional apparatus, in order to fit a shutter 7, having an open end A slightly contacting or slightly opened, to the cartridge case 1, it was required to use opening jigs or a vacuum suction device. As a result, the work for mounting or fitting the shutter became complex and required a long time, thereby deteriorating the efficiency of the work.
SUMMARY OF THE INVENTION
The object of the present invention is to provide an apparatus for producing a disc cartridge in which a shutter with free ends of the flat plate portions can be easily fitted to a cartridge case.
The above-mentioned object can be achieved by an apparatus for producing a disc cartridge, in which a shutter made of synthetic resin is mounted on a cartridge case around the apertures of the cartridge case for receiving a magnetic head for the purpose of opening and closing the apertures, the apparatus comprising a conveying path for conveying the cartridge case a shutter conveying path for conveying the shutter an opening jig for opening the shutter at the free ends of the flat plate portions thereof and maintaining the same in an open condition and a fitting means for fitting the shutter to the cartridge case, so that the shutter is fitted to the cartridge case by the fitting means with its free ends maintained in an open condition when the shutter is conveyed by the shutter conveying means to pass over the opening jig.
When the shutter passes over the opening jig, the free ends of the flat plate portions of the shutter contacting or adjacent to each other are opened and maintained in an open condition to be fitted to the cartridge case.
BRIEF DESCRIPTION OF THE DRAWINGS
The above-mentioned and other objects, advantages and features of the invention will be made clearer from the following explanation of the preferred embodiments with reference to drawings, in which:
FIG. 1 is a plan view of a manufacturing apparatus for a disc cartridge according to an embodiment of the present invention;
FIG. 2 is a sectional view of an opening jig portion of the apparatus of FIG. 1;
FIG. 3 is a side view of the opening jig of FIG. 2;
FIGS. 4A, 4B, and 4C are illustrations showing conveying stages of the shutter;
FIG. 5 is a disassembled perspective view of a conventional disc cartridge; and
FIGS. 6A and 6B are side views of the shutter of FIG. 5.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawings, an embodiment of the present invention will be described below.
FIG. 1 shows a manufacturing apparatus according to an embodiment of the present invention, and illustrates a cartridge case 11 rotatably accommodating therein a disc not shown, a conveying path 12 for conveying the cartridge case 11 one by one, a conveyor 13 constituting the conveying path 12, a shutter 14, a conveying path 15 for conveying the shutter 14, one by one, extending in a direction inclined relative to the conveying path 12 for the cartridge case 11, fitting means 16 disposed on a side wall of the conveying path 12 for the cartridge case at a connecting or joining portion between the conveying path 12 for the cartridge case and the conveying path 15 for the shutter and composed of a conveying guide for the cartridge case 11 and a rotary plate 16a for fitting a shutter 14 to the recess 17 of the cartridge case 11, the rotary plate 16a being rotatably supported around a fulcrum point 16b by means of a rotary bearing (not shown) mounted on a base or frame of the apparatus, pressing means 18 disposed downstream of the conveying path 12 for the cartridge case 11, composed of a plunger for pressing the shutter 14 and reliably fitting the shutter to the recess 17 of the cartridge case 11, a guide shaft 19, a transfer body 20 of crank shape movable in parallel to the conveying direction of the shutter conveying path 15 under the guidance of the guide shaft 19 and provided with a pair of claws 20a, 20b at the lower portion thereof, a vertically movable stopper 21, an opening jig 22 disposed in the way of the shutter conveying path 15, and a stopper body 23 retractably projecting from the lower side of the shutter conveying path 15.
FIG. 2 is a sectional view of an opening jig 22 along line II--II of FIG. 1, and FIG. 3 is a side view of the opening jig 22. In the figures, there are shown a guide groove 24 for passing thereon the claws 20a, 20b of the transfer body 20, a tapered edge portion 25 (in FIG. 3) directed towards the upstream of the conveying path 15 for the shutter 14 and so slanted as to have a gradually increasing height toward the upstream. The opening jig 22 is located so that the bottom wall 22a of the opening jig 22 is spaced apart from the bottom surface 15a of the shutter conveying path 15, thereby making it possible for one of the flat plate portions 26a, 26b of the shutter 14 to pass therethrough. The opening jig 22 is tapered towards a free end 22c opposite to a fixed end 22b.
In the above-mentioned embodiment, the cartridge case 11 is conveyed one by one by the conveyor 13, and stands by at a position C near the fitting device 16. On the other hand, on the shutter conveying path 15, the claws 20a, 20b of the transfer body 20 intrude into the window 27 of the preceding two shutters 14a, 14b, respectively. The shutters 14a, 14b are transferred or conveyed when the transfer body 20 is moved in the conveying direction of the conveying path 12 for the cartridge case.
The shutter 14a at the head is opened (as shown in FIG. 2), when the tapered edge 25 of the opening jig 22 intrudes between the contacting flat plate portions 26a, 26b at the open end A or free ends, and is shifted to the fitting device 16 with the open condition maintained. The opened leading edge 14f of the shutter 14a is obliquely fitted over the recess 17 of the cartridge case 11 at the position C according to the advance of the shutter 14a along the shutter path. The guide portion 12a is not provided at a region where the conveying paths 12, and 15 join with each other to allow the above-mentioned fitting of the shutter to the cartridge case at the position C.
The fitting device 16 is so rotated as to fit the shutter 14 opened at the open end A to the recess 17 of the stand-by cartridge case 11, and the shutter 14 is placed in a position or posture in parallel to the conveying guide portion 12a of the cartridge conveying path 12. The cartridge case 11 fitted with the shutter 14 is then conveyed to the pressing device 18 under the guidance of the fitting device 16 and the conveying path 12, and then, pressed by the pressing device 18, thereby being reliably fitted to the recess 17.
Through the above-mentioned operations, the process of fitting a shutter 14 to a cartridge case 11 is completed.
FIGS. 4A to 4C are illustrations for explaining the operation of conveying the shutter 14 in detail. Reference characters 14a to 14d denote shutters, and numerals 27a to 27d denote the windows of the shutters 14a to 14d.
In FIG. 4A, the claws 20a, 20b of the transfer body 20 intrude into the windows 27a, 27b of the first shutter 14a and the second shutter 14b, respectively, while the claw 21a of the vertically (in perpendicular to the plane of sheet of FIGS. 4A to 4C) movable stopper 21 intrudes into the window 27c of the third shutter 14c.
After the first shutter 14a and the second shutter 14b have simultaneously been transferred toward the fitting device 16, as shown in FIG. 4B, the transfer body 20 is moved upwards to be disengaged from the shutters 14a, 14b and an operation for fitting the first shutter 14a to the above-mentioned cartridge case 11 is conducted. Then, the transfer body 20 is moved back toward an upstream position and moved downwards so that the claws 20a, 20b may intrude into the windows 27b, 27c of the second shutter 14b and the third shutter 14c, respectively. When the first shutter 14a and the second shutter 14b are transferred as mentioned above, the third shutter 14c is released from an engagement with the rotary stopper 21 and is also transferred. This is because a conveyor belt 15a provided at an upstream side of the stopper 23 constantly urges the shutters thereon downstream, and transfers the shutter(s) when the engagement thereof with the stopper is released. However, the stopper body 23 projects in synchronism with the transfer of the third shutter 14c under the control of a controller (not shown) and stops the third shutter 14c at the stand-by position, thereby making it possible for the claws 20a, 20b to intrude into the windows 27b, 27c of the second and third shutters 14b, 14c, respectively when they are moved down again.
When the claws 20a, 20b have intruded into the windows 27b, 27c, the stopper body 23 is retracted from the shutter conveying path 15. During a period of time when the shutter 14a is being fitted to the cartridge case 11 by the fitting device 16, the second and third shutters 14b, 14c are held by the transfer body 20. The claw 21a of the vertically movable stopper 21 intrudes into the window 27d of the fourth shutter 14d for holding the fourth shutter.
As mentioned above, according to the present invention, there is provided a manufacturing apparatus for a disc cartridge capable of automatically fitting a shutter to a cartridge case, even in the case when the shutter has a contacting or nearly contacting free ends of the flat plate portions, and having an improved operability.
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A manufacturing apparatus for a disc cartridge including a cartridge case accommodating a disc and having apertures for receiving a head, and a shutter of a U-shaped cross-section slidably fitted to the cartridge case. In the path for conveying the shutter, there is provided an opening jig which opens the open end of the shutter and maintains the open end of the shutter in an open condition, until the shutter is fitted to the cartridge case.
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This application is a continuation of U.S. patent application Ser. No. 10/604,142 filed on Jun. 27, 2003. now U.S. Pat. No. 7,410,919issued Aug. 12, 2008.
FIELD OF THE INVENTION
The present invention relates to the field of semiconductor processing; more specifically, it relates to an apparatus and method for aligning a solder bump mask to a substrate.
BACKGROUND OF THE INVENTION
The formation of solder bumps or controlled collapse chip connection (C 4 ) interconnects on semiconductor substrates requires assembly of an alignment fixture holding the substrate and a metal mask having holes through which the solder bump processes of sputter clean, pad limiting metallurgy evaporation and solder bump evaporation are performed. Prior to these process steps, the mask must be aligned to the substrate. Traditionally, alignment of mask to substrate has been done manually, however as solder bump sizes and spacing between solder bumps has decreased; manual alignment has been shown to be unable to provide the alignment accuracy needed.
SUMMARY OF THE INVENTION
A first aspect of the present invention is a system for of aligning a mask to a substrate comprising: an alignment fixture for temporarily holding the mask and the substrate in fixed positions relative to each other; means for holding the substrate by a bottom surface, the means for holding the substrate protruding through an opening in a table and an opening in the alignment fixture, the means for holding fixedly mounted on a stage assembly, the stage assembly moveable in first and second directions and rotatable about an axis relative to the table; means for temporarily affixing the alignment fixture containing the mask and the substrate to the table; means for controlling the means for temporarily affixing so as to generate a uniform force around a perimeter of the alignment fixture to effectuate the temporarily affixing; means for aligning the mask to the substrate, the means for aligning controlling movement of the stage assembly in the first and second directions and rotation about the axis; and means for temporarily fastening the alignment fixture together.
A second aspect of the present invention is a method for of aligning a mask to a substrate comprising in the order recited: (a) placing a bottom ring of an alignment fixture on an alignment tool; (b) loading a substrate onto a chuck; (c) securing the substrate on the chuck; (d) locating alignment targets on the substrate relative to fixed positions of a first X-Y stage and a rotational stage mounted on the first X-Y stage; (e) placing the mask on the bottom ring and placing a top ring of the alignment fixture on the mask, the top ring aligned to the bottom ring; (f) applying a clamping force of a first predetermined amount of force to the alignment fixture sufficient to prevent the mask from moving relative to the top and bottom rings; (g) locating alignment marks on the mask relative to a fixed position of a second X-Y-stage, the first X-Y stage and the table mounted to the second X-Y stage, X and Y orthogonal displacement directions associated with each of the first and second X-Y stages being co-aligned; (h) calculating an X distance in the X direction and a Y distance in the Y direction to move the first X-Y stage and an angle to rotate the rotational stage through in order to align the alignment marks to the alignment targets; (i) increasing the applied clamping force to a second predetermined amount of force, releasing the substrate from the chuck, and increasing the applied clamping force to a third predetermined amount of force; (j) temporarily fastening the alignment fixture containing the mask and the substrate together; and (k) releasing the applied clamping force.
A third aspect of the present invention is a method for of aligning a mask to a substrate comprising in the order recited: (a) providing an alignment fixture for temporarily holding the mask and the substrate in fixed positions relative to each other; (b) providing an alignment tool including a stage assembly and a table; (c) placing a bottom ring of the alignment fixture on the table; (d) securing the substrate on the chuck and locating alignment targets on the substrate relative to a fixed position of the stage assembly; (e) placing the mask on the bottom ring and placing a top ring of the alignment fixture on the mask, the top ring aligned to the bottom ring; (f) applying a affixing force of a first predetermined amount of force to the alignment fixture sufficient to prevent the mask from moving; (g) locating alignment marks on the mask relative to a fixed position of the stage assembly; (h) moving the substrate relative to the mask in order to align the alignment marks to the alignment targets; (i) increasing the applied affixing force to a second predetermined amount of force, releasing the substrate from the chuck, increasing the applied affixing force to a third predetermined amount of force; (j) temporarily fastening the alignment fixture containing the mask and the substrate together; and (k) releasing the applied affixing force.
BRIEF DESCRIPTION OF DRAWINGS
The features of the invention are set forth in the appended claims. The invention itself, however, will be best understood by reference to the following detailed description of an illustrative embodiment when read in conjunction with the accompanying drawings, wherein:
FIG. 1A is a top view of a bottom ring of a substrate to mask alignment fixture for forming interconnects according to the present invention;
FIG. 1B is a cross-section view through line 1 B- 1 B of FIG. 1A ;
FIG. 2 is a top view of an evaporative mask for forming interconnects according to the present invention;
FIG. 3A is a top view of a top ring of the substrate to mask alignment fixture for forming interconnects according to the present invention;
FIG. 3B is a cross-section view through line 3 B- 3 B of FIG. 3A ;
FIG. 4A is a partial cross-section view through the assembled substrate to mask alignment fixture for forming interconnects according to the present invention;
FIG. 4B is a top view and FIG. 4C is a side view of a spring clip illustrated in FIG. 4A ;
FIG. 5 is a top view of an alignment tool according to the present invention;
FIG. 6 is a cross-section view through line 6 - 6 of FIG. 5 ;
FIG. 7A is a cross-section view through an alignment pin mechanism according to the present invention;
FIG. 7B is a diagram illustrating the tolerances between the alignment pin of FIG. 7A and a mask;
FIG. 8 is a side view of a clamping mechanism according to the present invention;
FIG. 9 is a side view of a clipping mechanism, according to the present invention;
FIG. 10A is a top view of a substrate having alignment marks according to the present invention;
FIG. 10B is a top view of a mask having alignment marks according to the present invention;
FIG. 10C is a top view of the substrate and mask alignments are they would appear in perfect alignment;
FIG. 11A is a diagram of initial wafer alignment fiducials prior to mask to wafer alignment according to the present invention;
FIG. 11B is a diagram of initial mask alignment fiducials coordinates prior to mask to wafer alignment according to the present invention; and
FIG. 12 is a flowchart of the method for aligning a substrate to a mask according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
For the purposes of the present invention the term interconnect is defined as a solder bump or C 4 interconnection that is formed by evaporation onto a substrate through holes formed in a mask. The term substrate is defined to include but is not limited to semiconductor substrates (or wafers) including bulk silicon substrates and silicon-on-insulator (SOI) substrates. The term mask includes but is not limited to metal masks fabricated from molybdenum or other metals. Movement in any of the mutually orthogonal X, Y and Z directions and the rotational Θ direction (as described infra) includes movement in both positive and negative directions.
FIG. 1A is a top view of a bottom ring 100 of a substrate to mask alignment fixture for forming interconnects according to the present invention and FIG. 1B is a cross-section view through line 1 B- 1 B of FIG. 1A . In FIGS. 1A and 1B , bottom ring 100 includes an outer lip 105 and an inner lip 110 joined by an integral plate 115 . Inner lip 110 defines the extent of an opening 120 centered in bottom ring 100 . Plate 115 includes a multiplicity of openings 125 . Opening 120 provides access for a substrate positioning chuck (see FIG. 6 ) and openings 125 are for thermal expansion and heat retention control during evaporative processes and to make bottom ring 100 lighter. The difference in height between outer lip 105 and inner lip 110 is H 1 In one example, for a standard 200 mm diameter wafer about 650 microns thick, H 1 is about 0.007 inches. Bottom ring 100 also includes an alignment pin hole 130 A and a diametrically opposed alignment pin slot 130 B, each positioned adjacent to an outer perimeter 135 of the bottom ring. Bottom ring 100 further includes a multiplicity (in the present example 6) of retainer post holes 140 evenly spaced about and adjacent to outer perimeter 135 of the bottom ring.
FIG. 2 is a top view of an evaporative mask for forming interconnects according to the present invention. In FIG. 2 , a circular mask 145 includes a multiplicity of openings 150 arranged in groups 155 . Each group 155 corresponds to a chip on a substrate (not illustrated) that will be placed under mask 145 as illustrated in FIG. 4 and described infra. Mask 145 also includes an alignment pin hole 160 A and a diametrically opposed alignment pin slot 160 B, each positioned adjacent to an outer perimeter 160 of the mask. Mask 145 further includes a multiplicity (in the present example 6) of retainer post holes 165 evenly spaced about and adjacent to outer perimeter 160 of the mask.
FIG. 3A is a top view of a top ring 175 of the substrate to mask alignment fixture for forming interconnects according to the present invention and FIG. 3B is a cross-section view through line 3 B- 3 B of FIG. 3A . In FIGS. 3A and 3B , top ring 175 has a lower lip 180 protruding from a flange 185 . Lower lip 180 protrudes a distance H 2 . In one example, for a standard 200 mm diameter wafer having a thickness of about 725 microns, H 2 is about 0.002 inches. Top ring 175 includes an opening 190 centered within top ring 175 . Top ring 175 also includes an alignment pin hole 195 A and a diametrically opposed alignment pin slot 195 B, each positioned adjacent to an outer perimeter 200 of the mask. Top ring 175 further includes a multiplicity (in the present example 6) of retainer posts 205 evenly spaced about and adjacent to outer perimeter 200 of the mask.
FIG. 4A is a partial cross-section view through an assembled substrate to mask alignment fixture 210 for forming interconnects according to the present invention. In FIG. 4A , only a portion of assembled fixture 210 is illustrated. Substrate 215 and mask 145 are illustrated contained in alignment fixture 210 . Retainer posts 205 protrude through retainer post holes 140 in bottom ring 100 and pass through retainer post holes 165 in mask 145 . When spring clips 220 are slid onto retainer posts 205 perimeter 160 of mask 145 is held in a slightly pressed down position by lower lip 180 of top ring 175 against outer lip 105 of spring clips 220 thus holding substrate 215 , mask 145 , top ring 175 and bottom ring 100 together. Spring clips 220 are not put in place until mask 145 is aligned to substrate 215 .
The combination of the difference in heights between outer and inner lips 105 and 110 of bottom ring 100 and lower lip 180 of top ring 175 deflects (or bows) substrate 215 and mask 140 into very shallow but semi-spherical shape by pressing perimeter 160 of mask 145 and perimeter 225 of substrate 215 towards bottom ring 100 .
Since alignment fixture 210 is mounted in a dome of a metal evaporator, the bow imparted to substrate 215 prevents or reduces such problems associated with evaporation through an knife edge opening in a mask such as sputter haze, PLM flaring and solder pad haloing.
FIG. 4B is a top view and FIG. 4C is a side view of spring clip 220 illustrated in FIG. 4A . Spring clip 220 includes a notch 230 that engages a lower end 235 of retainer post 205 as illustrated in FIG. 4A . Spring clip 220 also includes a retraction hole 240 to enable removal of spring clips 205 and thus disassembly of alignment fixture 210 (see FIG. 4A ). FIG. 4C illustrates spring clip 220 before engagement with retaining post 205 .
FIG. 5 is a top view of an alignment tool 250 according to the present invention. In FIG. 5 , alignment tool 250 includes a top plate 255 a chuck 260 , alignment pin mechanisms (illustrated in FIG. 8A and described more fully infra), a multiplicity of clamping mechanisms 270 (illustrated in FIG. 9 and described more fully infra) and a multiplicity of clipping mechanisms 275 (illustrated in FIG. 10 and described more fully infra). Chuck 260 extends through an opening 280 in top plate 255 and includes a multiplicity of O-rings 285 . Each O-ring surrounds a vacuum port 290 centered within the ring. O-rings 285 are arranged in a ring and located adjacent to a perimeter 295 of chuck 260 . Clamping mechanisms 270 are evenly spaced around a locator ring 300 centered on chuck 260 that roughly defines the position occupied by alignment fixture 210 . Clipping mechanisms 275 are evenly spaced around locator ring 300 . Alignment pin mechanisms (containing alignment pins 305 ) are positioned diametrically opposed adjacent to and interior of locator ring 300 . Attached to an underside of top plate 255 is a fixed inner actuator ring 310 having outwardly protruding spokes 315 . Spokes 315 extend through eccentric slots 350 (not shown in FIG. 5 , see FIG. 6 ) in a rotatable outer actuator ring 320 . Outer actuator ring 320 can move up and down in the Z direction (see FIG. 6 ) as well as rotate in the θ direction (see FIG. 6 ) about an axis defined by the Z direction.
While six clamping mechanisms 270 and six clipping mechanisms 275 are illustrated in FIG. 5 , any number greater than or equal to three mechanisms of each type may be used. While two alignment pins mechanisms are illustrated in FIG. 5 , a greater number of alignment pin mechanisms may be employed in which case the number and arrangement of alignment pin holes 130 A and 195 A and alignment pin slots 130 B and 195 B (see FIGS. 1A and 3A respectively) will change.
While eight O-rings 285 are illustrated in FIG. 5 , chuck 260 may include a lesser or greater number of O-rings, the minimum number being three. The inventors have discovered that chucks using a conventional single O-ring design can induce errors up to 10 times greater then the accuracy of the encoders because of O-ring distortion during the alignment process. This distortion is caused by the fact that mask 145 (see FIG. 2 ) and substrate 215 (see FIG. 4A ) are in slight frictional contact that can cause a single O-ring to distort or creep. The radially orientated multi O-ring design of chuck 260 all but eliminates translation errors caused by O-ring creep. Note, a single O-ring design using a hard O-ring, presents other problems such as substrate breakage, since being less flexible there is insufficient compressibility in the O-ring to absorb acceleration induced shock.
FIG. 6 is a cross-section view through line 6 - 6 of FIG. 5 . In FIG. 6 , chuck 260 is mounted on an rotational stage 325 for θ adjustment that in turn is mounted on an upper X-Y stage 330 for X direction and Y direction (the Y direction is into plane of the paper) adjustment of the position of substrate 215 . Upper X-Y stage 330 is in turn mounted on a lower X-Y stage 340 . It is preferred, but not necessary that the X movement of upper X-Y stage 330 is perpendicular to the Y movement of lower X-Y stage 340 , the Y movement of upper X-Y stage 330 is perpendicular to the X movement of lower X-Y stage 340 and the top surfaces 325 A, 330 A and 340 A respectively of rotational stage 325 , upper X-Y stage 330 and lower X-Y stage 340 are parallel. Top plate 255 is also mounted on lower X-Y stage 340 via brackets 345 . Since alignment pin mechanism 265 is fixed to top plate 255 , a measurable and repeatable relationship exists between alignment pins 305 and chuck 260 as long as the relative positions of upper X-Y stage 325 and lower X-Y stage 340 are known.
As outer actuator ring 320 rotates spokes 315 fixed to inner actuator ring 310 and passing through slanted slots 350 in the outer actuator ring cause the outer actuator ring to translate in the Z direction. Note, the X, Y and Z directions are orthogonal to each other. A lip 355 attached to outer actuator ring 320 thus also moves in the Z direction. A push rod of clamping mechanism 270 rides on lip 355 (see FIG. 8 ) so clamping is controlled by the rotation of outer actuator ring 315 and clamping force is uniformly applied by all clamping mechanisms 275 (see FIG. 5 ). Alignment tool 250 also includes an optical system 360 (generally a lens and a camera) linked to a computer 365 containing pattern recognition software as well a software for controlling movement rotational stage 325 , upper X-Y stage 330 and lower X-Y stage 340 . The pattern recognition software detects the position of alignment targets on substrate 215 and alignment marks on mask 145 . Computer 365 is linked to stepping motors on rotational stage 325 , upper X-Y stage 330 and lower X-Y stage 340 for controlling movement of substrate 215 . Computer 365 calculates the amount of upper X-Y stage 330 , lower X-Y stage 340 and rotational stage 325 movement required to align mask 145 with the substrate 215 .
During the alignment process, it is important that movement of substrate 215 is precise and accurate. In one example, encoders within rotational stage 325 are accurate to 0.001 degree encoders within upper X-Y stage 330 and lower X-Y stage 340 are accurate to 1 micron.
FIG. 7A is a cross-section view through alignment pin mechanism 265 according to the present invention. In FIG. 7 , alignment pin mechanism 265 includes a body 370 having a lower chamber 375 open to an upper chamber 380 . Alignment pin 305 includes an upper narrow portion 385 and a wide lower portion 390 . Alignment pin 305 extends through upper chamber 380 into lower chamber 375 . Alignment pin 305 is restricted in movement in the X and Y directions by sleeve bearing 395 and is moveable in the Z direction due to spring 400 contained within lower chamber 375 . Lower portion 390 of pin 305 passes through alignment pin hole 130 A (or alignment pin slot 130 B) in bottom ring 100 as well as an opening 405 in top plate 255 . Upper portion 385 of pin 305 passes through alignment pin hole 160 A (or alignment pin slot 160 B) in mask 145 . Upper portion 385 of pin 305 also passes through alignment pin hole 195 A (or alignment pin slot 195 B) in top ring 175 .
FIG. 7B is a diagram illustrating the tolerances between alignment pin 305 of FIG. 7A and mask 145 . In FIG. 7B , upper portion 385 of alignment pin 305 has a diameter of D 1 . Lower portion of alignment pin 305 has diameters D 2 . Alignment pin hole 160 A of mask 145 has a diameter of D 3 . Note alignment pin slot 160 B (see FIG. 2 ) has a width of D 3 and is about 2D 3 long. D 2 is greater than D 1 . In one example D 2 −D 1 =0.010 inch and D 3 −D 1 =0.002 inch.
Returning to FIG. 7A , during alignment of mask 145 to a substrate 215 , it is important that the mask does not move. Mask 145 experiences forces in the X, Y and θ directions. Alignment pins 305 restrict this movement. It is also important that alignment pins 305 move freely in the Z direction. Spring 400 ensures that there is always a net upward force (positive Z direction) on alignment pin 305 to resist downward force (negative Z direction) imparted to mask 145 by clamping mechanisms 270 (see FIG. 5 ) during the alignment process to keep constant contact between the mask and bottom ring 100 .
FIG. 8 is a side view of clamping mechanism 270 according to the present invention. In FIG. 8 , clamping mechanism 270 includes a mounting bracket 410 mounted to top plate 255 , a body 415 , a moveable clamp finger 420 slidably mounted in body 415 and a push rod 430 that operably engages lip 355 of outer actuator ring 320 . Clamp finger 420 can be slid over or retracted from top ring 175 by a mechanism not illustrated. As outer actuator ring rotates 320 , because spokes 315 are fixed to inner actuator ring 310 and extend through eccentric slots 350 , lip 355 moves up or down depending on the direction of rotation of outer actuator ring 320 . Push rod 430 , engaged on lip 355 , moves up and down with lip 355 , causing clamp finger 420 to apply pressure to the assembled alignment fixture 210 comprising bottom ring 100 , substrate 215 , mask 145 and top ring 175 . Clamp finger 420 is spring loaded so movement of lip 355 toward top plate 255 works against the spring and moves clamp finger 420 away from alignment fixture 210 . As lip 355 lowers, increasing pressure is applied to alignment fixture 210 .
Once the alignment process is completed, it is important that the clamping process be uniform across alignment fixture 210 , smooth and reproducible time to time. Any non-uniformity will result sideway slippage of mask 145 and/or substrate 215 and thus misalignment after the alignment process. Any non-smoothness in clamping can result in a shock that can cause mask 145 and/or substrate 215 movement, again resulting in misalignment after the alignment process. Non-reproducibility in clamping pressure can result in clipping (see FIG. 9 and discussion infra) problems. Since all clamping mechanisms 270 are driven by outer actuator ring 320 clamping is uniform and smooth. A precision drive mechanism (not shown) driving outer actuator ring 320 ensures reproducible and precision controlled clamping pressure.
FIG. 9 is a side view of clipping mechanism 275 according to the present invention. In FIG. 9 , clipping mechanism 275 includes a base 435 mounted to top plate 255 , a slide 440 having a slot (not shown) to hold a clip 220 , and a roller 445 mounted to a support 450 attached to base 435 . In operation, a clip 220 placed on slide 440 . As slide 440 is pushed forward toward retaining post 235 , clip 220 is compressed by roller 445 . As slide 440 continues forward, clip 220 engages retaining post 235 and becomes released from roller 445 allowing clip 220 to “spring” open. When slide 440 is retracted, clip 220 remains in place due to friction forces between the clip and bottom ring 100 .
It is important that insertion of clips 220 do move top ring 175 to which retainer posts 235 are fixedly attached. Movement of top ring 175 will cause mask 145 to move, thus changing the alignment of mask 145 to substrate 215 . Clipping mechanism 275 “preloads” clips 220 so that forces in the Z direction are eliminated during insertion, resulting in minimal X direction and Y direction forces being applied to retaining post 235 and top ring 175 during insertion. Each slide 440 moved to engage retaining posts 235 simultaneously by a mechanical mechanism.
FIG. 10A is a top view of a substrate having alignment marks according to the present invention. In FIG. 10A , substrate 100 includes diametrically opposed (or nearly diametrically opposed) left and right course alignment targets 455 A and 455 B respectively and diametrically (or nearly diametrically opposed) left and right fine alignment target sets 460 A and 460 B respectively. Left and right course alignment targets 455 A and 455 B are used by pattern recognition software residing on computer 365 (see FIG. 6 ) during alignment operations. Left and right fine alignment targets 460 A and 460 B are used by an operator to check the quality of alignment operations.
FIG. 10B is a top view of a mask having alignment marks according to the present invention. In FIG. 10B , mask 145 includes diametrically opposed (or nearly diametrically opposed) left and right course alignment marks 465 A and 465 B respectively and diametrically (or nearly diametrically opposed) left and right fine alignment mark sets 470 A and 470 B respectively. Left and right course alignment targets 465 A and 465 B are used by pattern recognition software residing on computer 365 (see FIG. 6 ) during alignment operations. Left and right fine alignment targets 470 A and 470 B are used by an operator to check the quality of alignment operations. Also illustrated in FIG. 10B are alignment pin hole 160 A and alignment pin slot 160 B.
FIG. 10C is a top view of the substrate and mask alignments are they would appear in perfect alignment. In FIG. 10C , course substrate alignment target 455 A ( 455 B) is centered on the middle two course mask alignment marks 465 A ( 465 B). All mask fine alignment marks 470 A ( 470 B) are centered in substrate fine alignment targets 460 A ( 460 B).
FIG. 11A is a diagram of initial wafer alignment fiducial coordinates prior to mask to wafer alignment according to the present invention. In FIG. 11A , rotational stage in 325 can move the Θ direction and upper X-Y stage 330 can move in the X and Z direction. A reference location 475 has upper X-Y stage coordinates X 0 and Y 0 and rotational stage 325 coordinate Θ 0 . Rotational stage 325 and upper X-Y stage 330 are initially moved to coordinates X 0 , Y 0 and Θ 0 respectively (as described infra in reference to FIG. 12 ) and all subsequent motions of rotational stage 325 and upper X-Y stage 330 stage motions are referenced to coordinates X 0 , Y 0 and Θ 0 respectively. Wafer 215 includes a left fiducial mark 480 containing left course alignment target 455 A (see FIG. 10A ) and fine alignment targets 460 A (see FIG. 10A ) and a right fiducial mark 485 containing right course alignment target 455 B (see FIG. 10A ) and fine alignment targets 460 B (see FIG. 10A ). When rotational stage 325 and upper X-Y stage 330 are moved to coordinates X 0 , Y 0 and Θ 0 respectively, left fiducial 480 is at location X LW0 , Y LW0 and Θ LW0 and right fiducial 485 is at location X RW0 , Y RW0 and Θ RW0 .
FIG. 11B is a diagram of initial mask alignment fiducial coordinates prior to mask to wafer alignment according to the present invention. In FIG. 11B , lower X-Y stage 340 can move in the X and Z direction. Lower stage X-Y 340 is referenced to reference position 475 . All subsequent motions of lower X-Y stage 340 are referenced to coordinates X 0 and Y 0 . As long as the X movement of upper X-Y stage 330 is perpendicular to the Y movement of lower X-Y stage 340 , the Y movement of upper X-Y stage 330 is perpendicular to the X movement of lower X-Y stage 340 and the top surfaces of rotational stage 325 , upper X-Y stage 330 and lower X-Y stage 340 are parallel. Mask 145 includes a left fiducial mark 490 containing left course alignment mark 465 A (see FIG. 10B ) and fine alignment marks 470 A (see FIG. 10B ) and a right fiducial mark 495 containing right course alignment mark 465 B (see FIG. 10A ) and fine alignment marks 470 B (see FIG. 10B ). When lower X-Y stage 330 is referenced to coordinates X 0 and Y 0 , left fiducial 490 is at location X LM0 and Y LM0 and right fiducial 495 is at location X RM0 and Y RM0 .
Reference to FIGS. 11A and 11B will be useful in understanding the process illustrated in FIG. 12 and described infra. In FIG. 12 it is assumed that the X movement of upper X-Y stage 330 is perpendicular to the Y movement of lower X-Y stage 340 , the Y movement of upper X-Y stage 330 is perpendicular to the X movement of lower X-Y stage 340 and the top surfaces of rotational stage 325 , upper X-Y stage 330 and lower X-Y stage 340 are parallel. Any deviations from these conditions, requires more complex calculations then described infra in reference to FIG. 12 .
FIG. 12 is a flowchart of the method for aligning a substrate to a mask according to the present invention In step 500 , a bottom ring of the alignment fixture is loaded onto the alignment tool and in step 505 a substrate is placed on the chuck of the alignment tool and vacuum applied to the chuck, holding the substrate fast to the chuck.
In step 510 , the course substrate alignment targets are located. First, the upper X-Y and rotational stages are moved to a predetermined X 0 , Y 0 and θ 0 positions. For the substrate left course alignment target the pattern recognition software locates the center of the left course alignment target and moves the upper X-Y stage and the rotational stage so the center of the left course alignment target is aligned with the center of the optical system. The pattern recognition software again locates the center of the substrate left course alignment target and moves the upper X-Y stage and the rotational stage so the center of the left course alignment target is aligned with the center of the optical system. The double locating brings the substrate left course alignment target to the area of least distortion within the optical system. This fixes the substrate left course target starting position on the upper X-Y stage and the rotational stage as X LW0 , Y LW0 and θ LW0 .
For the substrate right course alignment target the pattern recognition software locates the center of the right course alignment target and moves the upper X-Y stage and the rotational stage so the center of the right course alignment target is aligned with the center of the optical system. The pattern recognition software again locates the center of the substrate right course alignment target and moves on the upper X-Y stage and the rotational stage so the center of the right course alignment target is aligned with the center of the optical system. The double locating brings the substrate right course alignment target to the area of least distortion within the optical system. This fixes the substrate right course target starting position on the upper X-Y stage and the rotational stage as X RW0 , Y RW0 and θ RW0 .
Next, in step 515 , the upper X-Y stage and the rotational stage are moved fixed distances D X , D Y and angle D θ . This motion compensates for the slack that is inherent in the stage mechanics.
In step 520 , the mask is positioned (using the alignment pins) over the substrate and in step 525 the top ring of the alignment fixture is positioned (using the alignment pins).
In step 530 , a light clamping pressure is applied by the clamping mechanisms in order to prevent motion of the mask during subsequent upper X-Y stage, rotational stage and lower X-Y stage movements. The pressure applied is just sufficient to bring the mask and top ring of the alignment fixture into contact.
In step 535 the upper X-Y stage and the rotational stage are moved a distance −D X /2, −D Y /2 and angle −D θ /2 (i.e. halfway back to X 0 , Y 0 and θ 0 ). This motion compensates for the slack that is inherent between the mask and the alignment pins and places the mask in a stable position.
In step 540 , the pattern recognition software locates the center of the mask left course alignment mark and moves the lower X-Y stage so the center of the left course alignment mark is aligned with the center of the optical system. The pattern recognition software again locates the center of the mask left course alignment mark and moves the lower X-Y stage so the center of the left course alignment mark is aligned with the center of the optical system. The double locating brings the mask left course alignment mark to the area of least distortion within the optical system. This fixes the left course mark starting position on the lower X-Y stage as X LM0 and Y LM0 .
For the mask right course alignment mark the pattern recognition software locates the center of the right course alignment mark and moves the lower X-Y stage so the center of the right course alignment mark is aligned with the center of the optical system (generally a lens and a camera). The pattern recognition software again locates the center of the mask right course alignment mark and moves the lower X-Y stage so the center of the right course alignment mark is aligned with the center of the optical system. The double locating brings the mask right course alignment mark to the area of least distortion within the optical system. This fixes the right course mark starting position on lower X-Y stage as X RM0 and Y RM0 .
In step 545 , first the rotational displacement of the substrate θ W =tan −1 ((Y LW0 −Y RW0 )/(X LW0 −X RW0 )) and the rotational displacement of the mask θ M =tan −1 ((Y LM0 −Y RM0 )/(X LM0 −X RM0 )) are calculated. Second, the relative rotational displacement (and correcting theta displacement) between the mask and substrate Δθ MW =θ M −θ W is calculated. In order to align the substrate to the mask in the X and Y directions compensation for the applied rotation is necessary. Third, the X-translation, X′=X WL0 cos Δθ MW −Y WL0 sin Δθ MW (or X′=X WR0 cos Δθ MW −Y WR0 sin Δθ MW ) and the Y-translation Y′=X WL0 sin Δθ MW +Y WL0 cos Δθ MW (or Y R ′=X WR0 sin θ MW +Y WR0 COS θ MW ) are calculated. Fourth, the correcting displacements ΔY=Y ML0 −Y′ or (ΔY=Y MR0 −Y′) and ΔX=X ML0 −X′ or (ΔX=X MR0 −X′) are calculated. Fifth, the Y ALIGN =ΔY+(−D Y /2), X ALIGN =ΔX+(−D X /2) and θ ALIGN =Δθ MW +(−D θ /2) movements of the upper X-Y and rotational stages are calculated.
In step 550 , the mask and substrate are aligned by moving the upper X-Y stage distances X ALIGN and Y ALIGN and moving the rotational stage angle θ ALIGN .
In step 555 , the clamping mechanism fully compresses the top ring, mask and substrate against the bottom ring. The chuck vacuum is released at about 75% full compression in order to avoid breaking the substrate, which is now slightly bowed by the clamping and could be further shocked by air entering the chuck when the substrate releases from the chuck under the condition of the clamping pressure being greater than atmospheric pressure.
In step 560 , clipping mechanisms install the clips on the retaining posts which keep the bottom ring, substrate, mask and top ring stack under compression and in alignment.
In step 565 , the fine alignment targets/marks are inspected to the alignment of mask to substrate is within specification.
Using the alignment fixture, alignment tool and alignment/clamping/clipping procedure described supra, the inventors have been able to achieve alignments between mask and substrate on 200 mm wafers of better than 20 microns.
The description of the embodiments of the present invention is given above for the understanding of the present invention. It will be understood that the invention is not limited to the particular embodiments described herein, but is capable of various modifications, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, it is intended that the following claims cover all such modifications and changes as fall within the true spirit and scope of the invention.
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A system for of aligning a mask to a substrate comprising: a fixture for holding the mask and the substrate in fixed positions relative to each other; means for holding the substrate, the means for holding the substrate protruding through openings in a table and the fixture, the means for holding fixedly mounted on a stage, the stage moveable in first and second directions and rotatable about an axis relative to the table; means for affixing the fixture containing the mask and the substrate to the table; means for controlling the means for temporarily affixing so as to generate a uniform force around a perimeter of the fixture to effectuate the temporarily affixing; means for aligning the mask to the substrate, the means for aligning controlling movement of the stage in the first and second directions and rotation about the axis; and means for fastening the fixture together.
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CROSS-REFERENCE
[0001] This application claims priority to U.S. application Ser. No. 62/071,098 filed on Sep. 15, 2014 and which is incorporated herein for any and all purposes.
FIELD OF THE INVENTION
[0002] The embodiments of the present invention relate to an illuminated garment system for riders of motorcycles or bicycles to better notify traffic of deceleration thereof.
BACKGROUND
[0003] Motorcycles are often not seen by other drivers because motorcycles provide a small visual target such that they are easily overlooked on busy roads. Moreover, motorcycles are capable of more rapid braking deceleration than other vehicles but such use activates brake lights. They can also achieve rapid deceleration by releasing the throttle or down shifting which eliminates the visual cue of the illuminated brake lights. The latter two challenges make the motorcyclist highly vulnerable to accidents with other vehicles and drive the need for an effective means of increasing the motorcyclist's visibility and for signaling deceleration.
[0004] Various methods have been attempted to make the motorcyclist more visible including the use of illuminated clothing. Some illuminated clothes are heavy and bulky and/or plugged into the motorcycle's electrical system. Still others have their own battery pack. For one reason or another, illuminated clothing has not become popular with the motorcycling public.
[0005] Thus, it would be advantageous to develop a stylish, light-weight, highly-visible garment that not only makes the motorcyclist more visible but also warns of a decelerating motorcycle regardless of the means of deceleration.
SUMMARY
[0006] The embodiments of the present invention comprise a garment (e.g., vest) designed to be worn over a motorcyclist's outer clothing with high intensity LED lighting installed on front and rear surfaces thereof and motion-sensing circuitry and corresponding software that detects motorcycle deceleration and controls the sequence, color and/or intensity of the LED lighting. A small, light battery pack installed in the garment powers the system. In one embodiment, the software of the present invention illuminates the LEDs using a repeating or random pattern. The motion-sensing circuitry and software detects that the motorcycle is decelerating when the driver releases or reduces the throttle, downshifts and/or applies the brakes. Responsive to the driver releasing or reducing the throttle, downshifting and/or applying the brakes, the electronics and software change the color output of LEDs on the rear surface of the garment to red. In one embodiment, the electronics of the garment are sealed in watertight assemblies.
[0007] Other variations, embodiments and features of the present invention will become evident from the following detailed description, drawings and claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 illustrates a front view of an illuminated vest showing a front LED array, microprocessors and motion-sensing circuitry, and battery and charge management assembly according to the embodiments of the present invention;
[0009] FIG. 2 illustrates a rear view of the illuminated vest showing a rear LED array according to the embodiments of the present invention;
[0010] FIG. 3 illustrates a block diagram of the electronic circuitry according to the embodiments of the present invention; and
[0011] FIG. 4 illustrates a flow chart detailing one methodology of operating said vest according to the embodiments of the present invention.
DETAILED DESCRIPTION
[0012] For the purposes of promoting an understanding of the principles in accordance with the embodiments of the present invention, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the invention is thereby intended. Any alterations and further modifications of the inventive feature illustrated herein, and any additional applications of the principles of the invention as illustrated herein, which would normally occur to one skilled in the relevant art and having possession of this disclosure, are to be considered within the scope of the invention claimed.
[0013] Those skilled in the art will recognize that the embodiments of the present invention involve both hardware and/or software elements which portions are described below in such detail required to construct and operate the method and system according to the embodiments of the present invention.
[0014] As will be appreciated by one skilled in the art, aspects of the present invention may be embodied as a system, method or computer program product. Accordingly, aspects of the present invention may take the form of an entirely hardware embodiment, an entirely software embodiment (including firmware, resident software, micro-code, etc.), or an embodiment combining software and hardware. Program code embodied on a computer readable medium may be transmitted using any appropriate medium, including but not limited to wireless, wireline, optical fiber cable, RF and the like, or any suitable combination of the foregoing.
[0015] Computer program code for carrying out operations for aspects of the present invention may be written in any combination of one or more programming languages, including an object oriented programming language such as Java, Smalltalk, C++ or the like or conventional procedural programming languages, such as the “C” programming language, AJAX, PHP, HTML, XHTML, Ruby, CSS or similar programming languages.
[0016] Aspects of the present invention are described below with reference to flowchart illustrations and/or block diagrams of methods, apparatus (systems) and computer program products according to embodiments of the invention. These computer program instructions may be provided to a processor of a general purpose computer, special purpose computer, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, create means for implementing the functions/acts specified in the flowchart and/or block diagram.
[0017] These computer program instructions may also be stored in a computer readable medium that can direct a computer, other programmable data processing apparatus, or other devices to function in a particular manner, such that the instructions stored in the computer readable medium produce an article of manufacture including instructions which implement the function/act specified in the flowchart and/or block diagram.
[0018] FIG. 1 shows the front surface of a garment in the form of a vest 1 including front LED strips/arrays 5 , battery and charge management circuitry assembly 10 and microprocessors and motion-sensing circuitry 15 . FIG. 2 shows the back surface of vest 1 including rear LED strips/arrays 20 and battery and charge management circuitry assembly 10 . The electronics of the system are contained in weather-proof assemblies and the electrical connections are weather proof. LED arrays 5 and 20 , battery and charge management circuitry assembly 10 , microprocessors and motion-sensing circuitry 15 as well as the electrical wiring (not shown) are detachable from the vest 1 to allow for cleaning of the same. In one embodiment, hook and loop fasteners are used to attach the components to the garment but any fasteners allowing removal of the components may be used. Alternatively, the components may be integral with the garment such they are not easily removed. As used herein, a “garment” should be understood to be any article (e.g., short, jacket, sweater, etc.) wearable by a user. The position and arrangement of the components on the vest 1 , may be modified without departing from the sprit and scope of the embodiments of the present invention.
[0019] In one embodiment, the battery and charge management circuitry assembly 10 comprises a battery pack 25 , charging circuitry 35 , charge management circuitry 40 , LED power supply 45 and on/off switch 50 . The battery pack 25 may be a rechargeable lithium ion, 7.4 volt UN rated battery. Those skilled in the art will recognize that other batteries may power the system detailed herein.
[0020] Charging circuitry 35 allows the system to be connected to external power supply 55 and configured to detect the battery voltage. If the battery voltage is below a predefined limit and external power supply 55 is connected, charging circuitry 35 executes a constant current/constant voltage-charging algorithm appropriate for a lithium ion battery regardless of whether the LED circuitry is switched on or off via on/off switch 50 . Charging circuitry 35 determines when battery pack 25 is fully charged and discontinues charging thereafter. On/off switch 50 controls power to charge management circuitry 40 , LED power supply 45 and/or microprocessors and motion-sensing circuitry 15 .
[0021] Charge management circuitry 40 monitors the battery pack 25 voltage during usage and provides a visual indication of current battery charge by illuminating a low battery indicator LED (not shown) when charge management circuitry 40 detects battery pack 25 voltage has dropped below a predefined minimum. LED power supply 45 regulates the battery voltage to provide a constant voltage to LED arrays 5 and 20 .
[0022] Microprocessor and motion-sensing circuitry assembly 15 contains electronics power supply 60 , motion sensor 65 , signal processor 70 , LED controller 75 , intensity selector 80 , pattern display selector 85 and color selector 90 . Electronics power supply 60 converts the voltage from battery pack 25 to the appropriate voltages and supplies the power to motion sensor 65 , signal processor 70 and LED controller 75 .
[0023] In one embodiment, motion sensor 65 is a programmable InvenSense 6500 or similar programmable sensor that monitors the movement of the wearer of the vest 1 and detects linear acceleration and deceleration in x, y and z axes and detects angular rate of rotation around each of the x, y and z axes. Motion sensor 65 also processes the acceleration/deceleration and rotation signals and provides data to signal processor 70 . Other motion sensors and more than one motion sensor may be used as well.
[0024] In one embodiment, signal processor 70 is a programmable Atmel ATmega 1284 or similar programmable processor that reads the data from motion sensor 65 . If signal processor 70 determines from the read data that a deceleration is occurring, the signal processor 70 transmits a signal to LED controller 75 .
[0025] In one embodiment, LED controller 75 is a programmable Atmel AT Mega 32U4 or similar programmable processor that monitors the signal from signal processor 70 and transmits a signal to LED arrays 5 and 20 . In one embodiment, the individual LEDs of LED arrays 5 and 20 are WS2812B RGB (red, green and blue) LEDs or similar LEDs with built in drivers that drive the individual red, green or blue diodes of each RGB LED based on data received from LED controller 75 . If the signal from signal processor 70 indicates no deceleration is occurring, LED controller 75 continually loops the selected display pattern through LED arrays 5 and 20 . The color and pattern configuration of LED arrays 5 and 20 are wearer selected and can be (i) a flashing or steady unchanging array; (ii) a flashing or steady program sequenced changing color array or (iii) a flashing or steady random color array. Various patterns may be stored in memory for access when needed. In one embodiment, each of the LEDs i s capable of displaying multiple colors. Besides LEDS, other illumination devices may be used.
[0026] The light intensity of the LED arrays 5 and 20 can be regulated by the wearer by pressing intensity selector switch 80 . Repeated pressing of the intensity selector switch 80 increases the LED light intensity until a peak intensity is reached. Pressing the light intensity switch 80 again repeats the process starting with the lowest light intensity and progressing to the peak intensity.
[0027] The color and pattern configuration of LED arrays 5 and 20 can be selected by the wearer pressing pattern display selector 85 and color selector 90 . Pressing pattern display selector 85 causes the pattern to cycle to the next available light pattern. Pressing color selector 90 causes the selected pattern to cycle to the next available color. The selected light pattern remains on until pattern display selector 85 is pressed again. The selected color remains on until color selector 90 is pressed again. If power is removed from vest 1 , the previously selected display pattern and color resume when power to vest 1 is restored.
[0028] If signal processor 70 determines from data received from motion sensor 65 that deceleration is occurring, signal processor 70 transmits a signal to LED controller 75 , which transmits a signal to LED array 20 on the rear surface of vest 1 causing the LED array 20 to revert to the “all red” state until such a time as signal processor 70 determines that the deceleration has ended. Such deceleration may be the result letting off the throttle, braking, downshifting and/or riding on upward-directed terrain. Once signal processor 70 determines that deceleration has ended, LED controller 75 resumes looping through the selected display pattern.
[0029] FIG. 4 illustrates a flow chart 100 detailing one methodology of operating said vest 1 according to the embodiments of the present invention. At 105 , the illuminated vest 1 is worn. At 110 , the vest 1 is configured as detailed above. At 115 , one or more motion sensors detect movement of said garment. At 120 , it is determined if deceleration has been detected. If not, the flowchart 100 loops back to 115 . If so, at 125 , a signal is transmitted to a light array controller. At 130 , responsive to receipt of said signal, said light array controller triggers one or more light arrays to illuminate in all red state notifying other traffic that said motorcycle or bicycle is decelerating.
[0030] While a motorcycle is used herein to describe the embodiments of the present invention, it is understood that motorcycle includes scooters, mopeds, three-wheeled vehicles (e.g., Trike) and four-wheeled vehicles (e.g., ATV). In addition, the garment system is also suitable for unpowered vehicles such as bicycles.
[0031] Although the invention has been described in detail with reference to several embodiments, additional variations and modifications exist within the scope and spirit of the invention as described and defined in the following claims.
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A garment (e.g., vest) designed to be worn over a motorcyclist's outer clothing with high intensity LED lighting installed on front and rear surfaces thereof and motion-sensing circuitry and corresponding software that detects motorcycle deceleration and controls the sequence, color and/or intensity of the LED lighting. A small, light battery pack installed in the garment powers the system. The motion-sensing circuitry and software detects that the motorcycle is decelerating when the driver releases or reduces the throttle, downshifts and/or applies the brakes. Responsive to the driver releasing or reducing the throttle, downshifting, applying the brakes and/or riding on upward-directed terrain, the electronics and software change the color output of LEDs on the rear surface of the garment to red. The electronics of the garment are sealed in watertight assemblies.
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CROSS REFERENCE TO RELATED APPLICATION
This application is a divisional application of copending application, Ser. No. 404,095, filed Nov. 5, 1973 and now U.S. Pat. No. 3,945,867.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a hose incorporating a cylindrical, braided, reinforcing means.
2. Description of the Prior Art
Flexible plastic hose has come into wide usage because of its ruggedness, resistance to deterioration, suitability for a wide variety of fluids, and other desirable properties. These uses range from sanitary applications in the food and drug industry to hydraulic and pneumatic applications, as in braking and other control systems. The latter may involve internal pressure of considerable magnitude, for example 500 psi working pressures and 2,000 psi burst strengths, or more. In order to provide light weight while at the same time providing the necessary strength to resist the circumferential and longitudinal forces exerted on the hose, reinforcement in the form of a surrounding tubular net is utilized.
A typical plastic hose includes an inner tubular core. Nylon is often used for this purpose because of its inertness, chemical properties, strength, and for other reasons. The reinforcing net is placed around the core and the composite structure coated with a plastic having abrasion resistance, coloration, and similar properties.
At present, many types of hoses constructed in accordance with the foregoing technique are prone to kinking and rippling when bent. When the hose is cut, the reinforcing net is subject to fraying and/or unraveling.
These defects are traceable to the lack of adequate adherence of the net and coating to the nylon core of the hose. While adhesion of the net to the core would overcome these defects, the lubricous properties which render nylon so suitable as a hose core material also make it difficult to join the net and coating to the core, as by glue or adhesives.
SUMMARY OF THE PRESENT INVENTION
It is, therefore, the object of the present invention to provide an improved plastic hose in which the net is secured to the core in an improved manner thereby overcoming the shortcomings noted above.
The present invention contemplates a plastic hose having an indirectly heatable bonding agent about the exterior of the core. The bonding agent is selected to be heat sealable to the core and to be thermally deformable. The reinforcing net is positioned around the bonding agent. The agent and net are brought into locking engagement, as by partially embedding the net in the agent, by heat induced deformation. The corenet assembly may then be coated. The article of the present invention thus exhibits mechanical joinder of the net to the agent and bonding joinder of the agent to the core. The mechanical engagement of the net and agent not only eliminates the kinking and fraying heretofore experienced, but also provides a smoother surface for the exterior coating of the pipe, through the partial embedment of the net in the agent. This reduces abrasion and wear.
Preferably, the agent has dispersed therein a particulate susceptor, heatable upon exposure to a selected form of indirectly applied energy, for example, a high frequency magnetic or electric field. Such susceptors may comprise inductively heatable metallic oxides such as an iron oxide, or dielectrically heatable compounds, such as polyvinyl chloride.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a perspective view of a plastic hose of the type to which the present invention pertains.
FIG. 2 is a cross-sectional view of a plastic hose showing the prior art construction.
FIG. 3 is a cross-sectional view similar to that shown in FIG. 2 showing a plastic hose constructed in accordance with the present invention.
FIGS. 4a through 4e show steps in the method of making the plastic hose of the present invention.
FIG. 5 shows an alternative step in the method for making the plastic hose of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Turning now to FIG. 1, there is shown therein plastic hose 10. Plastic hose 10 includes hollow core 12. Surrounding core 12 is a reinforcing net 14. Net 14 is formed of a lattice of strands 16 capable of receiving tensile forces and thus serves to resist the circumferential and longitudinal forces exerted on plastic hose 10 by the presence and passage of fluids through core 12. Coating 18 is provided over core 12 and net 14.
A plastic hose of the foregoing type constructed in accordance with the prior art is shown in cross section in FIG. 2. As will be noted from the Figure, strands 16 of net 14 lie along the exterior surface of core 12. This positioning, along with the absence of a bond between strands 16 and core 12, causes the kinking and rippling upon bending and the fraying and unraveling upon cutting noted earlier.
FIG. 3, on the other hand, shows the improved plastic hose 10a of the present invention. Plastic hose 10a includes core 12. Core 12 may be formed of a variety of materials. Nylon, typically nylon 11, may be used because of its strength and resistance to the effects of oil and water. Ethylene vinyl acetate may be used for food applications, such as milk handling.
In plastic hose 10a indirectly heatable bonding agent 20 is heat sealed to the exterior of core 12. Strands 16 of net 14 are at least partially embedded in agent 20 obviating the shortcomings heretofore encountered in the use of plastic hose. As noted supra, attainment of the features of the present invention depends on the mechanical engagement of the agent and net produced by this embedment and the heat seal between the agent and the core.
The bonding properties of agent 20 may be selected by considering its joinder to core 12. As such, bonding agent 20 may be a material similar to core 12, for example, a nylon 11 bonding agent for a nylon 11 core or a different material, the important consideration being the heat sealability or fusibility of the bonding agent to the core. Net 14 may be formed of orientable polymer yarn, typically polyester or nylon, or other suitable material. Bonding agent 20 typically posesses substantial bonding incompatability with net 14. Strands 16 of net 14 may be woven or braided or may comprise a plurality of parallel filaments as in a roving. Strands 16 may or may not intersect and may or may not be knotted at their intersections in forming net 14. With certain types of net and bonding agent materials, a greater or lesser amount of bonding may occur between these two elements but the primary coaction between the elements is the mechanical engagement noted above.
In order to provide this mechanical engagement the layer of bonding agent must be of appreciable thickness. While the exact thickness of the layer depends to some extent on the diameter of strands 16 and their material type, the layer of bonding agent is typically 5 to 10 mils (0.005-0.01 inch) thick. This is considerably in excess of adhesive coatings which tend to be less than 2 mils in thickness.
Another feature of the present invention is the manner in which the heating of bonding agent 20 is obtained. As can be appreciated, it is difficult to heat agent 20 with conventional means such as burners and heated platens and, at the same time, apply net 14. External heat also is likely to damage net 14.
The present invention therefore contemplates rendering the agent itself heatable upon exposure to a selected form of indirectly applied energy. By the term "indirectly applied" is meant that the energy is applied in the form of an electromagnetic field, for example, alternating magnetic or electric fields, rather than through the direct application of heat as by heated platens and the like. This may be accomplished by dispersing in agent 20 a particulate susceptor 22 heatable upon exposure to the indirectly applied energy, as shown in FIG. 3.
In the instance in which the indirect energy is applied in the form of an alternating magnetic field, susceptor material 22 may comprise an inductively heatable substance. Susceptors comprising, at least in part, non-conductive metallic oxides having ferromagnetic properties are suitable for use as an inductively heatable susceptor material. Ferrite materials may be used. The oxide compounds gamma Fe 2 O 3 , Fe 3 O 4 , and CrO 2 have been found to be useful susceptor materials. In addition to their high heat generating properties by hysteresis losses, such compounds may be reduced to extremely small size. This size reduction is without loss of heat generating properties and facilitates the dispersion of susceptor 22 in agent 20. Metallic oxide susceptors may be reduced to submicron particle sizes, for example, 0.01 microns. A typical maximum particle size is 20 microns.
In the instance in which the indirect energy is applied in the form of an alternating electric field, susceptor 22 may comprise a polar material heatable by dielectric losses. The polymers and copolymers of vinyl chloride, vinyle fluoride, vinylidene chloride, and vinylidene fluoride are suitable for use as dielectrically heatable susceptors. Polyvinyl chloride has been found useful.
Turning now to FIG. 4, typical steps in the process of making plastic hose 10a are illustrated. A hollow plastic core 12 shown in FIG. 4a is provided by conventional methods. Bonding agent 20 containing dispersed susceptor particles 22 may be obtained by a plurality of methods. For example, the granulated thermoplastic material of agent 20 and the particulate susceptor material 22 may be dry mixed together in the desired quantities in preparation for application to core 12. Depending on the type of thermoplastic material comprising agent 22 and the degree of dispersion desired, it may be necessary to pass this admixture through an extruder, regranulate the once extruded composition and reextrude it, as for example, directly on to the core.
More specifically, the bonding agent may be coextruded on the exterior of core 12 as the core is formed or the bonding agent may be extruded on an already formed core. The bonding agent may be formed as a film and wrapped on the exterior of core 12 or applied in liquid form. Yet another alternative is applying bonding agent 20 to strands 16 so that the bonding agent is applied to the core as net 14 is formed. The efficiencies obtainable by the process of the present invention permit the use of relatively low particle loading, for example 3 to 10% (preferably 8 to 10%) by weight with respect to the bonding agent 20.
Net 14 is then placed or drawn on the exterior of agent 20 as shown in FIG. 4C, by conventional means. Thereafter, core 12, agent 20, and net 14 are passed through induction heating coil 24. See FIG. 4D. Induction heating coil 24 is energized by high frequency alternating current power supply 26 so as to generate a high frequency magnetic field in the interior of the coil. A frequency range for the magnetic field of from 0.4 to 6 megahertz has been found suitable although useful heat is also achieved at higher frequencies up to a typical maximum of 30 megahertz for a conventional coil. The energization of coil 24 applies a high frequency magnetic field to agent 20 which generates heat in susceptor particles 22 causing the agent to become heated and deformable so as to permit the embodiment of strands 16 in the exterior of the core and the heat sealing of agent 20 to core 12. The embedment may be accomplished by the exudation of the hot bonding agent through the openings in net 14, by the circumferential tension existing in strands 16 and by any thermo-shrinking of strands 16 which may be present. A pressure means (not shown) may be applied to the exterior of agent 20.
The amount of time that agent 20 must be exposed to the magnetic field of coil 24 depends on the type of material utilized for agent 20, the concentration of susceptor material 22, the degree of embedment of strands 16 desired, the strength and frequency of the magnetic field, and other factors. However, because of the efficiencies obtainable with the technique of the present invention, only a short period of time is normally required to obtain the necessary softening of the exterior of agent 20. Times less than one second are common. In the case in which plastic hose 10 is being continuously formed in a processing line, the exposure time may be regulated by the velocity at which the hose passes through heating coil 24.
After passing through induction heating coil 24, agent 20 having net 14 embedded therein may be cooled by air blasts or the like. Agent 20 and net 14 are then coated with coating 18 as by spray guns 29 or by some other means such as a coater, extruder, brushes, or the like. See FIG. 4E. Coating 18 may typically be urethane rubber. This completes the manufacture of plastic hose 10a. It will be appreciated that coating 18 may be applied prior to heating bonding agent 20 if desired.
In the instance in which susceptor particles 22 are dielectrically heatable, a high frequency electric field may be formed between two plate-like electrodes 30 connected to high frequency generator 32, as shown in FIG. 5.
A typical embodiment of the invention comprises a hose having a nylon 11 core. A concentric coextruded layer of nylon 11 bonding agent 10 mils thick and containing 10% by weight of gamma Fe 2 O 3 particles is provided over the core. The net is formed of polyester yarn. The outside diameter of the product is approximately 0.6 inches.
The induction heating coil utilized to treat the hose described above consisted of two parallel windings providing a total of 28 turns of 3/16 inch insulated tubing. The axial length of the coil was 6/182 inches. The coil was energized by an induction heating generator operating at approximately 3.5 MHz with approximately 200 amperes of r-f current feeding each winding.
The velocity at which hose 10a passed through the coil was such as to expose a given point on the hose to the magnetic field of the coil for 0.6 seconds. This exposure caused sufficient melting of the nylon bonding agent to cause the nylon to exude outward through many small openings in the net and become visible on the exterior of the net in small quantities, thus locking the net to the core upon cooling. The product was suitable for receiving a coating of urethane rubber.
Various modes of carrying out the invention are contemplated as being within the scope of the following claims particularly pointing out and distinctly claiming the subject matter which is regarded as the invention.
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A hose includes a hollow plastic core having an indirectly heatable agent bonded to the exterior thereof by a heat seal. A reinforcing net is embedded in the agent and the composite structure covered with a coating.
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BACKGROUND OF THE INVENTION
The present invention is directed to a method, apparatus and tool for providing an improved soldered electrical connection. More particularly, the present invention is directed to a ring which is provided over an electrical wire and terminal, and compressed before soldering, by the use of a special tool.
The soldering of wires to terminals to make electrical connections has been used for many years. A relatively common problem in the soldering of wires to terminals is the production of cold soldered joints. Cold soldered joints often result from the movement of the wire relative to the terminal prior to the cooling of the solder. Attempts in the past to obviate this problem have included the winding of the wire around the terminal prior to soldering. However, the winding of a wire around the terminal has proved to result in other problems. For example, in the event of a severe overheating due to a severe electric current overload, the solder may melt and the wire wound around the terminal may unwind due to the spring force of the wound wire. Upon cooling, the soldered connection is not properly remade due to the unwinding, and therefore, a good electrical connection is not maintained.
SUMMARY OF THE INVENTION
The present invention provides a method, apparatus and tool for the making of an improved soldered electrical connection between a terminal and wire. The present invention provides several advantages, inter alia, the making of a strong mechanical connection between the wire and the terminal before soldering the wire to the terminal. This mechanical connection insures that a substantial length of the wire is maintained in intimate contact with a substantial length of the terminal. The mechanical connection prevents movement of the wire during the soldering process thereby preventing the formation of cold solder joints. Cold solder joints are typically caused by the movement of the wire before the solder has cooled thereby resulting in a high resistance electrical connection and generally a poor electrical connection. The mechanical connection provides the additional advantage of maintaining the wire in contact with the terminal in the case of a severe overheating of the electrical connection, which might even result in the melting of the solder. Such overheating might occur on a severe electrical overload. In such a case, an electrical connection is maintained by means of the mechanical connection, and, a new soldered electrical connection, of good quality, may be maintained due to the fact that the wire is held without movement in its normal position against the terminal by means of the compressed ring connector of the present invention.
Briefly, in accordance with the method of the present invention, an improved method of making an electrical connection between a wire and a terminal includes the step of providing a ring, preferably a split ring, having an inside diameter of sufficient dimension to allow said ring to fit over a terminal to which a wire is to be bonded. The method further includes the step of installing the split ring over the terminal, the wire to be bonded being inserted within the ring in juxtaposition to the terminal. The method further includes the step of compressing the split ring onto the terminal and the wire to form a mechanical connection between the terminal and the wire, and then soldering at least the wire to the terminal. Preferably, the split ring is provided with a solderable surface and the terminal, wire and compressed ring may be soldered together as a unit. Further, in accordance with a preferred method of the present invention, a tool may be utilized which is provided with pivoted jaws having slots formed therein for receiving the ring on end.
Further, in accordance with the present invention, the ring is preferably divided radially with the free ends thereof being offset one from the other to enable the sliding of the ends past each other upon compression of the ring. Preferably, the inside diameter of the ring is selected to provide minimal clearance over the terminal. In the case of terminals having a "T" shape, as is common, the inside diameter of the split ring is preferably selected to provide minimal clearance over the top of the "T" of the "T" shaped terminal whereby after compression of the split ring, the compressed split ring is locked under the top of the "T" shape of the terminal.
Further, in accordance with a preferred embodiment of the present invention, the inside diameter of the ring is selected to provide clearance over the top of a "T" of a "T" shaped terminal and is selected of minimal dimensions so that when it is placed over the terminal and a wire to be soldered is inserted between the inside diameter of the ring and the terminal, the ring is drawn under the top portion of the "T" of the "T" shaped terminal so that the rings may not be slipped off the top of the terminal with the wire in place.
In accordance with the present invention, a tool is provided for the making of the improved soldered electrical connection. The tool comprises a pair of members pivoted together between their ends. Each member is provided with a mating jaw formed at one end and a handle at the other. A longitudinal slot is provided in each jaw for receiving a split ring on end. The split ring may therefore be conveniently held for mounting over the terminal and during the process of inserting the wire to be soldered therein The handles of the tool may then be conveniently pressed together to compress the split ring onto the terminal and the wire to be soldered.
It is understood that the term solder means any metal or metalic alloy used when melted to join metalic surfaces and soldering means the uniting of elements by the use of such solder.
BRIEF DESCRIPTION OF THE DRAWINGS
For the purpose of illustrating the invention, there are shown in the drawings forms which are presently preferred; it being understood, however, that this invention is not limited to the precise arrangements and instrumentalities shown.
FIGS. 1 through 4 are elevation views, with the tool shown in cross-section similar to that of FIG. 7, of several of the steps of making an improved soldered electrical connection in accordance with the present invention.
FIG. 5 is a view in perspective of a split ring utilized in the making of an improved soldered electrical connection in accordance with the present invention.
FIG. 6 is an elevation view of a tool, with a split ring held on end in the jaws thereof, used in the making of an improved soldered electrical connection in accordance with the present invention.
FIG. 7 is a cross sectional view taken along line 7--7 of FIG. 6.
FIG. 8 is an elevation view of a portion of a terminal board having several terminals thereon with a wire mechanically connected to one of the terminals in accordance with the present invention.
FIG. 9 is a plan view of an unsplit ring, which may be substituted for the split rings shown in FIGS. 1 thru 8.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings in detail wherein like numerals indicate like elements, there is shown in FIGS. 1 through 4 several of the steps in the method of making an improved soldered electrical connection. Referring to these Figures, there is shown a split ring 10 held within the jaws 12 of a tool 14. The split ring 10 is being inserted on a terminal 16. An electrical wire 18 having insulation 20 is shown being mechanically connected to the terminal.
Referring now particularly to FIG. 1, there is shown a split ring 10 held on end within the grooves or slots 22 formed within jaws 12 of tool 14.
The split ring 10 is about to be placed over terminal 16. This is illustrated in FIG. 2. The wire 18 may be then inserted along the length of terminal 16 and through split ring 10. Pressure may then be applied to the handles 24 (FIG. 6) of tool 14 to compress split ring 10 onto wire 18 and terminal 16.
Although the aforesaid steps are deemed to be the preferred and best manner of practicing the method of the present invention with respect to the forming of a mechanical bond between the wire and the terminal, it is understood that the steps may be carried out in differing sequences within the scope of the present invention. For example, the wire 18 may be first placed through split ring 10, and then wire 18 and split ring 10 inserted over terminal 16.
Once the mechanical connection between the wire 18 and the terminal 16 is made, as illustrated in FIG. 4, the wire 18 is soldered to terminal 16. Preferably, split ring 10 is provided with a solderable surface, and split ring 10, wire 18 and terminal 16 may be soldered together as a unit.
The split ring 10 is further illustrated in FIG. 5. As may be seen from FIG. 5, taken in conjunction with the other figures in the drawing, split ring 10 is comprised of a ring which is divided or split radially at 26. The free ends of the split or divided ring 10 are offset one from the other to aid in or allow the free ends to slide past each other upon compression of the ring. This is particularly well illustrated in FIGS. 2 through 4. Split ring 10 may be comprised of any suitable material which is bendable so that the ring may be compressed and has sufficient rigidity so that it retains its bent or compressed condition to provide sufficient force on wire 18 and terminal 16 to retain wire 18 against terminal 16. Preferably, split ring 10 may be comprised of bronze, or other suitable material. Preferably, the material of split ring 10, such as bronze, may be tinned to enhance the solderability of split ring 10.
Although a split ring structure, such as split ring 10, with offset free ends is a preferred embodiment of the present invention, it is understood that a ring may be utilized which is not radially divided, such as ring 40 in FIG. 9. Ring 40 may be utilized in the same manner as described throughout for split ring 10 except that there would be no free ends which would readily slide past each other upon compression of the ring. Instead, ring 40 would be compressed upon the terminal and the wire causing bending and deformation of the ring structure so that the wire is compressed and held tight against the terminal. Preferably, ring 40 may be comprised of a somewhat more deformable material, such as copper, rather than bronze, but other suitable materials, including bronze, may be utilized. As in the case of split ring 10, ring 40 may be tinned to enhance the solderability of ring 40. The dimensions of ring 40 may be selected with the same considerations as set forth above and hereinafter with respect to ring 10.
Referring to FIG. 6, there is shown a tool which may be of substantial benefit and assistance in carrying out the method of the present invention, especially where the method and apparatus of the present invention in producing the improved electrical connections are to be carried out rapidly and efficiently, for example, in a production assembly line. The tool as illustrated in FIG. 14 is comprised of two members plvoted together between their ends at point 28. The members are provided with handles 24 at one end and with mating jaws 12 at the opposite end The jaws 12 are provided with mating longitudinal slots 22 for receiving split ring 10 on end therein. This is illustrated further in FIG. 7, along with the illustrations of FIGS. 1 through 4. Preferably, the depth of slots 22 is equal to the width of the member making up split ring 10. In other words, as may be seen in FIGS. 6 and 7, the depth of the slot 22 is preferably selected so that the remainder of the jaw extends to the inside diameter of split ring 10. By such selection of the slot depth, the possibility of excessive pressure of the ring on the wire and the terminal is prevented, thereby avoiding any possible cutting of the wire during compression of the ring. However, the invention herein is not limited to this best mode, and other slot depths may be used in practicing the invention with or without a stop means.
Referring to FIG. 8, there is shown a terminal block 30 provided with "T" shaped terminals 32. The "T" shaped terminal 32 is shown extending (in dotted lines) within an insulative cylinder as is conventional on terminal blocks. As shown on the middle terminal, the inside diameter of split ring 10 is preferably selected to provide minimum clearance over the top of the "T" terminal. By preferably selecting a split ring 10 having an inside diameter which provides minimal clearance over the top of the "T" terminal, compression of split ring 10 results in the ring being locked under the top of the "T" as shown on the left terminal. Although the locking of the compressed split ring 10 under the top of the "T" terminal is desirable, the present invention may be utilized with straight terminals 36 as shown in FIG. 8. In such a case, the compression of the split ring on the straight terminal and the wire provides a sufficiently strong friction bond between the wire and the terminal to hold the wire mechanically bonded to the terminal.
Additionally, in the case of "T" shaped terminals, the inside diameter of the ring is selected to clear the top of the "T" of the terminal and so that when it is placed on the terminal and the wire is inserted between the inside diameter and the terminal, the ring is drawn under the top of the "T" of the "T" shaped terminal, and the ring may not be slipped off the top of the terminal with the wire in place. The ring may then be compressed and the terminal, wire and ring soldered together as described above. In this manner, the ring is locked in place prior to soldering, and is permanently locked in place after soldering.
The present invention a described provides a number of significant advantages in the making of a soldered electrical connection between a wire and a terminal. In accordance with the present invention, the wire to be soldered to the terminal is firmly held against a substantial length of the terminal during the soldering process without any movement between the wire and the terminal. This insures a good soldered connection between the wire and a substantial length of the terminal. The prevention of movement during the soldering helps insure against the formation of a cold soldered joint. Furthermore, once the electrical connection is put into use, a substantial degree of protection is provided against the possibility of an electrical connection being lost during an overheating of the electrical connection. This is so because the wire is firmly maintained in its normal position in contact with the terminal by means of the mechanical connection formed by the compressed split ring. This also enables a good soldered connection to be reformed upon the cooling of the soldered terminal after the overheating condition passes. Furthermore, with the use of the tool of the present invention, electrical connections in accordance with the present invention may be made even more rapidly than by the conventional method of attempting to hold a wire in contact with the terminal during the soldering process.
The present invention maybe embodied in other specific forms without departing from the spirit or essential attributes thereof and, accordingly, reference should be made to the appended claims, rather than to the foregoing specification as indicating the scope of the invention.
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The method of providing an improved soldered electrical connection includes the step of providing a ring over an electrical wire and a terminal which are to be soldered together, and then compressing the ring to form a mechanical connection between the wire and the terminal prior to soldering. The mechanical connection holds the wire for a substantial length against the terminal and prevents movement during the soldering thereby insuring against a cold solder joint. Preferably, the ring is divided with the free ends preferably being offset to provide ease in sliding past each other. Preferably, a specially designed tool is utilized to compress the ring, the tool being provided with specially designed grooves in its jaws for holding the ring on end.
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BACKGROUND
Subsurface drip disposal (“SDD”) systems are systems for disposing of wastewater such as septic tank effluent and the like. Subsurface drip disposal provides a shallow, slow rate, pressure-dosed system used for land application of pretreated wastewater. In general, SDD systems are characterized by: (1) uniform distribution of effluent, (2) dosing and resting cycles, and (3) very shallow placement of trenches. SDD systems typically use small diameter piping with subsurface drip emitters. The effluent must be adequately filtered before distribution through the underground emitter system, and filters and the piping network must be routinely flushed or otherwise cleared of trapped particles.
Well-designed SDD systems distribute effluent uniformly at a relatively low application rate over an absorption field, also called the drip field. Waste fluids are applied at a controlled rate in the plant root zone, which tends to minimize percolation of the effluent. Hydraulic loading rates may vary, for example between 0.1 and 1.6 gallons per day per square foot.
Conventional SDD systems include valving and control systems referred to as headworks that direct and control the flow of the effluent. In a conventional SDD system the headworks include two or three solenoid valves that control the timing and sequence of fluid flows. A conventional SDD system may include a tank wherein the effluent is accumulated for dispersal, a pump for removing effluent from the tank, a supply manifold and return manifold, and a number of emitter lines that extend between the supply and return manifolds and are disposed in the drip field. The emitter lines include a number of small emitters distributed along their length through which the effluent is dispersed in the drip field.
In a typical conventional SDD system the pump is periodically engaged, and a first solenoid valve is opened, to send flow to the drip field for dispersal through the drip emitters. A valve on the return manifold is typically closed such that the pumped fluid flows uniformly away from the tank, and is dispersed through the emitters. This is typically referred to as “dosing” cycle, and may occur, for example, twelve times a day, for periods of 5-10 minutes. It will be appreciated that this frequency and duration for the dosing cycle is by way of example, and the actual timing selected will depend on the particular application.
In order to avoid accumulation of matter in the emitter lines and manifolds, cooperatively referred to herein as the “field piping network”, a conventional SDD system will periodically engage a field piping network flushing cycle wherein relatively high-velocity effluent is pumped through the field piping network to clean out the pipes, with the valve for the return manifold open such that the effluent is partially returned to the tank. The minimum required fluid velocity for the flushing operation is often specified by local and/or state regulations. The field piping network flushing cycle may be engaged, for example, every 12-48 hours, and typically pressurizes the entire system such that effluent is also dispersed to the drip field, although the amount of such dosing is typically difficult to determine and/or unknown.
A conventional SDD system also includes a filter that prevents or reduces the amount of solid matter that is pumped from the SDD tank to the emitter lines, in order to prevent clogging of the emitters. Conventional SDD systems periodically engage a filter flush cycle wherein a third valve is opened to allow flow to go through a filter flushing port and return to the tank. In the filter flushing cycle fluids at a relatively high velocity are provided to remove matter from the filter. Typically the pump pressurizes the entire system, resulting in effluent also being dispersed through the emitters, although again the amount of fluid discharged may be difficult to determine or predict. In an exemplary septic tank application, a filter flush cycle may be engaged once for every 5-20 dose cycles.
SDD systems, particularly in cold weather climates, are designed and installed to drain back from the field piping (e.g., the emitters and plenums) into the dose tank after each dose, so that effluent does not freeze in the lines, potentially damaging the system. However, the headwords active valving systems used in most conventional SDD systems tend to interfere with proper drainage from the field piping, which can result in damage to the field piping network Moreover, the valving systems add significant costs and complexity to the drip disposal system. In addition, conventional SDD systems require three different pumping operations. There is one pressure and flow requirement for dosing the field, a different pressure and flow requirement for flushing the field piping network, and a third flow and pressure requirement for flushing the discharge filter. The differences in these three operating conditions make it difficult to select a suitable pump, and requires operation of the selected pump at non-optimal conditions at least some of the time.
To avoid the disadvantages associated with conventional SDD systems having headworks, a system without full headworks has been proposed in Design & Performance of Drip Dispersal Systems in Freezing Environments (published online at http://www.geoflow.com/research_w.html), by S. Wallace. However, the systems described therein include a solenoid valve for drain back of the effluent, and a throttle valve on the return head. Moreover, the disclosed system does not appear to include a filter, or means for flushing a filter.
SUMMARY
This summary is provided to introduce a selection of concepts in a simplified form that are further described below in the Detailed Description. This summary is not intended to identify key features of the claimed subject matter, nor is it intended to be used as an aid in determining the scope of the claimed subject matter.
A subsurface drip effluent disposal system is disclosed having a wastewater tank, such as a septic effluent tank, and a subsurface field piping network for dispersing flow from the tank. A pump is provided in the tank that pumps fluids through a discharge line to a discharge filter that is capable of simultaneous flushing and filtering. A spin filter is a suitable type of discharge filter. A portion of the flow received by the discharge filter is used to flush the filter and returns to the tank, and another portion of the flow is discharged to the field piping network. The field piping network includes a supply manifold that is fluidly connected to one end of a plurality of emitter lines having spaced apart emitters for discharging a portion of the flow. The opposite end of the emitter lines are connected to a return manifold that returns a portion of the flow to the tank. Flow restrictors are provided, preferably on the filter flush return line, and on the field return line, such that the flow split between the filter, the filter flush return, the drip dose, and the field return can be predetermined. The present system simultaneously flushes the discharge filter, doses the field, and flushes the field piping network, and does not require the use of active headworks, such as a solenoid operated valve systems.
DESCRIPTION OF THE DRAWINGS
The foregoing aspects and many of the attendant advantages of this invention will become more readily appreciated as the same become better understood by reference to the following detailed description, when taken in conjunction with the accompanying drawings, wherein:
FIG. 1 is a perspective view of an exemplary subsurface drip effluent disposal system in accordance with the present invention, shown in isolation for clarity;
FIG. 2 is a partially side view of the wastewater tank shown in FIG. 1 , shown installed with the tops of the risers at approximately ground level;
FIG. 3A is a three-quarter front perspective view of the piping in the first riser of the wastewater tank shown in FIG. 1 ;
FIG. 3B is a three-quarter rear perspective view of the piping in the first riser of the wastewater tank shown in FIG. 1 ; and
FIG. 4 is an exploded perspective view of an exemplary flow restrictor for the drip effluent disposal system shown in FIG. 1 .
DETAILED DESCRIPTION
A perspective view of an exemplary subsurface drip effluent disposal system 100 in accordance with the present invention is shown in FIG. 1 . The disposal system 100 includes a wastewater tank 102 , for example a septic system effluent tank, which are well-known in the art. For example, the wastewater tank 102 may be an injection-molded fiberglass-reinforced polyester septic tank. The exemplary wastewater tank 102 shown in FIG. 1 includes oppositely-disposed first and second risers 104 and 106 , respectively. Of course, other suitable tank construction may alternatively be used. A tank fluid inlet 108 provides a fluid conduit for supplying fluids to the wastewater tank 102 . In a current embodiment of the drip effluent disposal system 100 , for example, the inlet 108 is formed from four inch ABS piping. The inlet 108 may be fluidly coupled to a pretreatment tank or system (not shown), for example to substantially remove solids and/or harmful organisms, from the wastewater.
A supply manifold 110 , extends from the wastewater tank 102 , terminating in an air/vacuum relief valve 112 . A plurality of generally U-shaped emitter lines 115 are provided having a first end 114 fluidly connected to the supply manifold 110 , and a second end 116 fluidly connected to a return manifold 120 . The emitter lines 115 include a number of spaced emitters (not shown), as are well-known in the art. For example, pressure-compensated emitters are adapted to produce a relatively constant outflow over a range of fluid pressures. Non-pressure-compensated emitters may alternatively be used. The inflow manifold 120 terminates at one end with a second air/vacuum relief valve 112 , and at the other end returns to the tank 102 through a field return line 154 . A portion of the effluent pumped through the emitter lines 115 is expelled through the emitters, thereby dosing the drip field. It will be appreciated by the artisan that in a typical alternative configuration the supply manifold 110 and return manifold 120 may be spaced a distance apart, with the emitter lines 115 extending therebetween.
In regions where freezing is a consideration, the emitter lines 115 are generally installed to slope towards the supply manifold 110 and/or the return manifold 120 such that when the system 100 is not pressurized, fluid in the emitter lines 115 will be gravity-driven towards one or both of the manifolds 110 , 120 . In these regions it is desirable that the emitter lines 115 not have any sag that would trap fluids therein. The supply manifold 110 and return manifold 120 are installed to slope towards the wastewater tank 102 , such that when the system is not pressurized, fluid in the manifolds 110 , 120 will flow under gravity towards the wastewater tank 102 . In regions where freezing is not a consideration, the grading of the field piping is not a primary consideration.
Refer now to FIG. 2 , which shows an installed, partially cut-away side view of the wastewater tank 102 . In the disclosed embodiment, a pump 131 is disposed in a pump package 130 , which may include other related components such as waste filtering and/or treatment components 132 such as products marketed by Orenco Systems, Inc. under the trademark Biotube®. A pump discharge line 133 receives effluent from the pump 131 , which is thereby delivered under pressure to the supply manifold 110 ( FIG. 1 ). A manual shutoff valve 134 may be provided on the discharge line 133 . A conventional junction box 125 is conveniently disposed in the second riser 106 , for providing electrical power to the system 100 .
Refer now also to FIG. 3A and FIG. 3B which show the piping in the first riser 104 (the first riser 104 is shown in phantom, for clarity), from different perspectives to better show the piping. FIG. 3A shows a generally three-quarter front perspective view and FIG. 3B shows a generally three-quarter rear perspective view. The discharge line 133 is fluidly connected to a discharge filter 136 that is capable of simultaneously filtering effluent and flushing the filter 136 , for example a spin filter. The discharge filter 136 removes solids from the effluent prior to its discharge into the supply manifold 110 . The discharge filter 136 has one end attached to a filter flush return line 138 that returns effluent with filtered solids captured by the discharge filter 136 to the wastewater tank 102 . A first flow restrictor 140 is disposed between the discharge filter 136 , and the discharge filter flush return line 138 . Suitable flow restrictors are known in the art. An exemplary flow restrictor 140 having a flow balance orifice 146 is shown in FIG. 4 . In this embodiment, the first flow restrictor 140 includes a fitting 142 that supports a disk-shaped blocking member 144 with a calibrated aperture 146 therethrough, and a second fitting 143 that is attachable to the first fitting 142 , as shown. An o-ring 145 provides a seal about the flow balance orifice 146 . The function of the first flow restrictor 140 is discussed in more detail below.
An optional flow meter 150 and pressure gauge 152 are also provided on the discharge line 133 , upstream of the supply manifold 110 .
Referring again to FIG. 1 , the effluent flow through the supply manifold 110 is distributed to the emitter lines 115 , where a portion of the flow is dosed to the drip field. A portion of the effluent flow enters the return manifold 120 , and is recirculated back to the wastewater tank 102 . The return manifold 120 fluidly connects to a field return line 154 that extends into the wastewater tank 102 . Referring now again to FIG. 3A and FIG. 3B , the field return line 154 includes a second flow restrictor 148 (discussed below) located prior to the return flow being discharged into the wastewater tank 102 . The second flow restrictor 148 is similar in structure to the first flow restrictor 140 shown in FIG. 4 . An optional pressure gauge 152 is also provided on the field return line 154 .
The operation of the present subsurface drip effluent disposal system 100 will now be described. Generally at prescheduled intervals the pump 131 is activated and pumps fluids from the wastewater tank 102 through the discharge line 133 . As the flow encounters the discharge filter 136 , a portion of the flow flushes the discharge filter 136 and returns to the wastewater tank 102 through the filter flush return line 138 , and a portion of the flow is discharged to the supply manifold 110 . The supply manifold flow is then distributed to the emitter lines 115 , wherein a portion of the effluent is dosed to the drip field, and a portion is returned to the return manifold 120 , and thereby to the wastewater tank 102 , with flow velocities throughout the field piping network that are sufficient to flush the pipes. For a given effluent disposal system 100 , the flow splits between the filter flush portion, the field dose portion, and the piping flush portion are determined by the size of the apertures in the first and second flow restrictors 140 , 148 .
Frequently, subsurface drip effluent disposal systems must comply with local regulations, manufacturer recommendations and/or practical limitations regarding the amount of dosing that can be applied to a given drip field over a given period of time, piping network flushing flow velocity requirements, and filter flushing requirements.
With the present system, the dosing operation, piping network flushing and filter flushing can occur simultaneously. In particular, as disclosed herein the design of the SDD system can be accomplished using the following steps:
1. Specify the required wastewater discharge rate, for example in gal/day.
2. Identify the drip field soil type, and the allowable loading rate, for example in gal/ft^2/day.
3. Determine the emitter flow rate, the number of emitters required and the emitter lateral and in-line spacing requirements.
4. Calculate the required dimensions of the drip field.
5. Determine the piping flushing and filter flushing minimum flow requirements.
6. Determine the size of the supply manifold, emitter lines, and return manifold required to achieve the desired minimum flushing velocities.
7. Determine the optimal field piping network pressure, and pressure range for emitter lines.
8. Calculate the flow restrictor sizes required to achieve the desired flow splits to produce the desired minimum flow velocity in the field piping network, and to achieve the desired dosing and filter flushing flow rates.
It will be appreciated that the above method permits the calculation of the flow rate and head or piping pressures, which allows selection of the appropriate pump size. In order to optimize the system, a standard pump size may then be selected and the flow restrictor sizes re-optimized for the selected pump. Typically, the filter flushing flow rate may be increased to improve filter flushing without adversely impacting the pressure in the field piping network.
The SDD system 100 disclosed above provides significant advantages over the prior art. The active headworks with electronically-controlled valves is eliminated. Flow restrictors are provided that may be fixed aperture or pre-set upon installation. Although fixed aperture flow restrictors are shown and currently preferred, it is contemplated that the flow restrictors 140 , 148 may alternatively be field-adjustable, such that the user may adjust the system, for example to optimize the flow rates during installation. The elimination of the headworks reduces cost and complexity, and increases the reliability of the system by promoting complete drain back to the tank between dosing cycles.
It will be appreciated that the present system and method provides for a uniform pumping cycle that simultaneously doses the drip field, flushes the discharge filter, and flushes the piping network. A properly designed system will achieve the requisite fluid velocities and flows required. This configuration reduces the number of times that the pump must be activated, and permits the designer to select an optimal pump size. In prior art systems wherein the flushing and dosing operations are separately conducted, the required flow rates are dramatically different, resulting in the pump operating outside of its optimal range for many cycles. The present system and method provides for a single dosing/flushing operation, and therefore one pump operating condition, allowing selection of a pump that will operate at or near its best efficiency point.
While illustrative embodiments have been illustrated and described, it will be appreciated that various changes can be made therein without departing from the spirit and scope of the invention.
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A subsurface drip wastewater disposal system and method are disclosed that eliminate the need for headworks, reduce the risk of damage to the system, and permit optimal pump sizing by simultaneously dosing, flushing the pipe network and flushing the filter. A tank and pump package provide effluent under pressure to the field piping network comprising a supply manifold, a return manifold, and a plurality of emitter lines. A discharge filter that is capable of simultaneous filtering and flushing is provided on the discharge line, and a first flow restrictor is provided on the filter flush return line. Effluent is discharged at a rate and pressure that permits simultaneous pipe flushing and dosing, with the return manifold returning to the tank through a field return line having a second flow restrictor. The size of the first and second flow restrictors is selected to provide the desired flow splits.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The field of the present invention relates to frame quilting machines which are large table-like structures used to sew patterns into large textile items; in particular bedspreads and quilts. The field of the present invention also relates to industrial sewing machine apparatus and processes used to sew patterns and stitching into large fabrics, which sewing operation is not easily performed on conventional sewing machine. The field of the present invention also relates to machines which include a method of duplicating a selected pattern over an entire bedspread or quilt. Finally, the field of the present invention relates to computer controlled quilting machines wherein the stitching pattern of the sewing machine head and the table movement of the frame relative to the sewing machine head are both controlled by computers or process controllers.
2. Description of the Prior Art
Industrial sewing machine operations are known in the prior art. Patterns and stitching into fabrics is commonly performed on industrial sewing machines. The operator hand guides the fabric between the needle and the sewing machine table and the pattern is sewn into the fabric. This process is practical for small pieces of fabric and is commonly done on piece goods such as garments. When handling larger pieces of fabric such as a roll of fabric, a metnod known in the prior art is roll to roll sewing. The sewing machine head is located along an X-axis and the material is unwound from a roll and caused to move transverse to the sewing machine head such that the fabric moves along a Y-axis. The sewing machine sews a stitch into the large fabric as the head moving along the X-axis and the fabric moving along the Y-axis intersect each other. The fabric is then wound onto a second receiving roll.
When sewing a very large piece of fabric such as a bedspread or quilt, a frame quilting machine is used. The frame quilting machine comprises a large frame, usually made of metal, onto which the fabric to be sewn is spread. Commonly, the pattern is sewn by a sewing machine guided by a computer into which a predetermined pattern has been programmed. The fabric remains stationary on the frame and the sewing machine head moves along the fabric and stitches in the predetermined pattern.
The current method for computer programmable quilting patterns uses a digitizer/cursor board with a method of plotting patterns. It is also used in the design of patterns and is accomplished on a scaled down version of the patterns. Plotting is accomplished using a mouse for indexing points on an XY axis. The points are programmed and followed through use of the computer. The prior art uses standard patterns which are preprogrammed into the computer and selected individualized patterns which are created as the bedspread or quilt is on the machine.
A major problem with all prior art embodiments is that the stitching function of the sewing machine needle and the frame table movement in the X and Y directions are controlled by a single computer. As a result, when it becomes necessary to program or reprogram the machine for a new stitch or pattern, or to make modifications in the existing stitch or pattern, all of the movements in the stitch function and table movement function must be reprogrammed. This results in an enormous amount of work in that thousands of combined stitch and movement operations must be reprogrammed and the effort takes many hours and sometimes days.
The inventors have previously filed three patent applications which are presently co-pending. These patent applications are as follows:
1. Patent application Ser. No. 07/220,734 filed 07/18/88 for "Automatic Quilting Machine For Specialized Quilting Of Patterns Which Can Be Controlled By A Remote Joy Stick And Monitored On A Video Screen".
2. Patent application Ser. No. 07/247,696 filed 09/22/88 for "Automatic Quilting Machine For Specialized Quilting Of Patterns Which Can Be Controlled By A Remote Joystick And Monitored On A Video Screen Including Pattern Duplication Through A Reprogrammable Computer".
3. Patent application Ser. No. 07/336,007 filed 04/10/89 for "Automatic Quilting Machine For Specialized Quilting Of Patterns Which Can Be Created By A Scanner Or On A Video Screen Utilizing Computer Graphics In Conjunction With A Reprogrammable Computer Which Includes Computer Aided Design".
The prior art known to the inventors is discussed in the above three referenced patent applications. None of this prior art discloses the concept of separate computers or process controllers to control the sewing machine functions and the frame table movements so that each can be independently programmed or reprogrammed to make adjustments or changes in either the stitch or accessory functions such as trim, etc. or in the table movement in the X and/or Y direction.
Therefore, there is a significant need for a system which selectively breaks down the the three functions of sewing machine stitch pattern, X movement and Y movement into individualized computer program modes so that reprogramming of one element does not require reprogramming the entire system.
SUMMARY OF THE PRESENT INVENTION
The present invention relates to an automatic quilting machine for use in stitching individual selected patterns into a large fabric such as a bedspread or quilt. The bedspread or quilt is stretched on a large metal frame which is mounted on a table which can be moved in the X-direction, the Y-direction, or any X-Y combination direction, either through a manually operated automatic joystick or mouse or through an automatic remote control directed by a computer. The sewing machine head is mounted on a cross beam which is aligned at the approximate center point of the metal frame on which the fabric is stretched. The needle of the sewing machine head can stitch a pattern into any location in the fabric and the metal frame is moved in any direction relative to the fixed sewing machine head in order to bring the desired stitch location on the fabric into alignment with the sewing machine head.
In addition, the present invention also relates to a reprogrammable function integrated into the system wherein the operator first manually draws the desired pattern on a monitor using conventional graphic systems apparatus such as a mouse. The tracing function is facilitated through a computer aided design program which automatically converts the drawn pattern into computer language which then can cause the stitch to be reprogrammed at any desired location on the fabric. An example of such a computer aided design program is AutoSketch-R or AutoCad-R which are federally registered trademarks of Autodesk, Inc. At the end of this step, the traced pattern is stored into the memory of the computer as a digitalized image of the pattern embodied in the computer aided design program. The computer aided design program then permits the patterns to be duplicated as often as desired after information concerning the dimension of the fabric and the desired locations for the repeated pattern are input into the computer program. At the end of this step, the computer will have generated and stored a digitalized map of the entire area to be quilted. In the third step of the process, the operator will command the start of the automated quilting generated process and the computer will cause the machine to to the marked locations in the computer which are comparable to the marked locations on the bedspread or quilt and repeat the individualized pattern which was created by the operator. The commands are placed into the remote control operation which causes the movement of the frame quilting table.
Further, the present invention also relates to a system wherein the sewing machine function is controlled by one computer usually connected to the sewing machine head and the quilting table motion in the X-direction, Y-direction, and X-Y direction is controlled by a separate computer. When it is desired to change a sewing machine computer function such as a stitch or accessory functions such as trim, the sewing machine computer can be independently reprogrammed. When it is desired to change the pattern, the separate computer controlling the X-Y table movement direction can be independently reprogrammed. It is not necessary to reprogram both functions which is an enormous task. Instead, only one of the functions needs to be reprogrammed, thereby greatly simplifying the process.
In general, this is a frame quilting machine. A bedspread, comforter, quilt, etc. is stretched securely on a metal frame. It is placed on an X-Y positioning table for movement controlled through a sewing machine. The sewing machine has been modified and mounted on a steel frame (two cross beams top and bottom) that can accommodate twelve feet by twelve feet six inches of stitching dimensions. Of course it can be made larger or smaller. The machine has been engineered and built to satisfy increased production needs of manufacturers who supply "customer, hand-guided, or outline quilted patterns". The key elements of the present invention are: (a) sewing and auxiliary functions; (b) the electronic coordination of movement and sewing speeds relative to direction and distance of travel of the remote control apparatus; (c) a reprogrammable computer into which the individualized pattern which can be converted into machine language by the computer aided design program of the computer can be programmed into the computer and after at least one point for each subsequent pattern duplication has been marked into the computer aided design computer program, the individualized pattern can be duplicated in each desired location of the bedspread or quilt through activation of the reprogrammable computer which commands the remote control apparatus to move the quilting table relative to the sewing needle; and (d) two separate computers, one which controls the sewing machine function and one which controls the table movement in the X-direction, Y-direction and combination X-Y direction.
It has been discovered, according to the present invention, that if a frame quilting machine can be moved relative to a fixed sewing machine head in the X-direction, the Y-direction or any X-Y combination direction by a remote operating means such as a computer, and the frame quilting machine comprises a metal table or frame on which a bedspread or quilt is stretched such that the surface area of the bedspread or quilt is open and unobstructed, and the metal frame can move relative to and between a pair of cross beams which hold a sewing machine head and plate, then an operator can cause a precise pattern to be programmed into the computer through the use of a computer aided design feature which converts the graphic picture pattern into machine readable language and is stored in the memory of the computer, which in turn through a remote control apparatus can cause the programmed pattern to be precisely stitched into the bedspread or quilt by moving the metal frame or quilting table relative to the fixed cross beams housing the sewing machine components in any desired direction to arrive at any desired location on the bedspread or frame where a stitch or pattern is to be sewn, and further the sewing function or the pattern through the table movement can be separately changed by reprogramming the sewing machine computer or the table movement computer separately.
It has further been discovered, according to the present invention, that if one computer controls the sewing function of the sewing machine and a second computer controls the movement of the quilting table, then reprogramming either computer is greatly simplified.
It is therefore an object of the present invention to provide an apparatus by which an operator can remain at a remote location from a large frame quilting machine and cause a precise pattern to be sewn into the large bedspread, comforter, quilt, or other fabric which is held on the metal frame or table of the frame quilting machine, through the use of a computer aided design feature in which the pattern can be drawn on a monitor by movement of a cursor which is guided by a remote movement apparatus such as a joystick or mouse and the drawn pattern can thereafter be automatically converted into machine readable language through use of a computer aided design program such as AutoSketch-R or AutoCad-R, which can automatically duplicate a graphic pattern into machine readable form. Thereafter, the pattern is stored in the memory of the reprogrammable computer and the pattern can be duplicated into the fabric through commands from the computer which guides a remote control apparatus which causes the frame quilting table to be moved relative to the sewing needle. If it is desired to change the pattern, the reprogrammable computer need only be reprogrammed to change the movement pattern of the table in the X-direction, Y-direction, and combination X-Y direction without having to also reprogram the sewing machine commands. If it is desired to change the sewing machine function, only the sewing machine function needs to be reprogrammed without having to also reprogram the frame table movement.
It is a further object of the present invention to provide an apparatus which can accommodate computerized pattern quilting of a predetermined computer generated pattern and also accommodate specialized hand selected patterns, or any combination thereof, in the same unit.
It is an additional object of the present invention to increase the rate of production of hand guided patterns sewn into large fabrics such as bedspread or quilts.
It is also an object of the present invention to provide a system for automatically duplicating the individualized patterns through a specialized computer aided design program or scanner, to thereby eliminate the necessity of using a digitizer/cursor board to individually record numerous plotted points of the pattern drawing and thereafter burn them into a E-Prom.
It is a further object of the present invention to provide a system wherein the computers which control the sewing machine function and the quilting table movement are segregated to thereby reduce the effort involved in reprogramming the computers.
Defined very broadly, the present invention is a method of repetitively sewing a pattern into a fabric having a large surface comprising: (a) positioning a sewing machine head having a source of thread and a sewing needle relative to said fabric; (b) retaining said fabric on a movable structure which can be made to move in a horizontal direction relative to the sewing needle and which can cause a portion of the surface of the fabric to be reached by the sewing needle so that thread can be sewn into the fabric; (c) causing said movable structure to move relative to the sewing machine through commands from a first process controller; and (d) causing said sewing machine head to perform stitching or alternative sewing machine functions from commands through a second process controller.
The present invention can also be defined as an apparatus for sewing thread into fabric, comprising: (a) a first structure supporting a sewing machine head having a sewing needle and a source of thread; (b) a second structure supporting the fabric in a position relative to said sewing needle so that thread may be sewn into the fabric; (c) said second structure capable of horizontal movement in the X-direction, the Y-direction, or any combination X-Y direction relative to said sewing needle; (d) means for generating the horizontal movement of said second structure in the X-direction, the Y-direction, or any combination X-Y direction; (e) a first process controller having an Input/Output board which is connected to said means for generating horizontal movement of said second structure and which processes commands for controlling movement of said second structure in the horizontal direction; (f) a second process controller connected to said sewing machine and which processes commands for controlling the sewing function of the sewing machine head, the second process controller also connected to said Input/Output board of said first process controller; and (g) said first process controller and said second process controller capable of being independently programmed so that programs and modifications to programs in one of the process controllers can be made independently of the other process controller.
Further novel features and other objects of the present invention will become apparent from the following detailed description, discussion and the appended claims, taken in conjunction with the drawings.
DRAWING SUMMARY
Referring particularly to the drawings for the purpose of illustration only and not limitation, there is illustrated:
FIG. 1 is a perspective view a frame quilting machine, including a process controller with computer aided design program and a sewing machine with a separate computer.
FIG. 2 is a block diagram of the components of the electronic control components of the present invention automatic quilting machine including pattern duplication through a reprogrammable computer or process controller which comprises a computer aided design computer program for controlling frame table movement and a sewing machine with a separate computer or process controller.
FIG. 3 is a top plan view of the main body of a frame quilting machine which includes the present invention of a separate process controller to control the table movement and a separate process controller to control sewing machine operation.
FIG. 4 is a front elevational view of a frame quilting machine which includes the present invention of a separate process controller to control the table movement and a separate process controller to control sewing machine operation.
FIG. 5 is an enlarged perspective view of the front portion of the main support bean of the frame quilting machine.
FIG. 6 is an enlarged perspective view of the rear portion of the main support beam of the frame quilting machine and attachments thereto.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Although specific embodiments of the invention will now be described with reference to the drawings, it should be understood that such embodiments are by way of example only and merely illustrative of but a small number of the many possible specific embodiments which can represent application of the principles of the invention. Various changes and modifications obvious to one skilled in the art to which the invention pertains are deemed to be within the spirit, scope and contemplation of the invention as further defined in the appended claims.
Referring to FIG. 1, the main structural elements of the automatic frame quilting machine for specialized quilting of patterns including pattern duplication through a reprogrammable computer which may comprise a computer aided design computer program (hereinafter referred to as "automatic quilting machine") will be discussed first. The entire automatic quilting machine is designated as 10. The main structural member of the automatic quilting machine 10 is a pair of posts or box members, comprising a left box member 12 and a right box member 14. By way of example, the left box member 12 which serves only as a support member can be made of quarter inch plate steel and can have a base which is twenty inches wide by twenty-four inches deep and fifty-two inches tall. The right box member 14 which includes the electronics and motors, as will be described later, in addition to acting as a support member, can also be made of quarter inch plate steel and can have a base which is forty-four inches wide by twenty-four inches deep and fifty-two inches tall. The two support boxes 12 and 14 support a pair of cross beams; an upper cross beam 16 and a lower cross beam 18. Upper cross beam 16 can be made of quarter inch plate steel and can be twenty-four feet long, four inches wide and eight inches tall. Lower cross beam 18 can be made of quarter inch plate steel and can be twenty-four feet long, eight inches wide and eight inches tall. As illustrated in FIG. 1, the two beams 16 and 18 run parallel to each other between support box members 12 and 14, and are separated by a gap "H" which by way of example may be nine and a half inches. The cross beams 16 and 18 are permanently attached to the supporting box members 12 and 14 by conventional means such as welding.
Referring to FIGS. 1 and 3, on the ground between the supporting box members 12 and 14 and beneath the lowermost cross beam 18 is the base track 20. The base track 20 is comprised of track supports 22 and 24 which support thereon a gear and rack system which will be described in greater later on. Track support 22 further comprises a track 23 on which a pair of rollers may roll. Track support 24 further comprises a track 25 on which a pair of rollers may roll. The track supports 22 and 24 are aligned parallel to each other and are attached by means of transverse spacing members 26 and 28 which also run parallel to each other, thereby forming a generally square base which rests on the ground. Resting immediately above the base track 20 is a first movable support member track 30. The first movable support member track 30 is comprised of a pair of parallel X-direction beams 32 and 34 and a pair of Y-direction beams 36 and 38 which are connected together to form a generally rectangular frame. The frame comprised of members 32, 34, 36 and 38 of first movable support members 30 supports transverse roller member 40 and 42. Transverse roller member 40 is supported between Y direction beams 36 and 38 and is generally parallel to X-direction beams 32 and 34 and is aligned directly over track support 22. Transverse roller member 40 further comprises a pair of rollers 39 and 41. Transverse roller member 42 is supported between Y-direction beams 36 and 38 and is generally parallel to X-direction beams 32 and 34 and is aligned directly over track support 24. Transverse roller member 42 further comprises a pair of rollers (not shown). First movable support track 30 can move in the X direction as the rollers on transverse roller members 40 and 42 can roll on the track 23 contained on track support 22 and on track 25 contained on track support 24 respectively. Y-direction beam 36 further comprises a track 35 and Y-direction beam 38 further comprises a track 37. Y-direction beams 36 and 38 further comprise gear and rack assemblies, as will be described later.
Resting immediately above the first movable support member track 30 is a second movable support member track 50. The second movable support member track 50 is comprised of a pair of parallel X-direction beams, one of which is shown at 52 and a pair of Y direction beams, one of which is shown at 58, which are connected together to form a generally rectangular frame. The Y-direction beams on the second movable support member track 50 each further comprise a pair of rollers which enable the second movable support track 50 to move in the Y-direction. Y-direction beam 58 comprises a pair of rollers 59 and 61 which move on track 37 and Y-direction beam 56 comprises a pair of rollers (not shown) which move on track 35.
Second movable track member 50 further comprises four posts at its corners, two of which, 60 and 62 are shown in FIG. 1. The four posts support quilt table 70 which is comprised of X-direction table beams 72 and 74 and Y-direction table beams 76 and 78, connected together by means such as welding. X-direction table beam 72 is supported on posts 60 and 62 and X direction table beam 74 is supported on the two opposite posts (not shown). Y-direction table beams 76 and 78 are supported on the two X-direction table beams 72 and 74 adjacent their respective ends, as shown in FIGS. 1 and 3. The two X-direction table beams 72 and 74 are parallel to each other and the two Y-direction table beams 76 and 78 are parallel to each other.
As illustrated in FIGS. 1 and 3, the posts on second movable track member 50 support the table beams such that the table beams 76 and 78 pass through gap H between cross beams 16 and 18 and table beams 72 and 74 can pass through the gap H if the Y direction movement is of sufficient length. In operation, a bedspread or quilt 100 is stretched across the table beams 72, 74, 76, and 78, which by way of example can form a table surface of approximately twelve feet in the X-direction by twelve and a half feet in the Y-direction, such that the quilt 100 is supported at its edges by the four table beams 72, 74, 76 and 78 which result in a fully accessible quilt over its entire interior upper and lower surface. The table beams are caused to move in the X-direction by first movable support track 30 as the rollers on transverse roller members 40 and 42 move along tracks 23 and 25 respectively. The length "L" of gap "H" is preferably at least twice the length of the two X-direction table beams 72 and 74. In this way, the entire X-direction area of the quilt table 70 can be reached by the centermost position along the cross beams 16 and 18. The table beams are caused to move in the Y direction by second movable support member track 50 when the rollers on its Y-direction beams move along tracks 35 and 37. The length of tracks 35 and 37 is at least twice the length of the two Y-direction table beams 76 and 78. In this way, the entire Y-direction area of the quilt table 70 can be reached by the centermost position along the cross beams 16 and 18. Through this combination of X and Y movements, the entire area of the quilt table 70 and the quilt 100 spread thereon can be reached by the centermost position of cross beams 16 and 18. In the preferred starting position, the quilt table 70 is centered relative to the cross beams 16 and 18 and can move in any X-Y direction relative the the centermost position of the cross beams.
The quilt table 70 can be caused to move in the X and Y directions as previously described by numerous conventional types of means, such as a gear and rack assembly. One such gear and rack assembly is illustrated in FIG. 4. Track support 22 supports track 23 on which rollers 39 and 41 can roll in the X-direction. Track support 22 further contains on its interior surface a rack assembly 80 having a conventional multiplicity of teeth which can accommodate a gear. Transverse roller member 40 further supports a rotatable gear 82 which is caused to rotate by a conventional gear drive mechanism 84 having smaller gears driven by a belt to drive the rotatable gear 82. The gear drive mechanism is driven by a conventional linkage hookup to a drive motor which causes a motor shaft to rotate and thereby drive the gear drive mechanism 84 which in turn causes the rotatable gear 82 to rotate. When the rotatable gear rotates in the clockwise direction, the rotatable gear moves along the rack assembly 80 and causes the transverse roller member 40 (and opposite transverse roller member 42) to move to the right in the X-direction. When the rotatable gear rotates in the counterclockwise direction, the rotatable gear moves along the rack assembly 80 and causes the transverse roller member 40 (and opposite transverse roller member 42) to move to the left in the X-direction. It will be appreciated that a comparable rack and gear assembly is supported on Y-direction beam 38 and Y-direction beam 58, thereby enabling Y-direction beams 58 (and the opposite Y-direction beam on second movable support member track 50) to move back and forth in the Y-direction.
It will be appreciated that conventional adjustment modifications can be incorporated into this system. For example the overall height of the quilt table 70 can be adjusted up and down by creating slidable adjustments in the the posts (60, 62 and to two opposite posts) in order to adjust the height of quilting table 70 relative to the cross beams 16 and 18.
Referring to FIGS. 4, 5, and 6, a sewing machine head 110 is bolted stationary to upper cross beam 16. To achieve the goal of the present invention in segregating the computer controlling the sewing functions from the computer controlling the quilting table movement, it is required that a sewing machine head having its own computer 120 be used. As illustrated in the block diagram of FIG. 2 and also in FIG. 6, the sewing machine 110 has attached to it a separate process controller or computer 120 which received input from the process controller of the frame quilting machine and thereafter feeds the commands to the sewing machine 110. This will be discussed in greater detail later on. By way of example, one type of sewing machine head which can be used with the present invention is the Mitsubishi Industrial Sewing Machine Model LS2-180 high speed, single needle lockstitch sewing machine. A microprocessor connected to this type of sewing machine head provides many auxiliary functions such as control of needle position, presser foot lift, undertrim, and tension release disk. The sewing machine head 110 is attached to the underside of upper cross beam 16 such that the sewing needle 112 is at the approximate center of cross-beam 16. In this manner, the sewing needle 112 can reach any portion of the quilt table 70 and quilt 100 thereon by the X-Y movement of the quilt table, as previously discussed. The sewing machine plate 114 is formed into the top of lower cross beam 18 such that the plate 114 is aligned with the needle 112, as best illustrated in FIG. 6.
A bobbin 124 is supported by a frame member 126 attached to one edge of upper cross beam 16. Thread 128 is wound on the bobbin 118 and is guided by conventional means through the sewing machine head 110 and to the needle 112.
While it would be possible to physically move the quilting table 70 as the needle is sewing the pattern, it is not practical since the table is heavy and could not be moved fast enough by hand to quickly guide the portion of quilt 100 to the area where the sewing needle 112 is sewing the next stitch. Therefore, an automatic electrical system for moving the quilting table 70 and quilt 100 thereon into position for appropriate sewing of the pattern is required. A block diagram of the electronics for performing this operation is presented in FIG. 2. A source of alternating current power 150 energizes the entire system. In one connection, the source of alternating current power 150 is connected to a monitor 140. In a second connection, the alternating current source is connected to an alternating current to direct current transformer 160. The transformer 160 is in turn connected to a process controller or computer 172 which provides control functions for movement of the quilting table beams in the X-direction, the Y-direction, and therefore the X-Y direction for subsequent duplication of the pattern as will be discussed hereafter. The AC to DC transformer 160 is also connected to a remote control apparatus such as a joystick or mouse 180 which in turn is connected to a control 170. The controller 170 has an X-axis input and a Y-axis input into the process controller or computer 172. The process controller 172 has an Input/Output (hereinafter "I/O") Board 177 which connects the process controller to an X-output and a Y-output. The X-output of the I/O Board 177 is connected to an X-axis controller 162 which in turn is connected to the X direction motor 164 which is a direct current motor. The I/O Board 177 of process controller 172 also has a Y-direction output which in turn is connected to a Y-axis controller 166 which in turn is connected to the Y direction motor 168 is which a direct current motor. In the block diagram of FIG. 2, the process controller 172 is also shown connected to an external memory 174. It is also within the spirit and scope of the present invention for the process controller to have an internal memory. Included within the process controller 172 is a graphics card 173 through which the process controller 172 is connected to the monitor 140. The process controller 172 may also be programmed through floppy disks or a hard disk with a computer aided design ("CAD") program 175.
Through use of the process controller 172, its graphics card 173 and the CRT monitor 140, a pattern may be drawn through use of the Joystick/Mouse 180 and drawn on the CRT Monitor 140. Thereafter the pattern is programmed into the process controller 172 through programming means such as a Computer Aided Design Program 175. The process controller 172 through the I/O Board 177 puts out RPM Commands through its X-output and Y-output to direct the X-axis controller 162 and Y-axis controller 166 to cause the X-axis motor 164 and Y-axis motor to run at certain RPM's and move the quilting table 70 is the desired pattern direction. The I/O Board 177 of the process controller 172 is also connected to the separate sewing machine controller 120. The process controller 172 through its I/O Board 177 sends out voltage commands to the sewing machine process controller 120. Typically, the voltage commands are from 0 to 10 volts. Upon receiving the voltage command, the sewing machine process controller converts them into RPM commands and directs the sewing machine 110 to perform either stitching functions or else to perform auxiliary functions such as trim, tension open disk, foot lift, etc. The critical element in the present invention concept is that the movement of frame quilting table 70 is controlled by one process controller 172 while the sewing machine 110 is controlled by its separate process controller 120. If it is desired to reprogram the pattern being sewn or to make a modification in the existing pattern, which therefore requires a program modification to change the commands which cause the frame quilting table 70 to move in a given set of directions relative to the sewing machine head 110, it is only necessary to reprogram the process controller 172 to change the movements of the frame quilting table 70. It is not necessary to also reprogram the stitching functions of the sewing machine process controller 120 or the sewing machine 110. Therefore, instead of having to reprogram all of the combinations of table movement and stitches to be made to correspond to the table movement which can take many hours and sometimes days to complete, it is only necessary to reprogram the table movement into the machine process controller 172 and thereafter this process controller 172 sends its voltage commands to the sewing machine process controller 120 which in turn commands the sewing machine 110 to perform either stitching functions or auxiliary functions. The CAD Program 175 is one of the types of computer programs which can be used with the present invention.
The frame quilting table 70 can be programmed to move in any desired direction and variable speeds so that high-speed and low-speed moves can be programmed from the process controller 172. By way of example, the high-speed may be set to a maximum diagonal speed of approximately twenty-five feet per minute. Limit switches may be included to prevent the table's overtravel. The DC motors 164 and 168 may be variable speed motors which are coupled to the quilt table through conventional drive belts, gears and racks, as previously described. The mechanical portion of the drive system can be suitable for adaptation to a computer controlled servo system and can therefore be controlled by the process controller 172. The electronic control components including the AC to DC transformer 160, the X-axis controller 162, the Y-axis controller 166, the X-direction motor 164, the Y-direction motor 168 and the controller 170 can all be housed in the larger supporting box member 14. In the illustration of FIG. 1, the process controller 172 is shown adjacent the monitor 140. It is also possible to house the process controller 172 and its external memory 174 within larger supporting box member 14. In the preferred embodiment, the sewing machine controller 120 is also housed within larger supporting box member 14 and connected to the sewing machine 110 through wires extending through the upper cross beam 16 and/or lower cross beam 18.
An improvement which may be used in conjunction with the present invention two computer or process controller system is a computer aided design system for creating the pattern which will be sewn by the frame quilting machine. The individual can select a pattern which is to be sewn into the machine. The pattern can be hand drawn onto the monitor 140 through use of a cursor moving apparatus such as a mouse 170. The cursor moving apparatus 180 can hand drawn the pattern onto the monitor 140 and the individual can make any number of modifications and selections so that a hand designed pattern can be completely drawn on the monitor 140. After the hand drawn pattern has been drawn onto the monitor 140, the operator feeds the drawing data into the computer aided design program 175 which automatically converts the drawn graphic image into machine readable form. In the event modifications are required, the graphic pattern can be called up on the monitor 140 and the required changes made by movement of the cursor through the mouse 170 until the modified pattern has been achieved. Then the pattern is once again fed through the computer aided design program 175 and converted into machine readable form. In addition, the operator can select a grid on the monitor 140 and program a point from the graphic pattern at each location on the grid where the pattern is to be duplicated. This information can also be fed into the computer aided design program and stored. Therefore, the process controller can automatically direct the frame quilting table to move in the desired X, Y, or X-Y direction to automatically sew the programmed pattern into the fabric 100 and to cause the pattern to be duplicated on the points as marked on the computer monitor grid. Commands are fed from the I/O Board 177 of the process controller 172 through the X-axis output to the X-axis controller 162 to the X motor 164, and from the I/O Board 177 of the process controller 172 through the Y-axis output to the Y-axis controller 166 to the Y motor 168. Therefore, the present invention of two separate computers used in frame quilting can be combined with a computer aided design program (which by way of example can be an AutoSketch-R or an AutoCad-R program) so that individualized patterns can be hand drawn on the computer monitor and automatically converted into machine readable language from which the process controller can automatically sew the pattern into the fabric (such as a quilt or bedspread) and further duplicate the pattern at any multiplicity of desired locations.
By way of example the computer aided design program 175 can be the AutoSketch-R program. The AutoSketch R program is a full-function computer-aided design package for generating line art. The drawing is created using a mouse and menus which have therein various shapes such as lines, arcs, circles, points, polygons and spline curves (spline curves are curves fitted to a frame of control points which have been specified). After the drawing has been made, the drawing can be duplicated at any desired location and in any manner. The drawings can be enlarged to add fine points or otherwise modified to suit the final desired pattern.
The key design element of the present system is that the process controller 172 which controls the X-Y movement of the quilting table and the trace pattern which is stored in the computer's memory as a computer aided design pattern is separate from the computer on the sewing head 110 which controls the sewing needle stitch and speeds. This is accomplished by using a sewing head which has its own independent computer such as a Mitsubishi Industrial Sewing Machine Model LS2-180 high speed, single needle lockstitch sewing machine. In this way, if it is necessary to add new stitch patterns into memory, it is a much simpler task to add the new stitch and program commands to the process controller 172 without also having to reprogram the stitching and other needle functions on the sewing machine head.
Because of the independent computer capability of the machine with one computer controller the X-Y movement and a second computer on the sewing machine controlling the sewing and stitching functions, the operator can trace a straight line pattern into the X-Y process controller 172 and a software program command to the X-Y process controller 172 will enable the pattern to be automatically modified into a zig-zag or any other desired pattern. This is a valuable modification which cannot be easily achieved with prior art systems where the computer for the sewing machine and X-Y movement is integrated into one large computer. The software program for such prior art systems is too complicated. In such prior art systems, each stitch and each movement for each stitch would need to be programmed. In the prior art you have for example 5 stitches per inch and 4,000 linear inches per fabric so 20,000 stitches and movements per stitch must be programmed. With the present invention, only the table movement needs to be programmed because the stitch pattern is a separate independent program controlled by a separate computer on the sewing machine.
Of course the present invention is not intended to be restricted to any particular form or arrangement, or any specific embodiment disclosed herein, or any specific use, since the same may be modified in various particulars or relations without departing from the spirit or scope of the claimed invention hereinabove shown and described of which the apparatus is intended only for illustration and for disclosure of an operative embodiment and not to show all of the various forms or modification in which the invention might be embodied or operated.
The invention has been described in considerable detail in order to comply with the patent laws by providing full public disclosure of at least one of its forms. However, such detailed description is not intended in any way to limit the broad features or principles of the invention, or the scope of patent monopoly to be granted.
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An automatic quilting machine for use in stitching individual selected patterns into a large fabric such as a bedspread or quilt. The bedspread or quilt is stretched on a large metal frame which is mounted on a table which can be moved in the X-direction, the Y-direction, or any X-Y combination direction, either through a manually operated automatic joystick or mouse or through an automatic remote control directed by a computer. The sewing machine function is controlled by one computer connected to the sewing machine head and the quilting table motion in the X-direction, Y-direction, and X-Y direction is controlled by a separate computer. When it is desired to change a sewing machine computer function such as a stitch or accessory functions such as trim, the sewing machine computer can be independently reprogrammed. When it is desired to change the pattern, the separate computer controlling the X-Y table movement direction can be independently reprogrammed. It is not necessary to reprogram both funcions which is an enormous task. Instead, only one of the functions needs to be reprogrammed, thereby greatly simplifying the process.
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FIELD OF THE INVENTION
The present invention relates to liquid crystal display (LCD) devices, and particularly to an LCD device having a temperature control system.
BACKGROUND
Because LCD devices have the advantages of portability, low power consumption, and low radiation, they have been widely used in various portable information products such as notebooks, personal digital assistants (PDAs), video cameras, and the like. Furthermore, LCD devices are considered by many to have the potential to completely replace cathode ray tube (CRT) monitors and televisions.
FIG. 3 is a schematic, exploded side view of a conventional LCD device. The LCD device 1 includes a liquid crystal (LC) panel 11 , and a backlight module 12 arranged under the LC panel 11 . The backlight module 12 provides light beams to the LC panel 11 so that the LC panel 11 is able to display images.
The LC panel 11 includes a top substrate 191 , a bottom substrate 192 parallel to the top substrate 191 , and a liquid crystal layer 190 sandwiched between the top substrate 191 and the bottom substrate 192 .
The backlight module 12 includes an optical film unit 13 , a light guide plate (LGP) 15 , a reflective plate 17 , and a light source 16 . The LGP 15 includes a light incident surface 151 , a top light emitting surface 152 adjoining the light incident surface 151 , and a bottom surface 153 adjoining the light incident surface 151 . The light source 16 is a set of light emitting diodes (LEDs), and is disposed adjacent to the light incident surface 151 of the LGP 15 . The optical film unit 13 is disposed adjacent to the light emitting surface 152 . The reflective plate 17 is disposed adjacent to the bottom surface 153 .
Light beams emitted by the light source 16 enter the LGP 15 through the light incident surface 151 . Most of the light beams are reflected by the bottom surface 153 of the LGP 16 , and then transmit through the light emitting surface 152 . Some of the light beams transmit out of the LGP 15 through the bottom surface 153 , are reflected by the reflective plate 17 back into the LGP 15 , and then transmit through the light emitting surface 152 . The light beams emitting from the light emitting surface 152 transmit through the optical film unit 13 to illuminate the LC panel 11 .
When the light beams illuminate the LC panel 11 , simultaneously, an electric field is applied between the top substrate 191 and the bottom substrate 192 . Liquid crystal molecules of the liquid crystal of the liquid crystal layer 190 are driven by the electric field to rotate from one direction to another direction. The liquid crystal molecules work as light switches, and allow certain parts of the light beams to pass through the LC panel 11 . Thereby, the LC panel 11 displays images.
The freezing point of the liquid crystal is about −40° C. When the temperature of the liquid crystal is in the range from −10° C. to −30° C., the liquid crystal layer 190 becomes stickier, and the liquid crystal molecules rotate slower than normal. This is liable to cause flicker and image delay. That is, the display quality of the LCD device 1 is impaired. Furthermore, when the temperature of the liquid crystal is below −40° C., the liquid crystal layer 190 may even freeze, whereupon the LCD device 1 stops working.
Accordingly, what is needed is an LCD device that can circumvent the above-described difficulties.
SUMMARY
An exemplary LCD device includes a liquid crystal panel and a heating system. The heating system heats the liquid crystal panel when the temperature of the liquid crystal panel is below a predetermined temperature.
Another exemplary LCD device includes a liquid crystal panel and a temperature control system. The temperature control system is used for maintaining the temperature of the liquid crystal panel in a predetermined threshold range.
Other novel features and advantages will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings. In the drawings, all the views are schematic.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded, side view of an LCD device according to a preferred embodiment of the present invention, the LCD device including a backlight module.
FIG. 2 is a top plan view of certain parts of the backlight module of FIG. 1 .
FIG. 3 is an exploded, side view of a conventional LCD device.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Referring to FIG. 1 and FIG. 2 show aspects of an LCD device according to a preferred embodiment of the present invention. The LCD device 2 includes an LC panel 21 , a backlight module 22 arranged under the LC panel 21 for providing light beams to the LC panel 21 , and a heating system (not labeled) for heating the LC panel 21 .
The LC panel 21 includes a top substrate 291 , a bottom substrate 292 parallel to the top substrate 291 , and a liquid crystal layer 290 sandwiched between the top substrate 291 and the bottom substrate 292 . A main central area of the LC panel 21 is defined as a display area (not labeled).
The backlight module 22 includes an optical film unit 23 , an LGP 25 , a reflective plate 27 , and a light source 26 . The LGP 25 includes a light incident surface 251 , a top light emitting surface 252 adjoining the light incident surface 251 , and a bottom surface 253 adjoining the light incident surface 251 . The light source 26 is preferably a set of LEDs, and is disposed adjacent to the light incident surface 251 of the LGP 25 . The optical film unit 23 is disposed adjacent to the light emitting surface 252 . The reflective plate 27 is disposed adjacent to the bottom surface 153 .
Referring also to FIG. 2 , the heating system includes a temperature sensor 280 , a set of infrared ray-emitting diodes 28 , and an infrared ray absorbing film 24 . The temperature sensor 280 is arranged on an edge portion of a bottom surface of the bottom substrate 292 . Thereby, the temperature sensor 280 indirectly senses the temperature of the liquid crystal layer 290 by detecting the temperature of the LC panel 21 . The infrared ray-emitting diodes 28 are arranged adjacent to the light incident surface 251 of the LGP 25 . In the illustrated embodiment, the infrared ray-emitting diodes 28 and the LEDs of the light source 26 are arranged alternately along a length of the light incident surface 251 . The infrared ray-emitting diodes 28 can emit infrared rays with a specific wavelength, typically over 800 nm. The LEDs of the light source 26 emit visible light with wavelengths in the range from 380 nm to 780 nm. The infrared ray absorbing film 24 is arranged between the LC panel 21 and the optical film unit 23 , and faces the display area of the LC panel 21 .
The infrared ray absorbing film 24 is a transparent film with high visible light transparence. The infrared ray absorbing film 24 can absorb infrared rays with a specific wavelength over 800 nm, and convert the energy of the infrared rays into thermal energy. In particular, the energy conversion occurs as follows. When infrared rays with specific frequencies irradiate the infrared ray absorbing film 24 , some atomic groups or molecular groups of the infrared ray absorbing film 24 that have the same oscillation frequency as the infrared rays resonate with the infrared rays and gain kinetic energy from the infrared rays. With the accumulation of the kinetic energy, the atomic groups or the molecular groups jump from a ground state with a lower energy level to an excited state with a higher energy level. Accordingly, the temperature of the infrared ray absorbing film 24 rises to a higher temperature.
In operation of the LCD device 2 , visible light beams emitted by the light source 26 enter the LGP 25 through the light incident surface 251 . Most of the light beams are reflected by the bottom surface 253 of the LGP 25 , and then transmit through the light emitting surface 252 . Some of the light beams transmit out of the LGP 25 through the bottom surface 253 , are reflected by the reflective plate 27 back into the LGP 25 , and then transmit through the light emitting surface 252 . The light beams emitting from the light emitting surface 252 transmit through the optical film unit 23 and the infrared ray absorbing film 24 to illuminate the LC panel 21 .
The temperature sensor 280 detects the temperature of the LC panel 21 . When the temperature of the LC panel 21 is below a first predetermined threshold temperature (e.g. −10° C.), the infrared ray-emitting diodes 28 are turned on and emit infrared rays. The infrared rays transmit into the LGP 25 through the light incident surface 251 and emit from the light emitting surface 252 . Then the infrared rays irradiate the infrared ray absorbing film 24 . The infrared ray absorbing film 24 gains energy from the infrared rays, so that the temperature of the infrared ray absorbing film 24 rises. Because the infrared rays absorbing film 24 abuts or is close to the LC panel 21 , the thermal energy of the infrared ray absorbing film 24 is transferred to the LC panel 21 and heats the liquid crystal layer 290 to a higher temperature.
When the temperature of the LC panel 21 is higher than a second predetermined threshold temperature, (e.g. 20° C.), the infrared ray-emitting diodes 28 are turned off and stop emitting infrared rays.
The above-described configuration provides the LCD device 2 with the heating system. The heating system detects the temperature of the LC panel 21 , and heats up the LC panel 21 when the temperature is below a predetermined threshold. This ensures that the liquid crystal layer 290 is maintained in a predetermined temperature range in which the LCD device 2 can work normally.
It is to be understood, however, that even though numerous characteristics and advantages of the present embodiments have been set out in the foregoing description, together with details of the structures and functions of the embodiments, the disclosure is illustrative only, and changes may be made in detail, especially in matters of shape, size, and arrangement of parts within the principles of the invention to the full extent indicated by the broad general meaning of the terms in which the appended claims are expressed.
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An exemplary liquid crystal display device ( 2 ) includes a liquid crystal panel ( 21 ) and a heating system. The heating system heats the liquid crystal panel when the temperature of the liquid crystal panel is below a predetermined threshold temperature. The liquid crystal display device can work normally without being adversely influenced by the surrounding temperature.
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BACKGROUND
[0001] 1. Field
[0002] A load control system and method for controlling electrical loads is disclosed. In particular, a load control system and method incorporating a swimming pool filter and circulation system with an air conditioning system to provide the best utilization of energy is disclosed.
[0003] 2. General Background
[0004] Electric utilities are required to have power generating capacity to supply a peak load on a power generating system. Peak loads can vary due to timing of the day and other seasonal characteristics. Additionally, there is an ever increasing demand for electrical energy, particularly during periods of extreme heat when consumers require high amounts of energy for cooling their houses and businesses.
[0005] During periods of high energy utilization, there is a need to transfer energy use to certain times of the day to best utilize energy resources. The best utilization of energy requires the controlled use of different appliances. There are several appliances that require a high electrical load to run. However, not all of these appliances are necessary at all times of the day, and can be run during time periods when the electrical needs of a community are smaller.
[0006] For example, pool filters require a high electrical load but do not need to run at certain times of the day. However, air conditioners are utilized at times when of high heat, usually during the middle of the day.
[0007] Thus, there is a need to provide a system to monitor the load on different elements, and control the loads on different elements to provide the most efficient utilization of energy.
SUMMARY
[0008] A load control system and apparatus for controlling the electrical loads to a plurality of load bearing members is disclosed. In an exemplary embodiment, the load control system comprises a first element having a first electrical load and a second element having a second electrical load, the first element acting as a control for the utilization of the second element.
[0009] In another embodiment, the load control system includes a load sensor for sensing the first electrical load to the first element. The load sensor is attached to a load control switch. The load control switch controls the load to the second element, only allowing the second element to be actuated when the first element is not running.
[0010] In another exemplary embodiment, the second element operates at a timed cycle of a predetermined run time until the first element is operating and carrying the first electrical load, wherein the second element pauses during the timed cycle, the load control switch disconnecting the second electrical load, the load control switch reconnecting the second electrical load and the second element operating at the point in the timed cycle where the second element previously paused once the first element is no longer carrying the first electrical load.
[0011] In exemplary embodiments, the second element is a pool filter system running on a timed cycle of a predetermined run time. The pool filter system comprises a pump, a first valve, a second valve at the end of a normal line, water from the second line exiting into a pool, the second valve open during normal operation, a third valve closed during normal operation, a filter and an inline pressure sensor monitoring pressure in the pool filter system.
[0012] In another embodiment, wherein once the pressure exceeds a set limit, the first valve is cracked to relieve pressure allowing water to a return line.
[0013] In some embodiments, the second element has a predetermined run time wherein the timed cycle of the second element runs about 8 hours in a 24 hour time period.
[0014] In another embodiment, the pool filter utilizes diatomaceous earth to filter the water. In other embodiments, the pool filter may utilize sand or cartridges.
[0015] In particular embodiments, the first element is an air conditioner.
[0016] In further embodiments, the pool filter runs a backwash cycle at the end of the timed cycle if the set limit is exceeded wherein the second valve closes, the third valve opens to run the backwash cycle, the third valve opening into waste. In particular embodiments, the backwash cycle runs about 30 seconds.
[0017] In other embodiments, an indicator light is lit when the set pressure limit is exceeded, the indicator light being reset only when the pool filter is serviced. In exemplary embodiment, the set pressure limit is about 20 to 30 pounds per square inch.
[0018] In some embodiments, the sensor of the load control system is a transformer.
[0019] In further embodiments, a manual override to allow the pool filter to run a backwash cycle and perform maintenance on the pool filter.
[0020] Other objects, features, and advantages of the present disclosure will become apparent from the subsequent description and the appended claims.
DRAWINGS
[0021] The foregoing aspects and advantages of present disclosure will become more readily apparent and understood with reference to the following detailed description, when taken in conjunction with the accompanying drawings, wherein:
[0022] FIG. 1 a - 1 c illustrates an exemplary schematic of an electrical drawing of one embodiment of the disclosed control system.
[0023] FIG. 2 illustrates a exemplary embodiment of a pool filter system for use with the disclosed control system.
DETAILED DESCRIPTION
[0024] A load control system for controlling the electrical loads to a plurality of load bearing members is disclosed. The load control system has a first element having a first electrical load and a second element having a second electrical load. When the first element is on, requiring an electrical load, the second element is not allowed to operate.
[0025] In exemplary embodiments, the first element controlled by the system is the air conditioning system. Other appliances utilizing high loads during the day may also be considered to control the system. For example, other appliances that may be utilized including washers/dryers, ovens and others.
[0026] In exemplary embodiments, the second element is a pool filter system. In an exemplary embodiment, the pool filter system 140 is controlled and run only when the air conditioning system is not running.
[0027] To accomplish this, the second element is connected to a control switch, the control switch being connected to a sensor indicating whether the load to the first element is running. When the first element requires a load, a control switch disconnects the load from the second element, not allowing the second element to run. When the first element is no longer running, the control switch switches the load back to the second element.
[0028] In exemplary embodiments, the system provides a way to control the amount of electricity being utilized during various portions of the day. By turning off the second element when the first element is running, there is better energy utilization. In particular embodiments, when the first element is an air conditioner, the first element will run more during the day. Since the second element does not need to necessarily run during this time, this system will run the second element at night. Thus, less load is required for the location during the peak hours of the day.
[0029] FIGS. 1 a , 1 b and 1 c illustrate the electrical components for an exemplary embodiment of the load control system. Both of the two elements, the pool filter and the air conditioner, are attached to a transformer 150 . For example, a 120 volt (primary) transformer 150 may be connected to deliver each load. When a load is actuated to the pool filter system 140 , the secondary of the transformer may provide a low voltage, such as a 24 volt, signal to the appropriate signal circuitry. The air conditioner is run at the higher voltage.
[0030] The low voltage signal is sent to a contactor 90 to control the load to the second element, the pool filter system 140 . Once this contactor 90 is actuated, a load is sent to the pool filter system 140 to run.
[0031] The pool filter system 140 is run on a 24 hour timer 125 . The 24 hour timer 125 is connected to a load sensing timer 130 . A load sensing timer 130 monitors the time that the load is being sent to the pool filter system 140 . Once the predetermined run time for the pool filter system 140 is finished, the load to the pool filter system is
[0032] Connected to the load sensing timer 130 is a current switch 120 . The current switch 120 disconnects the load to the pool filter system 140 when the air conditioner is running.
[0033] To run the system, a series of relays 20 , 25 , 30 , 35 , 40 , 45 are connected to the components of the system. In particular embodiments, the relays 20 , 25 , 30 , 35 , 40 , 45 are both double pole, normally open, normally closed relays. Each relay has two pairs of electrical poles or contacts, one which is normally closed, the other being normally open. Upon the activation or actuation of the relays, the normally closed relay contacts open, thus opening the associated line circuits, and shedding the electrical loads (appliances or elements) connected to the circuits.
[0034] In other embodiments, the load control system may comprise a different electrical system. For example, the system may be controlled by an electrical circuit board, having the same functions as the electrical components shown in the FIG. 1 . Various other circuitry and methods may also be utilized.
[0035] The pool filter is generally has a predetermined run for a timed cycle. The filter must run for this predetermined run time every 24 hours. Thus, the system includes a 24 hour timer connected to a load sensing timer. The load sensing timer 130 indicates the amount of time that a load is running to the system.
[0036] An exemplary pool filter system 140 is illustrated in FIG. 3 . The pool filter system 140 may comprise a pump 115 , a first, second, and third valve 95 and a filter 110 . The pool filter utilizes a pump 115 to cause water to flow to a filter 110 . The filter 110 removes impurities from the pool water. After the water flows through the filter 110 , the pool water flows through the second valve 100 , the water returns back into the pool.
[0037] In exemplary embodiment, the pool filter 110 typically contains diatomaceous earth held in grids of the filter 110 . Other types of pool filters may also be used in this system. For examples, both sand and cartridge filters may also be utilized with this system.
[0038] The filter grids can be damaged if exposed to excessive pressure. Additional problems can also occur to the filter system 140 under high pressure conditions. For example, the filter housing may also be damaged. If the housing or the filter 110 is damaged, these components are expensive and difficult to replace. Additionally, high pressure causes the pool pump 115 and motor to work much harder. When the pump 115 , need to work harder, more energy is needed to run the filter system 140 . By controlling the pressure in the system, the pressure is maintained at a lower temperature, and the less energy is utilized. Thus, it is advantageous to reduce the pressure in the system.
[0039] As a result, the filter system 140 includes an inline pressure switch 80 . The inline pressure switch 80 monitors the pressure in the pool filter system 140 . As the pressure increases past a certain point, the maximum set pressure point, a first valve 105 is cracked to relieve some of the pressure in the system. A minimal amount of water is bypassed from the normal line into a return line in the system.
[0040] In exemplary embodiments, the pressure in the system should not exceed between about 20 to 30 psi. In one particular embodiment, the first valve 105 is opened once the pressure reaches the maximum set pressure of 20 psi.
[0041] By opening the first valve 105 in the system, excessive pressure between the pump 115 and the filter 110 is avoided. Since there is less pressure between the components, less energy is needed to run the system, providing a more efficient and better pool filter system 140 . In addition to providing a system that utilizes a more efficient utilization of energy with two components, the disclosed system provides a more efficient pool filter system 140 .
[0042] Once the first valve 105 is activated in response to increased pressure in the system, an indicator light 75 is activated. The indicator light 75 will remain activated until maintenance is preformed on the pool filter system 140 . The system further comprises a reset button to turn the indicator light 75 off once maintenance has been performed on the filter system 140 .
[0043] The indicator light 75 allows the person in charge of maintenance of the pool filter to know when the system has been subject to overpressure. As a result, the person in charge of maintenance will know that the system has backwashed, indicating that the filter 110 may need service. The pool filter may need some diatomaceous earth added to the system, or may need other changes to the system.
[0044] To achieve the desired actions once the pressure exceeds a set point, the pressure sensor 80 activates several relays 50 , 55 60 , 65 . The relays 50 , 55 , and 65 controlling the indicator light 75 are activated, turning the light on. Additionally, another relay 60 activates the first valve 105 , cracking the valve slightly to release the pressure. The pressure sensor 80 also activates a relay on the backwash cycle to indicate a backwash cycle should be run at the end of a timed cycle.
[0045] The filter system 140 includes a timer 130 that requires the filter to run at a set time cycle daily for a predetermined run time. This load sensing timer 130 is connected to a 24 hour timer 125 that requires that the pool filter system 140 be run once every 24 hours. In exemplary embodiments, the filter system 140 has a run time of about 8 hours for every 24 hour time period. However, the time can be set to any amount of hours necessary to maintain proper pool filtration and health.
[0046] At the end of the predetermined run time for the filter system 140 , if the first valve 105 had been opened and the pool filter system 140 has been overpressured, a backwash of the system is initiated. To backwash the system, the first valve 105 is fully opened as the second valve 100 is closed. As the second valve 100 is closed, the third valve 95 is opened. The pump 115 is reactivated, and water is forced through the backwash line. After the backwash is performed, the valves are rotated back to the initial position, with the first valve 105 closed, the second valve 100 open, and the third valve 95 closed.
[0047] At the end of the timed cycle, the relays 20 , 25 , 30 , 35 , 40 , 45 controlling the backwash cycle become activated. These relays activate timers 10 , 15 in the electrical circuitry to activate the first valve 105 , second valve 100 , and third valve 95 and turn the valves into the proper position.
[0048] The first timer 10 energizes the relay 20 controlling the valves, switching the valves into proper open/closed position to run the backwash cycle. In exemplary embodiments, this timer 10 runs for about 20 seconds to turn the valves into the proper position. A second timer 15 is then activated. This timer 15 actuates a relay controlling the pump 115 , allowing the system to backwash.
[0049] The system is not backwashed at the time the pressure is increased, but waits until the entire timed cycle has run it course. This will keep the system running and maintain the filtration of the system, even when the system reaches too high of a pressure. This will maintain the system running in its timed cycle, and reduce the amount of maintenance that needs to be done on the system.
[0050] If the system does not reach the maximum set point pressure, there is no need for the system to perform the backwash cycle. Instead the system will continue to run, waiting for the next timed cycle to start again and perform the pool filtration.
[0051] In exemplary embodiments, the pool filter system 140 also has an override system. This will allow the user maintaining the pool filter to override the system and backwash the filter system 140 at any time. As a result, the pool filter system 140 is able to be cleaned and serviced without any overpressure occurring in the filter system 140 .
[0052] In other embodiments, the override system also allows the air conditioner and the pool filter system 140 to be run at the same time. This is also a useful component to the system. The maintenance on the pool filter may need to be run at the same time as the air conditioner.
[0053] When the pool filter is backwashed, the pool filter is cleared of dirt and debris, even in between maintenance service. As a result, the pool is much cleaner and healthier utilizing the pool filter system described herein.
[0054] While the above description contains many particulars, these should not be considered limitations on the scope of the disclosure, but rather a demonstration of embodiments thereof. The load control system and uses disclosed herein include any combination of the different species or embodiments disclosed. Accordingly, it is not intended that the scope of the disclosure in any way be limited by the above description. The various elements of the claims and claims themselves may be combined any combination, in accordance with the teachings of the present disclosure, which includes the claims.
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A load control system and apparatus to control the load to different elements is disclosed. The load control system is attached to both an air conditioner and a pool filter system. The pool filter system has a predetermined run time and is only operating when the air conditioner is not. When the air conditioner turns on, the load to the pool filter system is disconnected. When the air conditioner turns off, the load is returned to the pool filter which resumes running at the point in the run time where the pool filter had previously left off. The load control system provides a more efficient and better use of energy resources.
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BACKGROUND OF THE INVENTION
The present invention applies to engine control systems and particularly to throttle control systems for electronic fuel control systems.
Many vehicle throttle control systems now use electrical circuitry to deliver an electrical signal from the accelerator, e.g. an accelerator pedal or hand control lever, to an electronic fuel control system. For example, a voltage signal provided to the electronic fuel control system corresponds to accelerator pedal or hand control position. When an "in-range" voltage level arrives at the electronic fuel control system, the electronic fuel control system responds by injecting a corresponding volume of fuel into the engine fuel system.
In some applications, a control device failure can result in an invalid in-range throttle condition, i.e. an unintended in-range voltage level. Under such condition, even though the accelerator control device is at an idle position, the electronic fuel control system receives an erroneous throttle control signal and undesirably injects fuel into the engine fuel system. Loss of engine throttle control, and possibly unintended vehicle acceleration, can result. To avoid such error conditions, a separate idle validation switch has been added to the accelerator control device as backup protection against such a failure. Typically, this switch provides a single pole double throw function wherein one side of the switch delivers a logic signal corresponding to valid idle operation only and the other side validates throttle operation. The switch mounts to the accelerator control device in such a way that actuation of the accelerator control changes the switch position from its idle validation position to its throttle validation position. The electronic fuel control system ignores the throttle control signal until it receives a throttle validation signal by way of the switch.
Accordingly, if an erroneous in-range throttle signal arrives at the electronic fuel control system, unintended fuel delivery is avoided because the electronic fuel control system has not yet received a throttle validation signal.
The idle validation switch attaches to the accelerator pedal or hand control as a separate component. The switch mounts to the accelerator control device in such manner to provide the switching according to pedal or hand control lever position. It is necessary to adjust or calibrate the point at which the switching occurs to coincide with a specified throttle signal level, i.e. a point of transition between idle and throttle operation. This insures that the switch is in the idle valid mode when the driver releases the accelerator control device, and that the engine will have a smooth idle to power transition when the driver applies the throttle. Switch transition points are typically specified by the engine manufacturer. Installation of the switch can be difficult because of the sensitive calibration required to meet the engine manufacturer's specifications, and the complex test procedures needed to insure that proper switch functioning occurs. Additionally, the switch must meet stringent environmental quality standards to function reliably in typical operating environments.
These factors result in an expensive idle validation switch and, in some cases, marginal product reliability. The resulting product is also virtually impossible to service in the field without replacing the entire accelerator control assembly. Such difficult field service further adds to the overall cost of such idle validation systems.
SUMMARY OF THE INVENTION
In accordance with a preferred embodiment of the present invention, an accelerator position sensor is combined in an integrated sensor package with mechanical registration of the validation switch and throttle control sensor built into the sensor. The accelerator position sensor and idle validation switch are electrically separate units, but mechanically coupled for response to a common actuation mechanism. The common mechanical connection establishes and maintains constant the required mechanical registration. The resulting integrated sensor can be installed on the control device without significant adjustment, or without calibration of the switch and sensor. Also, packaging of the idle validation switch in the sensor housing protects the switch from its environment, and thereby increases its reliability. The integrated package thereby enjoys reduced number of parts, increased reliability and serviceability, and reduced overall cost.
BRIEF DESCRIPTION OF THE DRAWINGS
For a better understanding of the invention, and to show how the same may be carried into effect, reference will now be made, by way of example, to the accompanying drawings in which like reference numerals refer to like elements.
FIG. 1 is a side view of an accelerator pedal, an integrated throttle control and idle validation sensor, and an electronic fuel control system.
FIG. 2 is a sectional view of the pedal and sensor of FIG. 1 taken along lines 2--2 of FIG. 1.
FIG. 3 is a perspective view of the integrated throttle control and idle validation sensor of FIG. 1.
FIG. 4 is an exploded view of the sensor of FIG. 3.
FIG. 5 is a schematic diagram of the sensor and electronic fuel control system showing electronic coupling.
FIG. 6 illustrates the relationship between mechanical operation of the sensor and production of the throttle control signal, idle validation signal and throttle validation signal.
DETAILED DESCRIPTION
FIG. 1 shows a fuel control device, i.e., an accelerator pedal 10, pivotally coupled at pin 12 to a base plate 14. Base plate 14 attaches to the floor of a vehicle (not shown) in conventional manner. An integrated throttle control and idle validation sensor 16 mounts to the underside of pedal 10 for the combined functions of providing a throttle control signal, an idle validation signal, and a throttle validation signal. Sensor 16 couples by way of multi-conductor cable 18 to an electronic fuel control system 20. System 20 is a conventional control system, and in the illustrated embodiment corresponds to a Cummins electronic fuel control system available under the trade name CELECT. While illustrated with reference to a specific electronic fuel control system, it will be appreciated by those skilled in the art that sensor 16 may be adapted to operate with a wide variety of electronic fuel control systems and control devices.
A lever arm 22 pivotally mounts to sensor 16 and carries a roller 24 at its distal end. Base plate 14 includes an inclined surface 26 engaged by roller 24. As the operator depresses pedal 10 to accelerate the vehicle, pedal 10 rotates about pin 12 in the direction 30, clockwise in the view of FIG. 1. As roller 24 moves upward along surface 26 in response to downward actuation of pedal 10, lever arm 22 pivots in the direction 32, counter clockwise in the view of FIG. 1, about the axis 34. Sensor 16 detects such movement of lever arm 22 and delivers to system 20 by way of cable 18 suitable signals both indicating and validating the position of pedal 10.
FIG. 2 shows a sectional view of the assembly of FIG. 1 taken through the sensor 16 and arm 22. In FIG. 2, a double spring 40 encircles a shaft 42 mounted upon the body of pedal 10 for rotation about the axis 34. Spring 40 couples the underside of pedal 10 and lever arm 22 to bias lever arm 22 in the direction 33 opposite that of direction 32. Pedal 10 is thereby spring biased in the direction 31, opposite of direction 30, and toward the idle position as shown in FIG. 1. The shaft 42, pivotally mounts to the body of pedal 10, but fixedly attaches to lever arm 22 such that movement of pedal 10 results in rotation of shaft 42 relative to sensor 16 and about the axis 34. Sensor 16, being mechanically coupled to shaft 42, responds to rotation of shaft 42 by producing the desired throttle control, idle validation, and throttle validation signals according to pedal 10 position as described hereinafter.
FIG. 3 shows in perspective the throttle control and idle validation sensor 16. Sensor 16 includes a slot formation 46 for mechanical coupling to shaft 42 and an electrical connector formation 48 for electrical coupling to multi-conductor cable 18. Shaft 42 engages slot formation 46 and rotates slot formation 46 about the axis 34 as a mechanical input to sensor 16. Movement of pedal 10 about pin 12 results in mechanical input, by way of shaft 42, to sensor 16 at slot formation 46. In response, sensor 16 generates the necessary signals at the connector formation 48 for delivery by way of cable 18 to electronic fuel control system 20. It will, therefore, be appreciated by those skilled in the art that sensor 16 provides an integrated package receiving a mechanical input and developing suitable electrical outputs. Sensor 16 requires no calibration for idle validation relative to throttle control as such is built into the integrated package. Also, by enclosing the throttle control and idle validation functions in the housing of sensor 16, the risk of exposure to environmental conditions, possibly effecting operation of sensor 16, is eliminated.
FIG. 4 is a view of sensor 16 exploded along the axis 34. In FIG. 4, sensor 16 comprises an external housing 50, a seal 52, a printed circuit element 54, a termination wedge 56, a rotor 58, a spring 60, and a cover 62. Within housing 50, a terminal structure 64 carries conductive elements, corresponding to those of cable 18, from within the connector formation 48 to the interior of housing 50. As described more fully below, the printed circuit element 54 includes a resistive element 66, an idle conductive element 68, and a throttle conductive element 70 suitably etched onto the substrate of circuit element 54. The rotor 58 includes a throttle wiper 72 and an idle/throttle validation wiper 74. In assembly of sensor 16, seal 52 first inserts within housing 50, then circuit element 54 rests within housing 50 such that elements 66, 68, and 70 of circuit element 54 face inward. A flat portion 76 of printed circuit element 54 rests adjacent the terminal structure 64. Circuit element 54 includes additional conductive traces (not shown) for coupling elements 66, 68, and 70 to suitable terminal contact points (not shown) of flat portion 76. The termination wedge 56 suitably interconnects the elements 66, 68, and 70 of element 54, by way of the terminal contacts (not shown) of flat portion 76, with the conductors of terminal structure 64. Electrical coupling between individual conductors of cable 18 and portions of circuit element 54 is thereby established.
Rotor 58 inserts within housing 50 interior of circuit element 54 and the wipers 72 and 74 contact portions of circuit element 54. More particularly, the throttle wiper 72 contacts the resistive element 66 of circuit element 64 and the idle/throttle validation wiper 74 selectively contacts one of, or neither of, the idle conductive element 68 and the throttle conductive element 70. Seal 52 seal rotor 58 within housing 50 while allowing rotation about the axis 14. Spring 60 couples rotor 58 and housing 50 to suitable bias rotor 58 toward a full return position. Cover 62 attaches to housing 50 to rotatably support rotor 54 and to seal the entire assembly. Rotor 58 includes the slot formation 46 (not shown but indicated by numeral 46 in FIG. 4). Rotor 58 then rotates within housing 50 and about the axis 34 according to rotation of shaft 42, i.e. in response to actuation of pedal 10. Throttle wiper 72 thereby moves along resistive element 66 while, for given ranges of angular position for rotor 58, validation wiper 74 contacts one of the idle validation conductive element 68, a non-conductive portion 69, or idle validation conductive element 70.
FIG. 5 illustrates electrical connections between portions of the sensor 16 and the electronic fuel control system 20 as established by the conductors of cable 18. In FIG. 5, the validation wiper 74 together with conductive elements 68 and 70 and non-conductive portion 69 comprise a switch 78. The resistive element 66 and throttle wiper 72 comprise a potentiometer 80. Switch 78 and potentiometer 80 are mechanically coupled by way of rotor 58, but are electrically separate. A voltage supply conductor 82 of cable 18 connects, by way of structure 64, wedge 56, and conductive traces of circuit element 54, to wiper 74, i.e. to the common pole of switch 78. An idle active conductor 83 of cable 18 couples in similar manner to idle conductive element 68. A throttle active conductor 84 of cable 18 similarly couples to throttle conductive element 70. Switch 74 selectively routes the supply voltage present on conductor 82 to neither or one of cable conductors 83 and 84 for interpretation by electronic fuel control system 20. A supply voltage potential on idle active conductor 83 validates an idle position for pedal 10 while a supply voltage potential on throttle active conductor 84 validates an in-range throttle control signal. A supply voltage on neither of conductors 83 and 84, i.e., an open connection, indicates to system 20 a transition between an idle active and throttle active condition to pedal 10.
A second voltage supply conductor 85 of cable 18 delivers a supply voltage to end 66b of resistive element 66 while a ground conductor 87 of cable 18 connects to the opposite end 66a of resistive element 66 as a ground return to electronic fuel control system 20. A throttle position conductor 86 of cable 18 couples to wiper 72 of potentiometer 80 whereby the voltage potential on throttle position conductor 86 corresponds to the position of wiper 72, more particularly, to the position of pedal 10.
As noted above, the switch 78 and potentiometer 80 are mechanically coupled by way of rotor 58. As rotor 58 moves from its full return position through a given range of angular movement, corresponding to full actuation of pedal 10, wiper 72 moves from near end 66b toward end 66a of resistive element 66. Concurrently with such rotation of rotor 54, wiper 74 initially contacts conductive element 68, but as rotor 54 moves through a given angular transition zone range, it disengages conductive element 68 as it rests against non-conductive portion 69. At the end of this transition zone range, wiper 74 contacts conductive element 70. Thus, rotation of rotor 54 through its angular range of motion corresponds to a continuously variable voltage signal on throttle position conductor 86, and suitable presentation of discrete logic signals on idle active conductor 83 and throttle active conductor 84.
In the preferred embodiment, rotor 54 has a full range of approximately 70 degrees of rotation corresponding to movement of pedal 10 from idle to full acceleration. The transition zone range, between idle validation and throttle validation, is determined by the extent of non-conductive portion 69 of circuit element 54 separating conductive elements 68 and 70. As will be apparent to those skilled in the art, a variety of configurations for sensor 16 will yield a variety of rotor 54 movement ranges and transition zone ranges a desired.
FIG. 6 relates the wiper 72 position in terms of a rotation angle of rotor 58 on the horizontal axis to the throttle control signal voltage, on the vertical axis, delivered to electronic fuel control system 20 by way of conductor 86. As the angular position of rotor 58 moves from an idle position 100 to a full throttle position 102, the voltage at wiper 72 ramps linearly from an idle voltage 104 to a full throttle voltage 106. The wiper 74 similarly moves from contact with idle conductive element 68 through a transition zone 108 and on to contact with throttle conductive element 70. Thus, as rotor 58 moves from its idle position 100 to its full throttle position 102, the voltage on conductor 83 of cable 18, representing an idle active signal, remains at the supply voltage V s1 until wiper 74 loses contact with conductive element 68. At this time the idle active conductor 83 of cable 18 presents an open circuit to system 20. Continuing with rotation of rotor 58 toward the full throttle position 102, wiper 74 eventually contacts conductive element 70 whereat the voltage on conductor 84 of cable 18, representing a throttle active signal, moves from being open to the supply voltage potential V s2 .
Electronic fuel control system 20 monitors the throttle position conductor 86, idle active conductor 83 and throttle active conductor 84 of cable 18. A supply voltage potential on idle active conductor 83 validates the idle position for pedal 10 and system 20 ignores the signal on throttle position conductor 86. A supply voltage potential on throttle active conductor 84 validates an in-range throttle control signal on throttle position conductor 86 and an appropriate volume of fuel is delivered to the vehicle engine. An open circuit on both of conductors 83 and 84 indicates to system 20 a throttle transition between an idle condition and a throttle condition. System 20 reacts as programmed according to the necessary engine specification requirements for transition between idle and throttle.
Thus, an integrated throttle control and idle validation sensor has been shown and described. The integrated package reacts to accelerator pedal position by way of a single mechanical input and delivers suitable electrical signals by way of cable 18 to an electronic fuel control system. The sensor and validation switch enjoy protection from environmental conditions, i.e. the cab environment, by virtue of its integrated packaging. Also, installation of sensor 16 requires no calibration between the throttle control portions, i.e. wiper 72 and resistive element 66, and the idle validation portions, i.e. the wiper 74 and conductive elements 68 and 70.
It will be appreciated that the present invention is not restricted to the particular embodiment or application that has been described and illustrated and that many variations may be made therein without departing from the scope of the invention as found in the appended claims and the equivalents thereof. For example, while the invention has been shown for a foot operated accelerator pedal, it should be apparent that the invention may be applied to a variety of control devices where separate validation signals are desired.
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An integrated throttle control and idle validation sensor includes mechanically coupled but electrically independent throttle control and idle validation components. A single mechanical input to the protective sensor housing corresponds to an accelerator pedal position and causes selective coupling of a supply voltage to one of an idle validation conductor and a throttle validation conductor for interpretation by an electronic control system. The throttle control system within the sensor housing comprises a potentiometer adapted for movement corresponding to the mechanical input whereby a variable voltage throttle control signal may be delivered to the electronic fuel control system. The sensor integrates previous separate throttle control and idle validation functions into a single environmentally secure housing and requires no calibration. The disclosed throttle system is more reliable and less costly than previously available separate throttle control and idle validation functions.
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BACKGROUND OF THE INVENTION.
Specifically, though not exclusively, the invention is useful for mixing a mixture of solid loose materials, in powder or granular form, which may be mixed with a liquid.
Reference is particularly made to a mixer comprising a mixing chamber, having at least one inlet and one outlet for the material, internally of which chamber there is a rotor shaft bearing a plurality of radial blades for agitating the material.
1. Technical Field of the Invention
A mixer of this type is already known, in which the blades are normally arranged coaxially about a rotating shaft and extend radially to the shaft.
2. Prior Art
Known mixers of the above type are susceptible to improvement both in terms of homogenization of the mixture obtained and in terms of operative speed.
OBJECT OF THE INVENTION
The main aim of the present invention is to provide a mixer by means of which a much more homogeneous mixture can be obtained and faster than with known-type mixers.
An advantage of the invention is that it provides a mixer which is constructionally simple and economical.
A further advantage is that a mixer is obtained which can provide a high degree of homogenization of the various components of the mixture, with a relatively low energy consumption.
A further advantage is that the invention provides a mixer with short axial length and being therefore relatively small.
SUMMARY OF THE INVENTION
The mixer of the invention comprises a mixing chamber, having at least one inlet and one outlet for the material, internally of which chamber there is a rotor shaft bearing a plurality of radial blades for agitating the material.
BRIEF DESCRIPTION OF THE DRAWINGS
These aims and advantages and others besides are all attained by the invention as it is characterised in the claims that follow.
Further characteristics and advantages of the present invention will better emerge from the detailed description that follows of a preferred but non-exclusive embodiment of the invention, illustrated purely by way of non-limiting example in the accompanying figures of the drawings, in which:
FIG. 1 shows a schematic longitudinal section, in vertical elevation, of a mixer according to the invention;
FIG. 2 is a section made according to line II—II of FIG. 1;
FIG. 3 is an enlarged detail of FIG. 2;
FIG. 4 is a view from above of FIG. 3;
FIGS. 5 and 6 are two perspective views of the detail of FIGS. 3 and 4 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
With reference to the figures of the drawings, 1 denotes in its entirety a mixer, usable for mixing pasty material or solid loose material in powder or granular form. The mixer is especially useful for producing amalgams having a controlled viscosity, formed by one or more solid loose materials amalgamated with one or more liquids.
The mixer 1 comprises a material extraction chamber 2 , which is cylindrical and has a horizontal axis x-x, an inlet mouth 3 corrected to the lower outlet of a hopper (of known type and not illustrated) for infeeding the solid loose materials in granular and/or powder form. A rotatable shaft 4 is predisposed internally of the mixer 1 ; the shaft 4 can be commandably rotated about a horizontal axis x-x thereof. An arrow F indicates a rotation direction of the shaft 4 . The shaft 4 externally bears a coaxial spiral 5 operating internally of the extraction chamber 2 . By effect of the rotation of the shaft 4 , the spiral 5 extracts the powder or granular material from the bottom of the hopper and sends it on to a material batching chamber 6 arranged downstream of the extraction chamber 2 and being coaxial thereto. The batching chamber 6 is in fact an extension of the extraction chamber 2 . The spiral extends continuously through the batching chamber 6 , which batching chamber 6 is externally delimited by a calibrated cylindrical wall 7 having a diameter which is just greater than the external diameter of the spiral 5 , so that a seal against the loose material is created between the periphery of the spiral and the internal surface of the batching chamber 6 . By taking into account the geometrical characteristics of the shaft 4 , the spiral 5 and the batching chamber 6 , and by regulating the rotation speed of the shaft 4 , a desired delivery rate of loose material through the batching chamber 6 can be achieved. The mixer 1 comprises a mixing chamber 8 having a first inlet 9 , connected to the batching chamber 6 in order to receive the batched loose material therefrom, a second inlet 10 for supply of at least one liquid product, and an outlet 11 for the mixed material. The mixing chamber 8 is delimited by a cylindrical wall 12 which is coaxial to the shaft 4 .
The shaft 4 extends into the mixing chamber 8 , but the spiral 5 is replaced by a plurality of radial agitator blades 13 for agitating the material. The radial agitator blades 13 are arranged impeller-fashion about the shaft 4 .
Each agitator blade 13 comprises a first part 14 which is connected to the shaft 4 and extends prevalently in a radial direction (with reference to the axis of the shaft 4 ). This first part 14 has the task of penetrating the material. Each agitator blade 13 also has a second part 15 , joined to the first part 14 , which is situated at a predetermined radial distance from the shaft 4 and extends prevalently in a parallel direction to the shaft 4 . The second part 15 has the function of homogenizing the material, and extends for half its length to the right and for the other half of its length to the left of the first part 14 , with reference to the arrow F in the figures of the drawings.
The first part 14 of each blade 13 is wedge-shaped in order to penetrate well into the material being mixed. The wedge shape of the first part 14 can clearly be seen in FIG. 4 or 5 . The wedge exhibits a front end 140 which extends in length in radial direction. The transversal section of the first part 14 of the blades progressively increases from the centre towards the edge, in a radial direction with respect to the shaft 4 axis.
It has been observed that the radial part 14 of the blade being wedge-shaped, and the axial part 15 being prism-shaped, with a triangular base and a front side predisposed to impact frontally with the material to be mixed, together produce a combined effect which considerably improves the operative productivity of the mixer. Each blade 13 is symmetrical according to a plane which is perpendicular to the shaft 4 axis and which passes through the front end 140 of the wedge.
The second part 15 of each blade exhibits a frontal surface 150 (with reference to blade advancement direction F) which is destined to directly impact with the material during mixing, with a practically perpendicular direction of impact on the material. In the illustrated case, the front surface 150 is flat; it could, however, in the interests of improving the mix efficiency, be made slightly concave so as to exhibit at least a slightly recessed longitudinal central zone with respect to the two opposite longitudinal edges, external and internal respectively, further from or closer to the shaft 4 axis. The front surface 150 is located further back (again with reference to advancement direction F) with respect to the front end 140 of the wedge formed by the first part 14 . At the centre, the front surface 150 is joined to the first part 14 .
The second part 15 of each blade exhibits two surfaces, denoted by 151 and 152 , respectively external and internal with respect to the central shaft 4 , which two surfaces 151 and 152 are frontally joined respectively to the external and internal edges of the front surface 150 , and posteriorly joined one to the other.
The external surface 151 is slightly convex, while the internal surface 152 is slightly concave. The second part 15 of each blade exhibits a narrowing of section in a backwards direction with reference to advancement direction F of the blade, as can be seen in FIG. 3 .
The transversal section of the second part 15 , which is practically constant, is approximately triangular, having a shorter side arranged frontally and two longer sides extending backwards. The shorter front side, which is parallel to the front end 140 of the wedge, is arranged perpendicular to blade advancement direction F so as to have a frontal impact with the material as it is being mixed in the mixing chamber 8 .
The second part 15 of each blade is preferably located at about two-thirds along the overall length of the blade, starting from the blade connection with the shaft. This has been found to be the best position for the homogenizing action of the second part 15 of the blade.
Conformed and arranged in this way, it has been found that the blades 13 create a high degree of turbulence in the mixture of loose solid and liquid materials as they are mixing. In particular, the two parts 14 and 15 of each blade cooperate to increase considerably the effect of turbulence, with a consequently rapid and energetically efficient homogenization of the various components in the mixture.
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A mixer for mixing loose powder, granular and liquid materials includes a mixing chamber 8 having a rotatable shaft 4 therein. The shaft bears a plurality of radial blades for agitating the materials. Each of the radial blades 13 includes a wedge-shaped first part 14 and a second part 15 connected thereto. The first part includes a thin-edged front end 140 for penetrating the materials and the second part includes a frontal end 150 for impacting the materials. As a result, the mixer produces a high degree of homogenization with a relatively low degree of energy consumption.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application is based on Japanese Patent Applications No. 2004-196038 filed on Jul. 1, 2004, and No. 2004-327742 filed on Nov. 11, 2004, the disclosures of which are incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates to rotation detecting apparatus.
BACKGROUND OF THE INVENTION
A rotation detecting apparatus detects, for instance, revolutions of an engine mounted on a vehicle, and rotations of a rotator provided in a general-purpose machine. More specifically, the rotation detecting apparatus is capable of detecting rotation modes of the rotor by utilizing changes contained in resistance values of magnetic resistance elements.
Conventionally, as the above-described rotation detecting apparatus capable of detecting the rotations by utilizing the resistance value changes in the magnetic resistance elements, for example, a rotation detecting apparatus described in Japanese Laid-open Patent Application No. H07-333236 is known.
This rotation detecting apparatus includes a magnetic resistance element and a biasing magnet. The magnetic resistance element and the biasing magnet are stored into a case member. In this rotation detecting apparatus, a tip portion of the biasing magnet abuts against an inside bottom plane of the case member, and further, a tip portion of a molding member containing a magnetic sensor chip abuts against a projection portion formed on this inside bottom plane, so that such an “M-to-M distance” is determined, and this “M-to-M distance” corresponds to a distance between the magnetic resistance element and the biasing magnet. In other words, in this rotation angle detecting apparatus, deflection angles of the above-explained magnetic vectors which also contain a relationship with a rotor via a projected length of the projection portion formed on the inside bottom plane of the case member are optimized, namely, a sensing sensitivity as to the rotation angle detecting apparatus is optimized.
On the other hand, although the deflection angles of the magnetic vectors corresponding to the sensing sensitivity for the rotation detecting apparatus can be adjusted based upon the above-described M-to-M distance, the projected length of the projection portion formed on the case member must be changed in order to adjust this sensing sensitivity of the rotation detecting apparatus. As a result, in such a case that the above-explained M-to-M distance must be changed in view of unavoidable reasons and this distance change is caused by, for example, the shape of the rotor for the rotation detection mode, the case member itself must also be changed in view of the unavoidable reason. That is, for instance, parts numbers as to these changed case members must be increased, and also, a total number of metal molds must be unavoidably increased which are required to mold these changed case members. In an actual case, such an adjustment itself that the deflection angles of the magnetic vectors are adjusted only by changing the above-described M-to-M distance may cause some limitations. That is, a freedom of designing as to the rotation detecting apparatus is low, and the range for adjusting the deflection angles of the magnetic vectors is restricted in the practical field.
SUMMARY OF THE INVENTION
In view of the above-described problem, it is an object of the present invention to provide a rotation sensor having high sensing sensitivity and high degree of design freedom.
Rotation detecting apparatus for detecting rotation of a magnetic rotor includes: a sensor chip having a magnetoresistive device; and a bias magnet for applying bias magnetic field to the magnetoresistive device. The bias magnet and the sensor chip are integrated. The magnetoresistive device is capable of detecting change of a magnetic vector near the sensor chip on the basis of resistance change of the magnetoresistive device so that the rotation detecting apparatus detects the rotation of the magnetic rotor. The change of the magnetic vector is generated by the bias magnetic field and the rotation of the magnetic rotor. The bias magnet is disposed around the sensor chip so that a deflection angle of the magnetic vector is controllable.
The above apparatus can control the deflection angle of the magnetic vector so that the detection sensitivity of the rotation is improved. Further, the deflection angle of the magnetic vector can be controlled by the shape of the bias magnet so that the degree of design freedom becomes larger.
Preferably, the bias magnet includes a hollow portion having a groove, and the groove has a predetermined shape for providing control of the deflection angle of the magnetic vector. More preferably, the hollow portion of the bias magnet accommodates the sensor chip, and has a rectangular shape with a pair of wide sides. The wide sides of the hollow portion face the sensor chip, and are parallel to a surface of the sensor chip, the surface on which the magnetoresistive device is disposed, and the groove of the hollow portion extends in a longitudinal direction of the bias magnet.
Further, rotation detecting apparatus for detecting rotation of a magnetic rotor includes: a sensor chip having a magnetoresistive device; and a bias magnet for applying bias magnetic field to the magnetoresistive device. The bias magnet and the sensor chip are integrated in such a manner that the bias magnet is disposed around the sensor chip. The magnetoresistive device is capable of detecting change of a magnetic vector near the sensor chip on the basis of resistance change of the magnetoresistive device so that the rotation detecting apparatus detects the rotation of the magnetic rotor. The change of the magnetic vector is generated by the bias magnetic field and the rotation of the magnetic rotor. The bias magnet includes a hollow portion having a groove. The sensor chip is accommodated in the hollow portion of the bias magnet. The groove is disposed on an inner wall of the hollow portion.
The above apparatus can control the deflection angle of the magnetic vector so that the detection sensitivity of the rotation is improved. Further, the deflection angle of the magnetic vector can be controlled by the shape of the bias magnet so that the degree of design freedom becomes larger.
Further, rotation detecting apparatus for detecting rotation of a magnetic rotor includes: a sensor chip having a magnetoresistive device; and a bias magnet for applying bias magnetic field to the magnetoresistive device. The bias magnet and the sensor chip are integrated in such a manner that the bias magnet is disposed around the sensor chip. The magnetoresistive device is capable of detecting change of a magnetic vector near the sensor chip on the basis of resistance change of the magnetoresistive device so that the rotation detecting apparatus detects the rotation of the magnetic rotor. The change of the magnetic vector is generated by the bias magnetic field and the rotation of the magnetic rotor. The bias magnet includes a hollow portion. The sensor chip is accommodated in the hollow portion of the bias magnet. The hollow portion includes an inner wall, which faces the magnetoresistive device. The bias magnet has a low magnetic strength near the inner wall facing the magnetoresistive device, the low magnetic strength being lower than those of other positions of the bias magnet.
The above apparatus can control the deflection angle of the magnetic vector so that the detection sensitivity of the rotation is improved. Further, the deflection angle of the magnetic vector can be controlled by the shape of the bias magnet so that the degree of design freedom becomes larger.
Further, rotation detecting apparatus for detecting rotation of a magnetic rotor includes: a sensor chip having a magnetoresistive device; and a bias magnet for applying bias magnetic field to the magnetoresistive device. The bias magnet and the sensor chip are integrated in such a manner that the bias magnet is disposed around the sensor chip. The magnetoresistive device is capable of detecting change of a magnetic vector near the sensor chip on the basis of resistance change of the magnetoresistive device so that the rotation detecting apparatus detects the rotation of the magnetic rotor. The change of the magnetic vector is generated by the bias magnetic field and the rotation of the magnetic rotor. The bias magnet includes a hollow portion. The sensor chip is accommodated in the hollow portion of the bias magnet. The hollow portion includes an inner wall, which faces the magnetoresistive device. The bias magnet has a high magnetic strength portion near the inner wall not facing the magnetoresistive device, the high magnetic strength portion having high magnetic strength higher than those of other positions of the bias magnet.
The above apparatus can control the deflection angle of the magnetic vector so that the detection sensitivity of the rotation is improved. Further, the deflection angle of the magnetic vector can be controlled by the shape of the bias magnet so that the degree of design freedom becomes larger.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects, features and advantages of the present invention will become more apparent from the following detailed description made with reference to the accompanying drawings. In the drawings:
FIG. 1 is a cross sectional view showing rotation detecting apparatus according to a first embodiment of the present invention;
FIG. 2 is a plan view showing a biasing magnet of the apparatus according to the first embodiment;
FIG. 3 is a schematic cross sectional view showing the biasing magnet taken along line III—III in FIG. 2 ;
FIGS. 4A and 4C are plan view and side view showing a biasing magnet of the first simulation, and FIG. 4B is a schematic view showing a triangle groove of the biasing magnet of the first simulation, according to the first embodiment;
FIG. 5 is a schematic view explaining the first simulation, according to the first embodiment;
FIG. 6A is a perspective view showing magnetic flux of the biasing magnet with no groove, and FIG. 6B is a perspective view showing magnetic flux of the biasing magnet with a groove, according to the first embodiment;
FIGS. 7A to 7C are tables explaining results of the first simulation, according to the first embodiment;
FIG. 8 is a graph showing a relationship between a M-M distance and a deflection angle of a magnetic vector obtained by the first simulation, according to the first embodiment;
FIGS. 9A to 9E are plan views showing a triangle groove of the biasing magnet of the second simulation, according to the first embodiment;
FIG. 10 is a graph explaining results of the second simulation, according to the first embodiment;
FIG. 11 is a perspective view showing a biasing magnet of the third simulation, according to the first embodiment;
FIG. 12 is a table explaining results of the third simulation, according to the first embodiment;
FIG. 13 is a perspective view showing a biasing magnet according to a first modification of the first embodiment;
FIG. 14 is a perspective view showing a biasing magnet according to a second modification of the first embodiment;
FIG. 15 is a table explaining results of a simulation of the biasing magnet shown in FIGS. 13 and 14 , according to the first embodiment;
FIG. 16 is a plan view showing a biasing magnet according to a third modification of the first embodiment;
FIG. 17 is a schematic view explaining rotation detection by using rotation detecting apparatus according to a comparison of the first embodiment;
FIG. 18 is a cross sectional view showing the rotation detecting apparatus according to the comparison of the first embodiment;
FIG. 19 is a perspective view showing a bias magnet and a sensor chip in rotation detecting apparatus according to the second embodiment of the present invention;
FIG. 20 is a perspective view showing magnetic flux of a bias magnet, according to a comparison of the second embodiment;
FIG. 21 is a plan view showing the magnetic flux of the biasing magnet, according to the comparison of the second embodiment;
FIG. 22 is a perspective view showing magnetic flux of a biasing magnet, according to the second embodiment;
FIG. 23 is a plan view showing the magnetic flux of the biasing magnet, according to the second embodiment;
FIG. 24 is a graph showing a relationship between an air gap and a deflection angle of a magnetic vector obtained by the second embodiment and the comparison of the second embodiment;
FIG. 25 is a plan view showing manufacturing equipment of the biasing magnet, according to the second embodiment;
FIG. 26 is a cross sectional view showing the equipment taken along line XXVI—XXVI in FIG. 25 ;
FIG. 27 is a cross sectional view explaining orientation of magnetic powder before the orientation is controlled, according to the second embodiment;
FIG. 28 is a cross sectional view explaining orientation of magnetic powder after the orientation is controlled, according to the second embodiment;
FIG. 29 is a perspective view showing magnetic flux of a bias magnet, according to a third embodiment of the present invention;
FIG. 30 is a plan view showing manufacturing equipment of the biasing magnet, according to the third embodiment;
FIG. 31 is a cross sectional view explaining orientation of magnetic powder after the orientation is controlled, according to the third embodiment;
FIG. 32 is a perspective view showing magnetic flux of a bias magnet, according to a modification of the third embodiment; and
FIG. 33 is a plan view showing manufacturing equipment of the biasing magnet, according to the modification of the third embodiment.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
(First Embodiment)
The inventors have preliminary studied about rotation detecting apparatus as a comparison of a first embodiment of the present invention. The apparatus is capable of detecting rotations by utilizing resistance value changes in the magnetic resistance elements. FIG. 17 indicates a flat-surface structure of a rotation detecting apparatus such as a crank angle sensor of an engine.
As shown in FIG. 17 , in this rotation detecting apparatus, a sensor chip 11 has been arranged in such a manner that this sensor chip 11 is located opposite to a rotor “RT” which corresponds to an object to be detected. The sensor chip 11 has been equipped with a magnetic resistance element pair 1 which is constituted by two pieces of magnetic resistance elements MRE 1 and MRE 2 ; and also, another magnetic resistance element pair 2 which is constituted by two pieces of magnetic resistance elements MRE 3 and MRE 4 . Then, the sensor chip 11 has been manufactured in an integrated circuit form in combination with a processing circuit for this sensor chip 11 , and the integrated sensor chip member has been molded in an integral body by using a molding member 12 . Concretely, this rotation detecting apparatus owns the following structure. That is, the sensor chip 11 has been mounted on one end of a lead frame (not shown) inside the molding member 12 , and various terminals such as a power supply terminal T 1 , an output terminal T 2 , and a GND (ground) terminal T 3 have been conducted from the other end of the lead frame. Also, a biasing magnet 13 has been arranged in the vicinity of the sensor chip 11 in such a manner that this biasing magnet 13 surrounds the molding member 12 . The biasing magnet 13 applies biasing magnetic fields to both the above-described magnetic resistance element pairs 1 and 2 . Then, this biasing magnet 13 is made of a hollow cylindrical shape provided with a hollow portion 14 along a longitudinal direction of this biasing magnet 13 . While the molding member 12 has been stored in this hollow portion 14 , the biasing magnet 13 has been fixed at a predetermined position by using an adhesive agent, or the like.
In the rotation detecting apparatus constructed of the above-explained structure, when the rotor RT is rotated, changes contained in magnetic vectors which are generated in conjunction with the above-described biasing magnetic fields may be sensed as changes contained in resistance values of the respective magnetic, resistance elements MRE 1 to MRE 4 , and then, electric signals may be outputted from the sensor chip 11 in response to the sensed resistance value changes. That is, in this rotation detecting apparatus, changes contained in potentials at a center point between the magnetic resistance elements MRE 1 and MRE 2 of the magnetic resistance element pair 1 which constitutes a half bridge circuit, and also, in potentials at a center point between the magnetic resistance elements MRE 3 and MRE 4 of the magnetic resistance element pair 2 which similarly constitutes a half bridge circuit, are applied to the above-described processing circuit. In the processing circuit, various sorts of process operations such as a differential amplifying operation and a binary processing operation are carried out with respect to the potential changes, and thereafter, the process electric signals are derived from the output terminal T 2 .
Also, in the case that such a rotation detecting apparatus for detecting the rotation modes of the rotor is used in a practical field, both the molding member 12 which has molded the sensor chip 11 and the like, and the biasing magnet 13 are stored in a proper case member. In addition, while the entire rotation detecting apparatus has been stored in a resin case which may protect the respective terminals T 1 to T 3 in combination with this case member, the resultant resin case is mounted on an engine, and the like. FIG. 18 indicates an example as to rotation detecting apparatus having the above-explained structure, which is mounted on an engine, and the like.
As indicated in FIG. 18 , in such rotation detecting apparatus, both the molding member 12 and the biasing magnet 13 are stored into a case member 30 having a bottom-having cylindrical shape, and these members 12 , 13 , 30 are molded with a resin case 40 in an integral body. The molded resin case 40 is mounted on an engine, or the like. This resin case 40 may also function as a connecting connector which connects the own resin case 40 to an electronic control apparatus, and the like by a wiring manner. Also, the above-explained respective terminals T 1 to T 3 have been electrically connected to terminal conducting members 50 a to 50 c , which also have terminals functioning as the above-described connector. These terminal conducting members 50 a to 50 c have been provided within the resin case 40 in an integral manner. Then, in this rotation detecting apparatus, a tip portion of the biasing magnet 13 abuts against an inside bottom plane of the case member 30 , and further, a tip portion of the molding member 12 containing the sensor chip 11 abuts against a projection portion 31 formed on this inside bottom plane, so that such an “M (i.e., MRE)-to-M (i.e., Magnet) distance” is determined, and this “M-to-M distance” corresponds to a distance between the magnetic resistance element pairs 1 and 2 , and the biasing magnet 13 . In other words, in this rotation angle detecting apparatus, deflection angles of the above-explained magnetic vectors which also contain a relationship with the rotor RT via a projected length of the projection portion 31 formed on the inside bottom plane of the case member 30 are optimized, namely, a sensing sensitivity as to the rotation angle detecting apparatus is optimized.
On the other hand, although the deflection angles of the magnetic vectors corresponding to the sensing sensitivity for the rotation detecting apparatus can be adjusted based upon the above-described M-to-M distance, as previously explained, the projected length of the projection portion 31 formed on the case member 30 must be changed in order to adjust this sensing sensitivity of the rotation detecting apparatus. As a result, in such a case that the above-explained M-to-M distance must be changed in view of unavoidable reasons and this distance change is caused by, for example, the shape of the rotor RT for the rotation detection mode, the case member 30 itself must also be changed in view of the unavoidable reason. That is, for instance, parts numbers as to these changed case members 30 must be increased, and also, a total number of metal molds must be unavoidably increased which are required to mold these changed case members 30 . In an actual case, such an adjustment itself that the deflection angles of the magnetic vectors are adjusted only by changing the above-described M-to-M distance may cause some limitations. That is, a freedom of designing as to the rotation detecting apparatus is low, and the range for adjusting the deflection angles of the magnetic vectors is restricted in the practical field.
As a result of experiments performed by the inventors of the present invention, the following facts could be confirmed: That is, the deflection angles of the above-described magnetic vectors are changed in conjunction with the rotations of the rotor in correspondence with the sectional shape of the hollow portion of the biasing magnet, into which the sensor chip is stored. Moreover, the deflection angles of the magnetic vectors, namely, the sensing sensitivity as this rotation detecting apparatus can be greatly improved, depending upon the sectional shape of the hollow portion. As a consequence, in accordance with the above-explained structure as the rotation detecting apparatus, while a relative positional relationship (for example, previously-explained “M-to-M” distance) among the magnetic resistance elements and the biasing magnet is not always changed, the deflection angles of the magnetic vectors which are give influences to the magnetic resistance elements can be adjusted by the sectional shape of the hollow portion. Not only the deflection angles of the magnetic vectors may be enlarged in the above-described manner, but also the improvement of the sensing sensitivity as the rotation detecting apparatus may be easily realized. Moreover, the deflection angles of the magnetic vectors may be basically adjusted by arranging the sectional shape of the hollow portion, so that the freedom degree as to designing of this rotation detecting apparatus may be largely improved.
Also, in this case, as the sectional shape of the hollow portion of the biasing magnet, for instance, in accordance with an inventive idea, such a shape may become advantageous that a groove has been formed in an inner side wall of the hollow portion of the above-described biasing magnet. This shape could also be confirmed by the experiments made by the inventors of the present invention.
Then, as this groove, for example, in accordance with an inventive idea, in such a case that the hollow portion of the biasing magnet has been formed in a substantially rectangular shape which corresponds to the sectional shape of the sensor chip, it may be effective to provide a groove in such a forming mode that this groove is elongated along a longitudinal direction of the biasing magnet with respect to an inner side wall of each of long edge sides of the hollow portion, which is located in parallel to and opposite to the arranging plane of the magnetic resistance elements in the sensor chip of the hollow portion. Moreover, in this case, in accordance with an inventive idea, since this groove is formed in the center portions of the inner side walls on the side of the respective long edges of the hollow portion, while the symmetrical characteristic as to the deflection angles of the magnetic vectors may be maintained, the deflection angles of the magnetic vectors can be easily adjusted, namely, can be readily enlarged.
It should be understood that, for example, in accordance with an inventive idea, as to a shape of the above-described groove, the below-mentioned shape can be employed:
(A) A groove is employed, the sectional shape of which is a triangular shape where a groove bottom portion constitutes a vertex.
Alternatively, in accordance with an inventive idea, as to a shape of the above-described groove, the below-mentioned shape can be employed:
(B) A groove is employed, the sectional shape of which is a semi-circular shape where a groove bottom portion constitutes an arc. Since the groove whose sectional shape is a triangular shape or semi-circular shape is employed, when the biasing magnet is molded by employing a metal mold, fluidity owned by a magnetic material within this metal mold can be hardly blocked by the groove. As a consequence, the magnetic material having better uniformity can be molded as the biasing magnet, as compared with that of such a case that a groove having another different shape is employed. Also, since these groove shapes are employed, the above-described adjusting operation as to the deflection angles of the magnetic vectors can be easily and firmly realized, which could also be confirmed by experiments made by the inventors of the present invention.
Referring now to FIG. 1 to FIG. 12 , a first embodiment mode for embodying a rotation detecting apparatus according to the present invention will be described.
FIG. 1 indicates an entire structure of the rotation detecting apparatus according to this embodiment mode. As indicated in FIG. 1 , this rotation detecting apparatus has been arranged in a similar mode as represented in, for example, FIG. 17 . That is, a molding member 12 containing a sensor chip 11 in which both the magnetic resistance element pairs 1 and 2 have been arranged in the similar mode, and a biasing magnet 13 which applies biasing magnetic fields to both the magnetic resistance element pairs 1 and 2 have been stored in a bottom-having cylindrical shaped case member 30 . This case member 30 has a projection portion 31 . Also, this case member 30 has been assembled in a resin case 40 in an integral body. The resin case 40 has been molded in such a manner that this resin case 40 may also function as a connecting connector which connects the own resin case 40 to an electronic control apparatus, and the like by a wiring manner. On the other hand, the above-explained respective terminals T 1 to T 3 have been electrically connected to terminal conducting members 50 a to 50 c which also have terminals functioning as the above-described connector. These terminal conducting members 50 a to 50 c have been provided within the resin case 40 in an integral body. However, in accordance with this embodiment mode, the above-described biasing magnet 13 has been manufactured with the following feature, as separately shown in a front view thereof of FIG. 2 . That is, in this biasing magnet 13 , a triangular groove 17 has been formed in a center portion of an inner side wall on the side of each of long edges which are located parallel to and opposite to the arranging planes of the magnetic resistance element pairs 1 and 2 in the sensor chip 11 . Each of the triangular grooves 17 has been formed in such a triangular shape as viewed in a sectional plane thereof. In this triangular shape, a groove bottom portion constitutes a vertex. As apparent from also FIG. 1 , this triangular groove 17 is elongated along the entire longitudinal direction of the above-explained biasing magnet 13 .
FIG. 3 is a perspective view for showing a sectional structure of the biasing magnet 13 in the case that such a biasing magnet. 13 is cut along a line III—III represented in FIG. 2 . An internal shape of the above-described triangular groove 17 formed in this biasing magnet 13 , and an internal shape of a hollow portion 14 are illustratively shown in this drawing.
Next, a description is made of results of simulations which were performed by the inventors of the present invention as to the deflection angles of the above-described magnetic vectors which were changed, since the triangular grooves 17 were formed in the hollow portion 14 of the biasing magnet 13 .
The contents of the respective simulations are given as follows: That is, as a first simulation, in the biasing magnet 13 where the above-described triangular grooves 17 had been formed, an analyzing operation was carried out with respect to the deflection angles of the magnetic vectors in such a case that the previously explained “M-to-M distance” was changed. Also, as a second simulation, an analyzing operation was carried out with respect to the deflection angles of the magnetic vectors in the case that the shapes of the triangular grooves 17 were changed. Furthermore, as a third simulation, an analyzing operation was carried out with respect to the deflection angles of the magnetic vectors in the case that the lengths of the triangular grooves 17 were changed. Simulation conditions, simulated results, and the like will be subsequently described in detail according to the first to third simulations.
[First Simulation]
First, a description is made of an analyzing condition with respect to the above-explained first simulation. As shown in FIGS. 4A to 4C , as the biasing magnet 13 which is employed in this analyzing operation, the below-mentioned biasing magnet was used. That is, dimensions of this biasing magnet 13 were given: a length of this biasing magnet 13 was “13.5 mm”; a lateral width thereof was “10.0 mm”; and a longitudinal width thereof was “9.0 mm.” In this biasing magnet 13 , such a hollow portion 14 was formed, the dimensions of which were given: a lateral width of the hollow portion 14 was “6.5 mm”; and a longitudinal width thereof was “2.6 mm.” Also, as the triangular grooves 17 which are formed in this hollow portion 14 , such a triangular groove as shown in FIG. 4B was used. That is, dimensions of this triangular groove 17 were given: a width “X” of the triangular groove 17 (namely, width of bottom edge) was “2.0 mm”; and a depth “Z” thereof was “0.8 mm.” Then, with employment of the above-described biasing magnet 13 , the analyzing operations are carried out in accordance with the following conditions: That is, as analyzing points for analyzing open degrees of the magnetic vectors which are required so as to calculate the above-explained deflection angles of the magnetic vectors, two sets of an analyzing point “IVA” and another analyzing point “IVB” are employed which correspond to positions where the above-described magnetic resistance element pairs 1 and 2 are actually arranged. Also, while distances between these two analyzing points IVA, IVB, and a rotor opposing plane 13 a as an edge plane of the biasing magnet 13 are changed, namely M-to-M distances are changed, an analyzing operation is carried out as to how a deflection angle of a magnetic vector is represented with respect to each of the M-to-M distances.
On the other hand, as the rotor RT employed in this first analyzing operation, such a rotor “RT” having a shape indicated in FIG. 5 was used. Then, open degrees of magnetic vectors at the above-described analyzing points “IVA” and “IVB” were analyzed when a point “VM” of a hill portion and another point “VC” of a valley portion were located opposite to the above-described rotation detecting apparatus while this rotor RT of FIG. 5 was rotated. Both the point “VM” of the hill portion and the point “VC” of the valley portion have been formed on an outer peripheral portion of the rotor RT. Then, it is so assumed that deflection angles of magnetic vectors are calculated based upon such an angle difference between an open angle of the magnetic vectors at the analyzing points “IVA” and “IVB” when the rotation detecting apparatus is located opposite to the point “VC”, and another open angle of the magnetic vectors at the analyzing points “IVA” and “IVB” when the rotation detecting apparatus is located opposite to the point “VM.” It should also be understood that as indicated in this FIG. 5 , a distance between a rotor opposing plane of the rotation detecting apparatus and a hill portion of the rotor RT is defined as “0.5 mm”, namely, an air gap “AG” is set to 0.5 mm.
FIGS. 7A to 7C indicate results of this first simulation. FIG. 7A shows the simulation results obtained from such a biasing magnet 13 that the above-described triangular grooves 17 are not formed. FIG. 7B indicates the simulation results obtained from such a biasing magnet 13 that the above-explained triangular grooves 17 have been formed.
As apparent from these simulation results indicated in FIG. 7 A and FIG. 7B , as to each of the M-to-M distances, although a magnetic sensitivity of the biasing magnet 13 where the triangular grooves 17 have been formed becomes lower than a magnetic sensitivity of such a biasing magnet 13 where the triangular grooves 17 have not been formed, a deflection angle of a magnetic vector of the first-mentioned biasing magnet 13 with the groove 17 exceeds a deflection angle of a magnetic vector of the last-mentioned biasing magnet 13 with no groove. By the way, as a factor causing the magnetic strength to be lowered, the below-mentioned reason may be conceived. That is, as to the biasing magnet 13 where the triangular grooves 17 have been formed, a volume of this biasing magnet 13 as the magnet is lowered by a volume of the triangular grooves 17 , as compared with such a biasing magnet 13 where the triangular grooves 17 are not formed. On the other hand, as a factor causing the deflection angle of the magnetic vector to be enlarged, the below-mentioned reason may be conceived. That is, since the magnetic strength is lowered, the deflectability as to the magnetic vector could be improved. It should also be understood that the following fact may also be conceived as one of these factors. That is, since the triangular grooves 17 are formed in the biasing magnet 13 , a generation mode as to magnetic fluxes (magnetic fields) generated from the biasing magnet 13 itself is changed. In other words, as indicated in FIG. 6A , in the previously-explained biasing magnet 13 where no triangular grooves 17 are formed, which has been provided in the rotation detecting apparatus exemplified in FIG. 18 , magnetic flux density (arrows of solid lines indicated in FIG. 6A ) along the rotation direction of the rotor RT relatively becomes low, as compared with magnetic flux density (white-blanked arrows shown in FIG. 6A ) along a direction which is located perpendicular to this rotation direction of the rotor RT. To the contrary, in the biasing magnet 13 where the triangular grooves 17 have been formed, as shown in FIG. 6B , magnetic flux density (white-blanked arrows indicated in FIG. 6B ) along the rotation direction of the rotor RT relatively becomes high, as compared with magnetic flux density (arrows of solid lines shown in FIG. 6B ) along a direction which is located perpendicular to this rotation direction of the rotor RT. As a result of the high magnetic flux density, it can also be predicted that the deflection angles of the magnetic vectors may be enlarged.
Also, as apparent from a comparison made between values of areas which are surrounded by broken lines in FIG. 7A and FIG. 7B , as to magnetic field strengths at the above-described point “VM”, a magnetic field strength of the biasing magnet 13 having no triangular grooves 17 , the M-to-M distance of which is “1.3 mm” becomes such a value of “−14.0 mT”, whereas a magnetic field strength of the biasing magnet 13 having the triangular grooves 17 , the M-to-M distance of which is “1.4 mm” becomes such a value of “−13.9 mT”, namely these magnetic field strengths at the point VM are substantially equal to each other. However, also even in this case, the deflection angle of the magnetic vector as to the biasing magnet 13 having no triangular grooves 17 is equal to “24.3 degrees”, whereas the deflection angle of the magnetic vector as to the biasing magnet 13 having the triangular grooves 17 is equal to “28.0 degrees”, resulting in an improvement of the deflection angle of the magnetic vector, while the adverse influence caused by the “M-to-M” distance can be mitigated.
On the other hand, FIG. 7C shows such a simulation result that the sensitivities of both the magnetic resistance element pairs 1 and 2 have been considered with respect to the magnetic strengths which have been acquired in FIG. 7A and FIG. 7B . This simulation result of FIG. 7C is represented as a graph in FIG. 8 . As indicated in FIG. 8 , deflection angles of magnetic vectors as to the biasing magnet 13 where the triangular grooves 17 have been formed are enlarged over all of the M-to-M distances, as compared with deflection angles of magnetic vectors as to the biasing magnet 13 where the triangular grooves 17 have not been formed. For example, in the “M-to-M” distance of “1.3 mm” which corresponds to an area surrounded by a broken line of FIG. 7C , a deflection angle of a magnetic vector as to the biasing magnet 13 where the triangular grooves 17 have been formed is enlarged approximately “1.35” times higher than a deflection angle of a magnetic vectors as to the biasing magnet 13 where the triangular grooves 17 have not been formed.
As previously explained, such a confirmation can be made. That is, since the triangular grooves 17 are formed in the hollow portion 14 of the biasing magnet 13 , this groove formation may give an extremely large merit in order to enlarge the deflection angles of the magnetic vectors.
[Second Simulation]
Next, a second simulation is explained. In this second simulation, analyzing operations were carried out as to deflection angles of the above-described magnetic vectors in such a case that a width “X”, and a depth “Z” as to a triangular groove 17 which will be formed in the hollow portion 14 were changed respectively. It should also be understood that other shapes of this biasing magnet 13 are made equal to those of the previously explained first simulation.
FIGS. 9A to 9E shows shapes of triangular grooves 17 which constitute analysis objects in this second simulation. As represented in FIGS. 9A to 9E , in this second simulation, 5 samples “S 1 ” to “S 5 ” were analyzed respectively. That is, as the samples “S 1 ” to “S 3 ”, the below-mentioned triangular grooves 17 have been employed, the widths “X” of which were “0.5 mm”; “1.0 mm”; and “1.5 mm”, and also, the depth “Z” of which was “0.5 mm.” Furthermore, as the samples “S 4 ” to “S 5 ”, the below-mentioned triangular grooves 17 have been employed, the depths “Z” of which were “1.0 mm”; and “1.5 mm”, and also, the width “X” of which was “1.0 mm.” It should also be understood that in this second simulation, the analyzing operations are carried out in such a case that the above-explained air gaps “AG” are three sorts of air gaps, namely, “0.5 mm”; “1.0 mm”; and “1.5 mm”, respectively. It should further be noted that as a shape of a rotor “RT”, the same shape as that of the first simulation is used. Further, the analyzing operations are carried out while the above-descried M-to-M distance is fixed to “1.3 mm.”
FIG. 10 is a graph for indicating results of this second simulation. The graph of FIG. 10 clearly represents deflection angles of magnetic vectors as to the above-explained samples S 1 to S 5 , and in addition, a deflection angle of a magnetic vector as to a biasing magnet where the triangular groove 17 is not formed, for the sake of comparisons. As apparent from the simulation results with respect to the samples Si to S 3 , which are graphically indicated in FIG. 10 , the wider the width “X” of the triangular groove 17 is widened, the larger the deflection angle of the magnetic vector is increased. Also, as apparent from the simulation results with respect to the samples S 2 , S 4 , and S 5 , which are graphically indicated in FIG. 10 , the deeper the depth “Z” of the triangular groove 17 is increased, the larger the deflection angle of the magnetic vector is increased. It should also be noted that angles which are attached among the respective graphs indicative of simulation results of these samples S 1 to S 5 correspond to such values for indicating how the deflection angles of the magnetic vectors as to the respective samples S 1 to S 5 have been enlarged when the air gaps AG thereof are equal to “1.5 mm” with respect to the deflection angle of the magnetic vector of the biasing magnet where the triangular groove 17 is not formed when the air gap AG thereof is selected to be similarly “1.5 mm.” As also can be understood from these values, only as to the above-explained samples S 1 to S 5 , if the depth “Z” of the triangular groove 17 is made large (deeper), then the deflection angle of the magnetic vector may be furthermore enlarged, as compared with such a case that the width “X” of the triangular groove 17 is made larger (wider).
[Third Simulation]
Next, a third simulation is explained. In this third simulation, analyzing operations were carried out as to deflection angles of the above-described magnetic vectors in such a case that a length “L” as to a triangular groove 17 was changed as exemplified in FIG. 11 , not in the case that the triangular grooves 17 were formed in the entire portion of the biasing magnet 13 along the longitudinal direction thereof. It should be noted that while other shapes of the biasing magnet 13 are made equal to those of the previous first simulation, analyzing operations were carried out in such a case that the above-explained air gaps “AG” were three sorts of air gaps, namely, “0.5 mm”; “1.0 mm”; and “1.5 mm”, respectively. It should also be noted that as a shape of a rotor “RT”, the same shape as that of the first simulation is used, and analyzing operations were carried out while the above-described M-to-M distance is fixed to “1.3 mm.”
FIG. 12 indicates results of this third simulation. As apparent from this FIG. 12 , in any case that the air gap AG corresponds to “0.5 mm”, “1.0 mm”, and “1.5 mm”, since the triangular groove 17 having the length “L” is formed in the biasing magnet 13 , a deflection angle of a magnet vector is increased (see samples “U 2 ” to “U 5 ”), as compared with that of such a biasing magnet (namely, sample “U 1 ”) where the triangle groove 17 is not formed. However, a large change cannot be seen from deflection angles of magnetic vectors as to biasing magnets in which lengths “L” of triangle grooves 17 are longer than a certain length, concretely speaking, the lengths “L” become longer than “6.7 mm” of the sample U 3 . From the above-explained conditions, the following fact can be revealed: That is, in order that the triangular groove 17 is formed in the hollow portion 14 so as to enlarge the deflection angle of the magnetic vector, if such a triangular groove 17 having a certain length separated from the rotor opposing plane 13 a of the biasing magnet 13 is formed in this hollow portion 14 , then the sufficiently enlarged deflection angle of the magnetic vector can be obtained.
Also, in this third simulation, an analyzing operation was carried out in the case that one triangular groove 17 has been formed only in any one of inner side walls on the long edge sides of the hollow portion 14 . In other words, as indicated as a sample U 6 in FIG. 12 , in the case that one triangular groove 17 has been formed only in any one of inner side walls on the long edge sides of the follow portion 14 , a degree of enlarging a deflection angle of a magnetic vector thereof is lower than that of such a case that the triangular grooves 17 have been formed in the inner side walls on the side of the long edges of the hollow portion 14 . However, the deflection angle of the magnetic vector of the first-mentioned biasing magnet 13 is enlarged, as compared with that of the conventional biasing magnet 13 (sample U 1 ) where the triangular groove 17 is not formed. As apparent from the above-described simulation result, in order that the triangular grooves 17 are formed in the hollow portion 14 so as to enlarge the deflection angles of the magnetic vectors, there is a merit even in such a structure that one triangular groove 17 is formed only in one of these inner side walls of the hollow portion 14 .
These results obtained in the first to third simulations will now be summarized as follows:
(a) Since the triangular grooves 17 are formed in the hollow portion 14 of the biasing magnet 13 , the deflection angles of the magnetic vectors are enlarged.
(b) The wider the width “X” of the triangular groove 17 is widened, the larger the deflection angle of the magnetic vector is enlarged.
(c) The deeper the depth “Z” of the triangular groove 17 is increased, the larger the deflection angle of the magnetic vector is enlarged.
(d) As to the depth “Z” and the width “X” of the triangular groove 17 , there is an advantage that if the depth “Z” is made deeper, then the deflection angle of the magnetic vector may be further enlarged.
(e) If the triangular groove 17 owns a certain length separated from the rotor opposing plane 13 a of the biasing magnet 13 , then a sufficiently large deflection angle of a magnetic vector may be obtained. Therefore, this triangular groove 17 is not always formed over the entire length of the biasing magnet 13 .
(f) Even when the triangular groove 17 is formed only in one of the inner side walls of the hollow portion 14 , the deflection angle of the magnetic vector may be enlarged.
As a consequence, in accordance with the above-described embodiment modes in which at least the above-explained structures (a) to (d) are employed, the below-mentioned effects can be achieved:
(1) While the relative positional relationship (for example, previously-explained “M-to-M” distance) among the magnetic resistance element pair 1 , the magnetic resistance element pair 2 , and the biasing magnet 13 is not always changed, the deflection angles of the magnetic vectors which are influenced to both the magnetic resistance element pairs 1 and 2 can be adjusted by the triangular grooves 17 formed in the hollow portion 14 . Not only the deflection angles of the magnetic vectors may be enlarged in the above-described manner, but also the improvement of the sensing sensitivity as the rotation detecting apparatus may be easily realized. Moreover, the deflection angles of the magnetic vectors may be basically adjusted by arranging the triangular grooves 17 of the hollow portion 14 , so that the freedom degree as to designing of this rotation detecting apparatus may be largely improved.
(2) Since the triangular grooves 17 are formed in the center portions of the inner side walls on the side of the long edges of the hollow portion 14 , while the symmetrical characteristic as to the deflection angles of the magnetic vectors may be maintained, the deflection angles of the magnetic vectors can be easily adjusted, namely, can be readily enlarged.
(3) Since the triangular groove 17 whose sectional shape becomes the triangular shape is employed as the groove to be formed in the hollow portion 14 , when the biasing magnet 13 is molded by employing a metal mold, fluidity owned by a magnetic material within this metal mold can be hardly blocked by the triangular groove 17 . As a consequence, the magnetic material having better uniformity can be molded as the biasing magnet, as compared with that of such a case that a groove having another different shape is employed.
It should also be understood that the rotation detecting apparatus of the above-described embodiment modes may be modified as follows:
That is, in the above-explained embodiment modes, the triangular grooves 17 have been formed in the entire portion of the biasing magnet 13 along the longitudinal direction. Alternatively, when the content of the summarized item (e) as to the simulation results is considered, the triangular groove 17 may be formed in such a way that this triangular groove 17 has a certain length (“6.7 mm”, in above example) separated from the rotor opposing plane 13 a of the biasing magnet 13 .
Similarly, when the content of the summarized item (f) as to the simulation results is considered, the triangular groove 17 may be alternatively formed in such a way that this triangular groove 17 is formed only in one of the inner side walls which constitutes the hollow portion 14 of the biasing magnet 13 .
In the above-described embodiment modes, such a biasing magnet 13 that the triangular grooves 17 have been formed in the hollow portion 14 has been exemplified. Alternatively, instead of the above-described triangular grooves 17 , for instance, as shown in FIG. 13 which corresponds to the previous drawing of FIG. 3 , such a biasing magnet 13 may be alternatively employed in which a semi-circular groove 18 has been formed, and a groove bottom portion of this semi-circular groove 18 has been made in an arc shape. Also, similar to the above modification, as represented in FIG. 14 which corresponds to the previous drawing of FIG. 3 , such a biasing magnet 13 may be alternatively employed in which a rectangular groove 20 has been formed and a groove bottom portions of this rectangular groove 20 has been formed in a rectangular shape. Analyzed results of deflection angles of magnetic vectors as to either the biasing magnet 13 which has employed the semi-circular grooves 18 or the biasing magnet 13 which has employed the rectangular grooves 20 will now be explained with reference to FIG. 15 . As represented in the analyzed results of FIG. 15 , the deflection angles of the magnet vectors as to the biasing magnet 13 (sample V 1 ) where the semi-circular grooves 18 have been formed are also enlarged, as compared with the deflection angles of the magnetic vectors as to the biasing magnet (sample U 1 of FIG. 12 ) where the triangular grooves 17 have not be formed. Moreover, a degree of the enlarged deflection angles becomes larger than that of such a biasing magnet (sample V 4 ) where the triangular grooves 17 having the same widths “X”, the same depths “Z”, and the lengths “L” have been formed. As a consequence, since the semi-circular grooves 18 are formed, the deflection angles of the magnetic vectors may be enlarged at the same degree, or higher degree than that of the above-explained triangular grooves 17 . In addition, the sensing sensitivity may be further improved. Also, in the case that this semi-circular groove 18 is employed in the biasing magnet 13 , similar to such a case that the above-described triangular groove 17 is employed in the biasing magnet 13 , there is a merit that fluidity of a magnet material used when this biasing magnet 13 is molded can be hardly blocked. On the other hand, the deflection angles of the magnet vectors as to the biasing magnets (samples V 2 and V 3 ) where the rectangular grooves 20 have been formed are also enlarged, as compared with the deflection angles of the magnetic vectors as to the biasing magnet (sample U 1 of FIG. 12 ) where the triangular grooves 17 have not be formed. Then, in this case, more specifically, the depth “Z” of this rectangular groove 20 is made equal to, or deeper than the depths of other grooves, so that the following fact can be revealed from the analyzed results of FIG. 15 . That is, an enlarging degree of the deflection angles of the magnetic vectors may become larger than the enlarging degrees of the deflection angles of the magnetic vectors as to the biasing magnet in which the triangular grooves 17 , or the semi-circular grooves 18 has been formed. As a consequence, as shapes of grooves, not only the above-explained triangular grooves 17 , but also the semi-circular grooves 18 and the rectangular grooves 20 may be properly employed. The Inventors of the present invention could confirm that the contents of the above-explained summarized items (a) to (f) with respect to the first to third simulation results may be similarly applied to these semi-circular grooves 18 and the rectangular grooves 20 .
In the above-described embodiment mode, such a biasing magnet 13 has been exemplified in which one of the triangular grooves 17 has been formed in each of the inner side walls of the hollow portion 14 on the side of the long edges thereof. For example, as shown in FIG. 16 , such a biasing magnet 13 may be alternatively employed in which a plurality of triangular grooves 23 (for instance, three triangular grooves 22 ) have been formed in each of inner side walls thereof on he long edge side. Also in this alternative case the inventors of the present invention could confirm that similar operation effects to those of the above-described embodiment modes may be achieved.
Also, in the above-described embodiment mode, the triangular groove 17 has been formed in the center portion of the inner side wall of the hollow portion 14 on the long edge side. However, the position where this triangular groove 17 is formed may be alternatively selected to be any positions if these positions are located within the hollow portion 14 . In this alternative case, although the symmetrical characteristic as to the deflection angles of the magnetic vectors cannot be maintained, the deflection angles of the magnetic vectors may be easily adjusted, namely may be readily enlarged in a similar manner to that of the above-explained embodiment mode.
(Second Embodiment)
Prior to descriptions as to a second embodiment mode of a rotation detecting apparatus according to the present invention, a basic idea of the present invention will now be explained with reference to FIG. 19 to FIG. 21 . It should be understood that for the sake of easy understandings, such a conventional rotation detecting apparatus which employs a biasing magnet is employed as an example, and a portion of this biasing magnet is indicated in an enlarging manner. In this biasing magnet, magnetic field strengths have been substantially uniformly set over an entire peripheral portion of the own biasing magnet. For the sake of convenience, the same reference numerals shown in the previous drawing of FIG. 17 , or FIG. 18 will be employed as those for indicating the same, or similar structural elements indicated in FIG. 19 to FIG. 21 .
FIG. 19 shows a perspective structure of a sensor chip 11 and a biasing magnet 13 in an enlarging manner, which constitute the rotation detecting apparatus. As indicated in FIG. 19 , the biasing magnet 13 has been formed in a hollow cylindrical shape and has been equipped with a hollow portion 14 , while a sectional shape of the hollow portion 14 along a direction perpendicular to a longitudinal direction of this biasing magnet 13 is made of a rectangular shape. The sensor chip 11 having magnetic resistance elements “MRE 1 ” to “MRE 4 ” has been stored into the hollow portion 14 in combination with a molding member 12 , so that a biasing magnetic field may be applied from the biasing magnet 13 with respect to the magnetic resistance elements MRE 1 to MRE 4 of this stored sensor chip 11 . It should also be noted that in this biasing magnet 13 , an edge plane 13 a located opposite to the above-explained rotor has been magnetized as an “N pole”, whereas another edge plane located opposite to the edge plane 13 a has been magnetized as an “S pole.”
While employing the enlarged perspective view of the biasing magnet 13 , conditions of magnetic fields which are generated from the biasing magnet 13 are illustratively shown in FIG. 20 . For the sake of convenience, it should also be noted that in FIG. 20 , magnetic fields on the side of long edges of the hollow portion 14 are represented by arrows denoted by 8 solid lines, and also, magnetic fields on the side of short edges of the hollow portion 14 are represented by arrows denoted by 2 solid lines. In the below-mentioned descriptions, high/low strengths of magnetic fields will be indicated based upon widthnesses of solid lines. However, as previously explained, since the magnetic field strengths of this biasing magnet 13 shown in FIG. 20 are substantially equal to each other over the entire peripheral portion thereof, the above-explained magnetic fields may be represented by all of solid lines having the same widthness. As indicated in FIG. 20 , in a single body of this biasing magnet 13 , magnetic fields generated from this single biasing magnet 13 are converged in a ring shape in such a mode that the magnetic fields are directed from the N pole to the S pole. However, when the tooth portion of the above-described rotor passes in opposite to the edge plane 13 a of the biasing magnet 13 , magnetic vectors may be produced at this tooth portion in such a condition that the magnetic fields are drawn. Then, changes contained in angles of the produced magnetic vectors may be sensed by the magnetic resistance elements MRE 1 to MRE 4 as changes contained in resistance values.
On the other hand, in the above-described rotation detecting apparatus, the angle changes of the magnetic vectors which are produced when the above-explained rotor is rotated may be sensed as the changes contained in the resistance values of the above-described magnetic resistance elements MRE 1 to MRE 4 . In the case of the biasing magnet 13 shown in FIG. 20 , all of the magnetic fields produced from this biasing magnet 13 may contribute to the generations of the above-explained magnetic vectors. As a consequence, in particular, the deflection angles of the magnetic vectors which are generated may also be limited by the magnetic fields produced on the side of the long edges of the hollow portion 14 . Referring now to FIG. 21 , a detailed description is made of the above-described limitations as to the deflection angles of the magnetic vectors.
FIG. 21 illustratively shows conditions of magnetic fields which are produced from the biasing magnet 13 by employing a plane view of the biasing magnet 13 which is viewed from the side of the edge plane 13 a located opposite to the above-explained rotor. As represented in FIG. 21 , such magnetic fields which are produced from a portion “XXIA 1 ” and another portion “XXIA 2 ” on the side of the short edges of the hollow portion 14 are easily influenced by rotations of the rotor, if an attention is paid only to the magnetic fields which are generated from these portions XXIA 1 and XXIA 2 , then magnetic vectors may be readily deflected which are produced by these generated magnetic fields in conjunction with the rotations of the rotor. In other words, deflection angles thereof are largely maintained by the own deflection angles. To the contrary, magnetic fields which are generated from a portion XXIB 1 and another portion XXIB 2 on the side of the long edges of the hollow portion 14 are intersected perpendicular to the rotation direction of the rotor. As a result, components of such magnetic vectors which are produced by the magnetic fields generated from these portions XXIB 1 and XXIB 2 in conjunction with the rotations of the rotor may give such an effect that the easy deflections of the above-explained magnetic vectors which are produced by the magnetic fields generated from the portions XXIA 1 and XXIA 2 in conjunction with the rotation of the rotor may be blocked. In other words, if the magnetic field strengths of the magnetic fields can be lowered which are generated from the portions XXIB 1 and XXIB 2 on the side of the long edges of the hollow portion 14 , then an enlargement of the deflection angles of the above-explained magnetic vectors can be expected.
FIG. 22 to FIG. 24 show a rotation detecting apparatus according to a second embodiment mode of the present invention, while the rotation detecting apparatus has been arranged based upon the above-described basic idea. Referring now to FIG. 22 to FIG. 24 , an arrangement of the rotation detecting apparatus according to this second embodiment mode will be described in detail. It should be noted that since a structure as the rotation detecting apparatus is basically identical to the above-described structure of the conventional rotation detecting apparatus, the same reference numerals shown in this conventional rotation detecting apparatus will be employed as those for denoting structural elements having the same, or similar functions, and thus, detailed descriptions thereof are omitted.
FIG. 22 illustratively indicates conditions of magnetic fields which are generated from a biasing magnet 13 employed in the rotation detecting apparatus according to the first embodiment mode, and this drawing corresponds to FIG. 20 . As shown in FIG. 22 , the biasing magnet 13 has been formed in a hollow cylindrical shape and has been provided with a hollow portion 14 . This hollow cylindrical shape of the biasing magnet 13 is not completely different from the shape of the conventional biasing magnet. A sectional shape of the hollow portion 14 is made in a substantially rectangular shape along a direction perpendicular to a longitudinal direction of the biasing magnet 13 . Also, a material for constructing the biasing magnet 13 is the same material as the conventional biasing magnet. However, this biasing magnet 13 owns the below-mentioned different point from the conventional biasing magnet whose the magnetic strengths have been substantially uniformly set. That is, in this biasing magnet 13 , magnetic strengths of biasing magnet portions which are located opposite to front/rear arranging planes of the magnetic resistance elements MRE 1 to MRE 4 in the sensor chip 11 (see FIG. 19 ) stored in the hollow portion 14 have been selectively set to low magnetic field strengths from an edge plane 13 a of this biasing magnet 13 to an opposing plane thereof. This edge plane 13 a is located opposite to the rotor. As a consequence, among the magnetic fields generated from the biasing magnet 13 , the magnetic fields which are generated from the biasing magnet portions located opposite to the front/rear arranging planes of the magnetic resistance elements MRE 1 to MRE 4 are indicated by arrows made of narrow solid lines, as compared with magnetic fields which are generated from other portions of this biasing magnet 13 .
FIG. 23 illustratively shows conditions of magnetic fields which are produced from the biasing magnet 13 by employing a plan view of the biasing magnet 13 which is viewed from the side of the edge plane 13 a located opposite to the above-explained rotor, which corresponds to the drawing of FIG. 21 . As represented in FIG. 23 , if an attention is paid to magnetic fields which are generated from a portion “XXIA 1 ” and another portion “XXIA 2 ” on the side of short edges of the hollow portion 14 within the biasing magnet 13 , similar to the previously explained biasing magnet 13 (see FIG. 21 ), then magnetic vectors may be readily deflected which are produced by these generated magnetic fields in conjunction with the rotations of the rotor, and thus, deflection angles thereof are largely secured. To the contrary, within the biasing magnet 13 , field strengths of such magnetic fields which are generated from the biasing magnet portions located opposite to the front/rear arranging planes of the magnetic resistance elements MRE 1 to MRE 4 , namely, field strengths of magnetic fields which are generated from a portion “XXIB 1 ” and another portion “XXIB 2 ” on the side of the long edges of the hollow portion 14 have been selectively set to low field strengths, which are different from those of the previously explained biasing magnet 13 . As a result, such magnetic vectors which are produced by the magnetic fields generated from these portions XXIB 1 and XXIB 2 in conjunction with the rotations of the rotor may be easily deflected, as compared with those produced from the previously explained biasing magnet 13 . Accordingly, such magnetic vectors may be suppressed which may block easy deflections of the above-described magnetic vectors which are produced by the magnetic fields generated from the portions XXIA 1 and XXIA 2 in conjunction with the rotation of the rotor. Then, as a consequence, the components of the magnetic vectors can be relatively strengthened, which are produced by the magnetic fields generated from this biasing magnet 13 in conjunction with the rotations of the rotor.
FIG. 24 represents a simulation result as to deflection angles of magnetic vectors which are produced from the magnetic fields generated from the biasing magnet 13 in conjunction with the rotations of the rotor, while the sensitivities of the magnetic resistance elements MRE 1 to MRE 4 have been considered. It should be understood that air gaps indicated in FIG. 24 represent distances between the rotor and a rotor opposing plane of a rotation detecting apparatus in the case that this rotation detecting apparatus has been arranged as shown in FIG. 18 . As apparent from this drawing, the deflection angles of the magnetic vectors produced in the case that the biasing magnet 13 is employed may exceed the simulation results about the magnetic vector deflection angles obtained in such a case that the conventional biasing magnet 13 is employed in substantially all of the air gaps. As a consequence, since the biasing magnet 13 is employed in which the magnetic field strengths of the portions located opposite to the front/rear arranging planes of the magnetic resistance elements MRE 1 to MRE 4 have been selectively set to the low magnetic field strengths, it is extremely effective so as to enlarge the deflection angles of the magnetic vectors.
Next, a method of manufacturing the above-explained biasing magnet 13 will now be explained with reference to FIG. 25 to FIG. 28 .
Normally, when a biasing magnet is manufactured, a molded body of a resin material which contains magnetic powder is formed, and then, this molded body of the resin material is magnetized. However, the above-explained biasing magnet 13 is featured by that the magnetic field strengths of the portions located opposite to the front/rear arranging planes of the magnetic resistance elements MRE 1 to MRE 4 have been selectively set to the low magnetic field strengths. As a consequence, in the below-indicated molding apparatus, while orientation modes of the magnetic powder contained in the above-described molded body are made different from each other, the above-explained magnetic field strengths are set in accordance with such differences in the orientation modes. Subsequently, the molding apparatus capable of executing such a molding step is described in detail.
FIG. 25 is a plan view for showing a molding apparatus 70 which forms the above-described molded body. As represented in FIG. 25 , this molding apparatus 70 has been arranged by employing a molding die 72 which has a cavity 71 corresponding to the shape of the biasing magnet 13 . It should also be noted that this molding die 72 is manufactured by a non-magnetic material. Also, this molding apparatus 70 has been constituted by providing two sets of energizing coils 73 at upper and lower portions of the cavity 71 . These two energizing coils 73 may cover the cavity 71 except for such cavity portions corresponding to the above-described magnet portions XXIB 1 and XXIB 2 .
FIG. 26 is a sectional view for representing the molding apparatus 70 which is cut along a line XXVI—XXVI shown in FIG. 25 . As indicated in FIG. 26 , the molding die 72 is constituted by an upper die 72 a and a lower die 72 b , and a molded body 74 is formed within the cavity 71 between the upper die 72 a and the lower die 72 b . Two sets of the energizing coils 73 having the above-described modes have been arranged in each of the upper die 72 a and the lower die 72 b.
Next, a description is made of the method for manufacturing the above-described biasing magnet 13 with employment of the molding apparatus 70 arranged in the above-described manner.
In other words, in the case that the biasing magnet 13 is manufactured by employing the above-described molding apparatus 70 , the below-mentioned manufacturing steps are executed:
(a) A resin material containing magnetic powder is injected into the cavity 71 of the molding die 72 . It should be understood that this injection of the resin material is carried out via a spool (not shown).
(b) While the respective energizing coils 73 are energized so as to apply proper magnetic fields with respect to the magnetic powder of the resin material filled in the cavity 71 , the orientation of the magnetic powder is controlled before the resin material is solidified.
(c) After the above-described resin material has been solidified as a molded body, the entire portion of this molded body is once demagnetized.
(d) Thereafter, a portion of the molded body, which is located opposite to the rotor, is magnetized as an “N pole”, whereas another portion of the molded body, which is located opposite to the first-mentioned portion, is magnetized as an “S pole” by using a magnetizing apparatus (not shown).
Now, a further detailed explanation is made of the above-explained manufacturing step (b). FIG. 27 shows an orientation mode of the magnetic powder before the orientation of this magnetic powder is controlled with employment of a sectional diagram of the above-described forming apparatus 70 which is cut along a line XXVII—XXVII shown in FIG. 25 . Also, FIG. 28 indicates an orientation mode of the magnetic powder after the orientation of the magnetic powder has been controlled, and corresponds to the drawing of FIG. 27 . It should also be noted that in FIG. 27 and FIG. 28 , in order to easily understand the orientation modes of the magnetic powder, the magnetic powder is displayed in an enlarging manner. As indicated in FIG. 27 , under such a condition obtained before the energizing coils 73 are energized, orientation of magnetic powder MP present in the resin material is brought into unmatched condition. In contrast to this unmatched condition, when the respective energizing coils 73 are energized so that magnetic fields are produced around the respective energizing coils 73 , as indicated in FIG. 28 , the orientation of the magnetic powder MP is controlled in correspondence with these generated magnetic fields. In other words, the orientation of the magnetic powder MP may be realized in such a way that the particles of the magnetic powder MP are directed to the respective energizing coils 73 . As a result, in the molded body which is manufactured by the molding apparatus 70 , orientation degrees of the magnetic powder MP of such portions thereof which correspond to the above-described magnet portions XXIB 1 and XXIB 2 are made lower, so that there is a difference in the orientation modes of the magnetic power MP within this molded body. Then, since the molded body having such different orientation modes is magnetized by way of the above-described manufacturing steps (c) and (d), the biasing magnet 13 which generates the previously explained magnetic fields shown in FIG. 22 and FIG. 23 can be manufactured.
Then, the above-described sensor chip 11 is stored in combination with the molding member 12 (see FIG. 19 ) into the hollow portion 14 of the biasing magnet 13 which has been manufactured via the above-described manufacturing steps (a) to (d), and thereafter, the stored structural members are assembled with a case member, and the like, in an integral manner. As a result, the rotation detecting apparatus shown in FIG. 18 may be manufactured.
In the above-described first embodiment mode, the below-listed effects can be achieved:
(1) The biasing magnet 13 has been formed in such a manner that the magnetic strengths of the biasing magnet portions (above-described portions XXIB 1 and XXIB 2 ) which are located opposite to the front/rear arranging planes of the magnetic resistance elements MRE 1 to MRE 4 have been selectively set to the low magnetic field strengths from the edge plane 13 a of this biasing magnet 13 to the opposing plane thereof. As a consequence, the magnetic field strengths at the plane where the magnetic vectors are changed may be selectively set to the low magnetic field strengths. As a result, the components of the magnetic vectors can be relatively strengthened which are produced by the biasing magnetic fields generated from the biasing magnet 13 in conjunction of the rotations of the rotor. In other words, while a relative positional relationship (for example, previously-explained “M-to-M” distance) among the magnetic resistance elements MRE 1 to MRE 4 and the biasing magnet 13 is not always changed, the deflection angles of the magnetic vectors which give influences to the magnetic resistance elements MRE 1 to MRE 4 can be adjusted, and also, the improvement of the sensing sensitivity as the rotation detecting apparatus may be easily realized.
(2) While the biasing magnet 13 may be formed as the molded body of the resin material which contains the magnetic powder, the magnetic field strengths as to the portions which are located opposite to the front/rear planes of the magnetic resistance elements MRE 1 to MRE 4 are selectively set to the low magnetic field strengths in accordance with the differences in the orientation modes of the magnetic powder in the molded body. As a consequence, the above-explained magnetic field strengths can be simply set by suitably utilizing the structure as the above-explained molded body. Also, since the conventional magnet material may be directly utilized, increasing of the manufacturing cost may be suppressed.
(Third Embodiment)
FIG. 29 shows a rotation detecting apparatus according to a third embodiment mode of the present invention, while the rotation detecting apparatus has been arranged based upon the above-described basic idea. Referring now to FIG. 29 , an arrangement of the rotation detecting apparatus according to this third embodiment mode will be described in detail. It should be noted that since a structure as the rotation detecting apparatus is basically identical to the above-described structure of the conventional rotation detecting apparatus, the same reference numerals shown in this conventional rotation detecting apparatus will be employed as those for denoting structural elements having the same, or similar functions, and thus, detailed descriptions thereof are omitted.
FIG. 29 illustratively indicates conditions of magnetic fields which are generated from a biasing magnet 13 employed in the rotation detecting apparatus according to the first embodiment mode, and this drawing corresponds to FIG. 20 . As shown in FIG. 29 , the biasing magnet 13 has been formed in a hollow cylindrical shape and has been provided with a hollow portion 14 . This hollow cylindrical shape of the biasing magnet 13 is not completely different from the shape of the conventional biasing magnet. A sectional shape of the hollow portion 14 is made in a substantially rectangular shape along a direction perpendicular to a longitudinal direction of the biasing magnet 13 . Also, a material for constructing the biasing magnet 13 is the same material as the conventional biasing magnet. However, this biasing magnet 13 owns the below-mentioned different point from the conventional biasing magnet. That is, in this biasing magnet 13 , magnetic strengths of biasing magnet portions which are located opposite to front/rear arranging planes of the magnetic resistance elements MRE 1 to MRE 4 , namely magnetic strengths of magnetic fields as to the above-explained portions XXIB 1 and XXIB 2 (see FIG. 21 ) have been selectively set to low magnetic field strengths from an edge plane 13 a located opposite to the rotor up to such a position which covers the magnetic resistance elements MRE 1 to MRE 4 of the sensor chip 11 . As a consequence, the magnetic fields which are generated from the biasing magnet portions whose magnetic field strengths have been selectively set to the low magnetic field strengths are indicated by arrows made of narrow solid lines, as compared with magnetic fields which are generated from other portions of this biasing magnet 13 .
Then, if an attention is paid to magnetic fields which are generated from the portion “XXIA 1 ” and another portion “XXIA 2 ” (see FIG. 21 ) on the side of the short edges of the hollow portion 14 within the biasing magnet 13 , similar to the previously explained biasing magnet 13 (see FIG. 21 ), then magnetic vectors may be readily deflected which are produced by these generated magnetic fields in conjunction with the rotations of the rotor, and thus, deflection angles thereof are largely secured. To the contrary, within the biasing magnet 13 , field strengths of such magnetic fields which are generated from the portions XXIB 1 and XXIB 2 over the positions for covering the magnetic resistance elements MRE 1 to MRE 4 from the above-described edge plane 13 a have been selectively set to low field strengths, which are different from those of the previously explained biasing magnet 13 . As a result, such magnetic vectors which are produced by the magnetic fields generated from these portions XXIB 1 and XXIB 2 in conjunction with the rotations of the rotor may be easily deflected, as compared with those produced from the previously explained biasing magnet 13 . Accordingly, such magnetic vectors may be suppressed which may block easy deflections of the above-described magnetic vectors which are produced by the magnetic fields generated from the portions XXIA 1 and XXIA 2 in conjunction with the rotations of the rotor. Then, as a consequence, the components of the magnetic vectors can be relatively strengthened, which are produced by the magnetic fields generated from this biasing magnet 13 in conjunction with the rotations of the rotor.
Next, a method of manufacturing the above-explained biasing magnet 13 will now be explained with reference to FIG. 30 and FIG. 31 . It should be understood that since the biasing magnet 13 is basically manufactured by way of the same manufacturing steps as those indicated in the above-described first embodiment mode, different points thereof will be mainly explained.
FIG. 30 shows a molding apparatus 70 for molding the above-explained biasing magnet 13 , and corresponds to the drawing of FIG. 25 . As indicated in FIG. 30 , this molding apparatus 70 has been arranged by employing a molding die 72 which has a cavity 71 corresponding to the shape of the biasing magnet 13 . It should also be noted that this molding die 72 is manufactured by a non-magnetic material. Then, two sets of energizing coils 73 have been arranged in an upper molding die 72 a (see FIG. 31 ) for constituting this molding die 72 , while these two energizing coils 73 may cover the cavity 71 except for such cavity portions corresponding to the above-described magnet portions XXIB 1 and XXIB 2 . To the contrary, an energizing coil 94 which covers the cavity 71 has been arranged in a lower molding die 72 b (see FIG. 31 ) which constitutes the molding die 72 . Thus, orientation of the above-explained magnetic powder may be controlled by operating these energizing coils 73 and energizing coil 94 .
FIG. 31 indicates an orientation mode of the magnetic powder after the orientation of the magnetic powder has been controlled, and corresponds to the drawing of FIG. 28 . When the respective energizing coils 73 and 94 are energized so that magnetic fields are produced around the respective energizing coils 73 and 94 , as indicated in FIG. 31 , the orientation of the magnetic powder MP is controlled in correspondence with these generated magnetic fields. In other words, the orientation of the magnetic powder MP may be realized in such a way that the particles of the magnetic powder MP are directed to the respective energizing coils 73 and 94 . As a result, in the molded body which is manufactured by the molding apparatus 70 , orientation degrees of the magnetic powder MP of such portions thereof which correspond to the above-described magnet portions XXIB 1 and XXIB 2 over the positions for covering the magnetic resistance elements MRE 1 to MRE 4 from the above-described edge plane 13 a of the biasing magnet 13 are made lower, so that there is a difference in the orientation modes of the magnetic power MP within this molded body. Then, since the molded body having such different orientation modes is magnetized by way of the above-described manufacturing steps (c) and (d), the biasing magnet 13 which generates the previously explained magnetic fields shown in FIG. 29 can be manufactured.
In accordance with the above-explained second embodiment mode, the below-mentioned effect can be obtained in addition to such effects which are equivalent to the above-explained effects (1) and (2) of the second embodiment modes.
(3) The biasing magnet 13 has been formed in such a manner that the magnetic strengths of the biasing magnet portions (above-described portions XXIB 1 and XXIB 2 ) which are located opposite to the front/rear arranging planes of the magnetic resistance elements MRE 1 to MRE 4 have been selectively set to the low magnetic field strengths from the edge plane 13 a of this biasing magnet 13 which are located to the rotor over the positions which cover the magnetic resistance elements MRE 1 to MRE 4 . As a result, the orientation controls of the magnetic powder as to such portions except for the portions which are defined from the edge plane 13 a located opposite to the rotor up to the positions which cover the magnetic resistance elements MRE 1 to MRE 4 may be realized in a similar control manner to the prior art, so that increasing of the manufacturing cost can be suppressed by applying the conventional molding die.
It should also be noted that the above-described respective embodiment modes may be alternatively modified so as to be carried out.
That is, in the second embodiment mode, the biasing magnet has been formed in such a manner that the magnetic strengths of the biasing magnet portions which are located opposite to the front/rear arranging planes of the magnetic resistance elements MRE 1 to MRE 4 have been selectively set to the low magnetic field strengths. Alternatively, only such a magnetic field strength as to a portion which is located opposite to the arranging plane of the magnetic resistance elements MRE 1 to MRE 4 may be selectively set to a low magnetic field strength. As a result, as indicated in FIG. 32 corresponding to FIG. 20 such a biasing magnet 13 may be realized in which the magnetic field generated from the portion which is located opposite to the arranging plane of the magnetic resistance elements MRE 1 to MRE 4 is illustratively represented by a solid line whose width is made narrower than that of other portion. Then, magnetic vectors may be easily deflected, as compared with those generated from the previously explained biasing magnet 13 (see FIG. 21 ), while these magnetic vectors are produced from the magnetic field generated from the portion which is located opposite to the arranging plane of the magnetic resistance elements MRE 1 to MRE 4 of this biasing magnet 13 in conjunction with the rotations of the rotor. As a consequence, in such a case that only such a magnetic field strength as to the portion which is located opposite to the arranging plane of the magnetic resistance elements MRE 1 to MRE 4 is selectively set to the lower magnetic field strength, a similar effect to that of the first embodiment mode may also be achieved. It should be understood that when this biasing magnet 13 is manufactured, such a molding apparatus 70 as shown in FIG. 33 corresponding to FIG. 25 is employed. That is, this molding apparatus 70 has been arranged by employing a molding die 72 which has a cavity 71 corresponding to the shape of the biasing magnet 13 . It should also be noted that this molding die 72 is manufactured by a non-magnetic material. Also, this molding apparatus 70 has been constituted by providing two sets of energizing coils 113 at upper and lower portions of the cavity 71 . These two energizing coils 113 may cover the cavity 71 except for the portion which is located opposite to the arranging plane of the magnetic resistance elements MRE 1 to MRE 4 . A method for manufacturing the biasing magnet 13 by using this molding apparatus 70 is carried out in the same manner to that of the first embodiment mode. Also, the above-explained biasing magnet in which only such a magnetic field strength as to the portion which is located opposite to the arranging plane of the magnetic resistance elements MRE 1 to MRE 4 is selectively set to the low magnetic field strength, may also be employed as a modification of the second embodiment mode.
In the above-explained second embodiment mode, the orientation of the magnetic powder contained in the molded body has been controlled by employing this energizing coils 73 . Alternatively, a permanent magnet may be employed. In this alternative case, similar to the above-explained embodiment mode, the orientation of the magnetic powder may be alternatively controlled by using the magnetic fields generated from the permanent magnet. It should also be noted that such a permanent magnet may also be alternatively employed as a modification related to the second embodiment mode.
In each of the above-described embodiment modes, the magnetic field strengths as to the portions which are located opposite to the front/rear planes of the magnetic resistance elements MRE 1 to MRE 4 have been selectively set to the low magnetic field strengths. Alternatively, when such a magnetic field strength is set, for instance, these magnetic field setting operations may be carried out by utilizing demagnetization. In other words, such a biasing magnet whose magnetic field strengths have been substantially uniformly set may be molded by employing a molding apparatus similar to the conventional molding apparatus. Thereafter, magnetic field strengths as to the portions which are located opposite to the front/rear arranging planes of the magnetic resistance elements MRE 1 to MRE 4 may be selectively set to low magnetic field strengths by employing a demagnetizing device (not shown). Also, in this alternative case, such a biasing magnet which generates the magnetic fields as shown in FIG. 22 and FIG. 29 may be realized.
The above-described respective embodiment modes have described such a case of the biasing magnet 13 having the hollow portion 14 , the sectional shape of which has been made in the rectangular shape. Alternatively, even when a biasing magnet having a hollow portion made in another shape is employed, this biasing magnet may be similarly covered by the inventive idea of the present invention. Also, as to the biasing magnet itself, not only such a biasing magnet formed in a hollow cylindrical shape may be employed, but also a biasing magnet formed in another different shape may be employed.
Such changes and modifications are to be understood as being within the scope of the present invention as defined by the appended claims.
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Rotation detecting apparatus for detecting rotation of a magnetic rotor includes: a sensor chip having a magnetoresistive device; and a bias magnet. The magnetoresistive device is capable of detecting change of a magnetic vector near the sensor chip so that the rotation detecting apparatus detects the rotation of the magnetic rotor. The change of the magnetic vector is generated by the bias magnetic field and the rotation of the magnetic rotor. The bias magnet is disposed around the sensor chip so that a deflection angle of the magnetic vector is controllable.
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CO-PENDING, CO-OWNED APPLICATIONS INCORPORATED HEREIN
[0001] The present application incorporates U.S. application Ser. No. ______, filed Apr. 29, 2013, entitled Cutter Assembly and Adjustable Cutter for use in Comminuting Apparatus and U.S. application Ser. No. ______ filed Apr. 29, 2013 entitled Mounting Block for Attaching a Reducing Element to a Rotary Drum, herein by reference for all relevant and consistent purposes.
FIELD OF THE DISCLOSURE
[0002] The field of the disclosure relates to anvils for comminuting apparatus such as grinders or chippers and, in particular, to anvils that are adjustable in length to maintain a clearance between the comminuting drum and a shear edge of the anvil.
BACKGROUND
[0003] Comminuting apparatus such as grinders and chippers are used to mechanically grind, chip or shred material to reduce the size of the material. Such apparatus may be used to reduce the size of material such as tree limbs, stumps or brush (i.e., arboraceous material)in land-clearing, municipal waste, composted materials or other vegetation, building materials or recycled material (e.g., car tires and the like). One common type of reducing machine is known as a horizontal grinder. A horizontal grinder may include a power in-feed mechanism that forces larger material (e.g., wood-based material such as tree trunks, tree branches, logs, etc.) into contact with a rotating comminuting drum. The larger material is contacted by reducing elements such as teeth, grinding elements or “knives” carried by the comminuting drum and portions of the material are forced past a fixed shear edge defined by an anvil of the horizontal grinder.
[0004] Upon passing the shear edge of the anvil, the material enters a chamber in which the material is further reduced by the reducing element carried by the comminuting drum. Once the material within the chamber is reduced in size, the material is discharged. Upon passing through the chamber, the reduced material is typically deposited on a discharge conveyor that carries the reduced material to a collection location. An example of a horizontal grinder is disclosed in U.S. Patent Publication No. 2009/0242677, which is incorporated herein by reference for all relevant and consistent purposes.
[0005] A continuing need exists for comminuting apparatus that maintain proper clearances between shear edges without replacement of comminuting components.
[0006] This section is intended to introduce the reader to various aspects of art that may be related to various aspects of the disclosure, which are described and/or claimed below. This discussion is believed to be helpful in providing the reader with background information to facilitate a better understanding of the various aspects of the present disclosure. Accordingly, it should be understood that these statements are to be read in this light, and not as admissions of prior art.
SUMMARY
[0007] One aspect of the present disclosure is directed to an adjustable anvil for a comminuting apparatus. The adjustable anvil includes a first plate having a trailing edge and a second plate having a leading edge. The first plate and second plate form an anvil work surface for bringing material into contact with a comminuting drum. The trailing edge of the first plate is adjacent the leading edge of the second plate. A margin is disposed between the trailing edge of the first plate and leading edge of the second plate. The margin has an adjustable length.
[0008] Various refinements exist of the features noted in relation to the above-mentioned aspects of the present disclosure. Further features may also be incorporated in the above-mentioned aspects of the present disclosure as well. These refinements and additional features may exist individually or in any combination. For instance, various features discussed below in relation to any of the illustrated embodiments of the present disclosure may be incorporated into any of the above-described aspects of the present disclosure, alone or in any combination.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is a perspective view of an apparatus for reducing the size of material;
[0010] FIG. 2 is a side view of an in-feed system, anvil, feed roller and comminuting drum of the apparatus of FIG. 1 ;
[0011] FIG. 3 is a perspective view of the anvil and comminuting drum;
[0012] FIG. 4 is a perspective view of the anvil;
[0013] FIG. 5 is an exploded view of the anvil;
[0014] FIG. 6 is a top view of a first top plate of the anvil;
[0015] FIG. 7 is a top view of a second top plate of the anvil;
[0016] FIG. 8 is a top view of the first top plate and second top plate with the first top plate abutting the second top plate;
[0017] FIG. 9 is a top view of the first top plate and second top plate with a margin having a length L 2 separating the first top plate and second top plate;
[0018] FIG. 10 is perspective view of a second embodiment of an anvil with rounded edges;
[0019] FIG. 11 is a perspective view of the anvil of FIG. 4 with the second top plate not shown;
[0020] FIG. 12 is a perspective view of the anvil with the second top plate and support plate not shown;
[0021] FIG. 13 is a perspective view of the anvil showing the top plate margin and support plate margin; and
[0022] FIG. 14 is a perspective view of the anvil showing a wider top plate margin and support plate margin relative to FIG. 13 .
[0023] Corresponding reference characters indicate corresponding parts throughout the drawings.
DETAILED DESCRIPTION
[0024] An embodiment of a comminuting apparatus for reducing the size of material is generally referred to as “ 5 ” in FIG. 1 . The apparatus 5 is depicted as a horizontal grinder having a power in-feed system 13 , a comminuting assembly 20 and a discharge conveyor 40 . While the present disclosure has been described with reference to a horizontal grinder, it should be noted that the principles described herein (e.g., an adjustable length anvil) may also apply to any suitable apparatus for comminuting material such as a wood chipper having a chute for discharging comminuted material.
[0025] The in-feed system 13 of the comminuting apparatus 5 includes an in-feed conveyor 15 (e.g., chain or belt) to move the material toward a comminuting drum 25 ( FIG. 2 ) in a feed direction indicated by arrow F. As shown in FIG. 2 , the in-feed system has a first end 37 proximal to an anvil 17 . The anvil 17 is disposed between the conveyor 15 and a comminuting drum 25 to bridge the gap between the conveyor 15 and comminuting drum 25 . A feed roller 30 rotates about an axis in direction R 30 to force material over the anvil 17 and to contact the comminuting drum 25 . The anvil 17 includes a first end 36 adjacent the conveyor 15 and a second end 27 adjacent the drum 25 .
[0026] The comminuting drum 25 carries a plurality of reducing elements 3 (e.g., teeth, blades, knives, etc. and/or combinations of these elements). During operation, the comminuting drum 25 rotates about an axis of rotation in direction R 25 such that the tips of the reducing elements 3 define a circumferential reducing path. In some embodiments (not shown), the apparatus may include a sizing screen that at least partially surrounds the comminuting drum 25 for forming a reducing chamber defined between the comminuting drum and the sizing screen. The principles of the present disclosure (e.g., use of an adjustable width anvil) may apply to apparatus that do not include such sizing screens such as the comminuting apparatus 5 described herein and may also apply to apparatus that include such sizing screens.
[0027] Referring now to FIGS. 3-5 , the anvil 17 includes a first top plate 6 (or simply “first plate) and second top plate 4 (or simply “second plate”). The first top plate 6 ( FIG. 6 ) includes a leading edge 22 (i.e., the edge over which material first passes along feed direction F) and an “undulating” or “serrated” trailing edge 16 . The leading edge 22 of the first top plate 6 may have any suitable profile (e.g., may be essentially straight or serrated). The second top plate 4 ( FIG. 7 ) has a serrated leading edge 14 and a trailing edge 23 . The trailing edge 23 of the second top plate 4 should match the profile of the reducing elements 3 (e.g., essentially straight or serrated depending on the angle (if any) of the reducing elements).
[0028] The first top plate 6 and second top plate 4 form an anvil work surface 24 ( FIG. 8 ) upon which material travels in feed direction F during operation. In this regard, the anvil work surface 24 may be continuous as shown in FIG. 8 or may be discontinuous (e.g., separated by a margin 63 ) as shown in FIG. 9 and discussed further below.
[0029] The trailing edge 16 of the first top plate 6 ( FIG. 6 ) includes a series of projections 39 and indentations 41 that form a serrated zig-zag pattern along the edge. The leading edge 14 of the second top plate 4 ( FIG. 7 ) also includes a series of projections 29 and indentations 31 that form a serrated “zig-zag” pattern along the edge. The projections 29 ( FIG. 7 ) of the second top plate 4 align with the indentations 41 ( FIG. 6 ) of the first top plate 6 and the projections 39 of the first top plate 6 align with the indentations 31 ( FIG. 7 ) of the second top plate 4 which allows the plates 4 , 6 to form a continuous anvil work surface 24 when fully adjoined ( FIG. 8 ). Use of a first top plate 6 and second top plate 4 that have aligned projections and indentations (e.g., that from a “zig-zag” pattern) prevents elongated debris (e.g., sticks or twigs) from being trapped within the top plate margin 63 ( FIG. 13 ). The first top plate 6 and/or second top plate 4 may include more or less projections 29 , 39 and indentations 31 , 41 than as shown in FIGS. 6-7 without departing from the scope of the present disclosure.
[0030] As shown in FIGS. 6-7 , the projections 29 , 39 terminate in a point 43 , 45 . However, the projections 29 , 39 may also be rounded ( FIG. 10 ) or have other suitable shapes. In embodiments in which the projections 29 , 39 are rounded, the radius of curvature of the projections and indentations may be less than about 0.5 cm (about 0.2 inches).
[0031] The anvil 17 includes a shear edge 18 ( FIG. 4 ) for comminuting material as the comminuting drum 25 rotates. The shear edge 18 is formed on an edge member 19 . As the drum 25 rotates, material is gripped between the reducing elements 3 and the shear edge 18 and the rotational force of the drum 25 causes the material to be comminuted. The shear edge 18 is positioned near the second end 27 of the anvil 17 . During use, a radial offset (i.e., clearance) is defined between the reducing elements ( FIG. 2 ) and the shear edge 18 .
[0032] Referring now to FIG. 11 (the second top plate and edge member not being shown), the anvil 17 includes a support plate 26 configured for mounting to the second top plate and edge member ( FIG. 4 ) such that the edge member 19 is mounted adjacent the second top plate 4 opposite the leading edge 14 of the second top plate. As shown in FIG. 11 , the edge member may be mounted by use of threaded bolts 42 . The first top plate 6 is mounted to a base 7 that extends across the trailing edge 16 ( FIG. 6 ) of the first top plate 6 and the leading edge 14 ( FIG. 7 ) of the second top plate 4 and extends beneath the support plate 26 .
[0033] As shown in FIG. 12 , the base 7 includes a ledge 9 adjacent the support plate 26 ( FIG. 11 ). The base 7 may be integral (e.g., the ledge and base surfaces may be attached such as by welding) or the anvil 17 may include various separate components that together form the base 7 . The second top plate 4 and support plate 26 are adjustably mounted to the base 7 . The second top plate 4 may be moved relative to the base 7 by use of first row of lengthwise openings or “through-slots” 33 ( FIG. 12 ) and second row of lengthwise through-slots 11 that extend through the base 7 and are generally perpendicular to the shear edge 18 ( FIG. 4 ). In this manner, the support plate 26 and ledge 9 of the base 7 form an adjustable-length support plate margin 61 having a length L 1 ( FIG. 13 ). Alternatively or in addition, the second top plate 4 may include lengthwise through-slots (not shown) that are generally perpendicular to the shear edge for adjusting the relative position of the second top plate 4 and first top plate 6 (i.e., the length of the margin between the first top plate 6 and second top plate 4 ). It should be noted that a series of through-holes may be substituted for the through-slots formed in the anvil 17 for relative adjustment of the anvil components.
[0034] The second top plate 4 and first top plate 6 form a margin 63 ( FIG. 13 ) having a length L 2 . In embodiments in which projections and indentations extend across the length of the second top plate 4 and first top plate 6 , no portion of the adjustable length margin 63 is parallel to the shear edge 18 and no portion of the adjustable length margin is perpendicular to the shear edge 18 . The margin 61 between the support plate 26 and ledge 9 of the base 7 is offset from the margin 63 between the first top plate 6 and second top plate 4 .
[0035] As shown in FIG. 9 , a first top plate serrated area A 6 is defined by the projections 45 and indentations 41 of the first top plate 6 and a second top plate serrated area A 4 is defined by the projections 43 and indentations 31 of the second top plate 4 . Generally, adjustment of the length of the margin between the first plate 6 and second plate 4 is limited such that the area A 6 of the first top plate 6 remains overlapped with the area A 4 of the second top plate 4 .
[0036] Referring now to FIG. 12 (second top plate, edge member and support plate not being shown), the base 7 is configured for mounting to the second top plate, edge member and support plate. The first row of lengthwise through-slots 11 and the second row of lengthwise through-slots 33 may be used to adjust the position of the second top plate, edge member and support plate relative to the base 7 and top plate 6 . The support plate 26 ( FIG. 11 ) and elements attached thereto may be adjusted relative to the base 7 by loosening bolts 55 , 59 that extend through through-slots 11 , 33 of the base 7 . Bolts 42 , 55 , 59 may be fastened to nut bars 56 a, 56 b, 56 c disposed beneath the base 7 .
[0037] Upon loosening bolts 55 , 59 , push bolts 44 ( FIG. 11 ) that contact an arm 50 of the support plate 26 on each side of the anvil 17 may be rotated to adjust the position of the support plate, second top plate and edge member relative to the base 7 . For example and as shown in FIG. 14 , the margins 61 , 63 may be made relatively wider than the margins 61 , 63 of FIG. 13 . Once repositioning to achieve the desired length L 1 , L 2 of margins 61 , 63 takes place, the bolts 55 , 59 and push bolts 44 may be retightened to maintain the desired alignment.
[0038] The apparatus 5 ( FIG. 1 ) is operable to reduce the size of material such as tree limbs, stumps or brush in land-clearing, municipal waste, composted materials or other vegetation, building materials or recycled material (e.g., car tires and the like). Material is conveyed on the in-feed system 13 ( FIG. 2 ) toward the adjustable anvil 17 and is driven over the anvil toward the comminuting drum 25 . As the drum 25 rotates, material is impacted and reduced in size and is forced through a clearance between the reducing elements 3 mounted on the drum and the edge member 19 .
[0039] Use of the apparatus 5 may cause the shear edge 18 ( FIG. 4 ) of the edge member 19 to become worn causing the clearance between the shear edge and the reducing elements 3 to increase. Such an increase in clearance may cause the product size to be increased to an undesirable amount. When it is desired to decrease the clearance between the shear edge 18 and the reducing elements 3 , the bolts 55 , 59 ( FIG. 11 ) which secure the second top plate 4 and support plate 26 ( FIG. 4 ) may be loosened and the push bolts 44 ( FIG. 11 ) may be rotated to cause the length L 1 , L 2 of the margins 61 , 63 ( FIG. 13 ) to increase, thereby increasing the length of the anvil 17 . After the material is reduced in size, the discharge conveyor 40 ( FIG. 1 ) carries the comminuted material to a desired collection location (e.g., a pile, bin, truck bed, etc.).
[0040] It should be noted that while the length L 2 of the margin 63 between the first top plate 6 and second top plate 4 may be adjusted by manipulating the position of the support plate 26 as described herein, the length of the margin may be adjusted by methods and anvil arrangements other than as described herein without departing from the scope of the present disclosure. In some embodiments (e.g., when an anvil having an unworn edge member is used), the length L 2 of the margin 63 is zero (i.e., the first top plate 4 and second top plate 6 are in an abutting relationship).
[0041] Compared to conventional apparatus for comminuting material, the apparatus described above has several advantages. For example, use of an anvil 17 ( FIG. 4 ) with a first top plate 6 that may be moved relative to a second top plate 4 allows the length of the anvil to be adjusted such as after the edge member 19 has become worn. Accordingly, a relatively consistent clearance length between the anvil and the comminuting drum may be maintained. This capability allows the shear edge 18 ( FIG. 4 ) of the anvil 17 to be kept in an appropriate cutting zone while preventing a large gap at the leading edge 22 of the first plate 6 (i.e., a large gap with the in-feed conveyor 15 ( FIG. 2 )) where material may otherwise become lodged. That is, an acceptable gap may be formed in the anvil mid-section, rather than forming such a break between the anvil and in-feed conveyor.
[0042] Further, the use of a second top plate 4 and support plate 26 that are adjustable relative to the first top plate 6 and ledge 9 of the base 7 allows the top-plate margin 63 and support plate margin 61 ( FIG. 13 ) to be non-aligned. Accordingly, debris is prevented from falling within the support-plate margin 61 . Use of a first top plate 6 and second top plate 4 that have aligned projections and indentations (e.g., that form a “zig-zag” pattern) prevents elongated debris (e.g., sticks or twigs) from being trapped within the top plate margin 63 ( FIG. 13 ). In embodiments in which the projections 29 , 39 ( FIGS. 6 and 7 ) are rounded, using projections 29 , 39 with a radius of curvature of less than about 0.5 cm (about 0.2 inches) also prevents elongated debris from being trapped within the top plate margin 63 ( FIG. 13 ).
[0043] As used herein, the terms “about,” “substantially,” “essentially” and “approximately” when used in conjunction with ranges of dimensions, concentrations, temperatures or other physical or chemical properties or characteristics is meant to cover variations that may exist in the upper and/or lower limits of the ranges of the properties or characteristics, including, for example, variations resulting from rounding, measurement methodology or other statistical variation.
[0044] When introducing elements of the present disclosure or the embodiment(s) thereof, the articles “a”, “an”, “the” and “said” are intended to mean that there are one or more of the elements. The terms “comprising,” “including,” “containing” and “having” are intended to be inclusive and mean that there may be additional elements other than the listed elements. The use of terms indicating a particular orientation (e.g., “top”, “bottom”, “side”, etc.) is for convenience of description and does not require any particular orientation of the item described, unless otherwise expressly stated to the contrary.
[0045] As various changes could be made in the above constructions and methods without departing from the scope of the disclosure, it is intended that all matter contained in the above description and shown in the accompanying drawing[s] shall be interpreted as illustrative and not in a limiting sense.
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The field of the disclosure relates to anvils for comminuting apparatus such as grinders or chippers. In some embodiments, the anvil is adjustable in length to maintain a clearance between a comminuting drum and a shear edge of the anvil.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority benefit under 35 U.S.C. Section 119(e) to U.S. Provisional Patent Ser. No. 61/148,792 filed on Jan. 30, 2009 the entire disclosure of which is incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to a method and a system for liquefying natural gas. In another aspect, the present invention concerns a method and a system for enhancing the production of liquefied natural gas.
BACKGROUND OF THE INVENTION
[0003] The cryogenic liquefaction of natural gas is routinely practiced as a means of converting natural gas into a more convenient form for transportation and storage. Such liquefaction reduces the volume of the natural gas by about 600-fold and results in a product which can be stored and transported at or near atmospheric pressure.
[0004] Natural gas is frequently transported by pipeline from the supply source to a distant market. While it is desirable to operate the pipeline under a substantially constant and high load factor, often the deliverability or capacity of the pipeline will exceed demand while at other times the demand may exceed the deliverability of the pipeline. In order to shave off the peaks where demand exceeds supply or the valleys when supply exceeds demand, it is desirable to store the excess gas in such a manner that it can be delivered when demand exceeds supply. Such practice allows future demand peaks to be met with material from storage. One practical means for doing this is to convert the gas to a liquefied state for storage and to then vaporize the liquid as demand requires.
[0005] The liquefaction of natural gas is of even greater importance when transporting gas from a supply source which is separated by great distances from the candidate market and a pipeline either is not available or is impractical. This is particularly true where transport must be made by ocean-going vessel. Ship transportation in the gaseous state is generally not practical because appreciable pressurization is required to significantly reduce the specific volume of the gas. Such pressurization requires the use of more expensive storage containers.
[0006] In order to store and transport natural gas in the liquid state, the natural gas is preferably cooled to −240° F. to −260° F. where the liquefied natural gas (LNG) possesses a near-atmospheric vapor pressure. Numerous systems exist in the prior art for the liquefaction of natural gas in which the gas is liquefied by sequentially passing the gas at an elevated pressure through a plurality of cooling stages whereupon the gas is cooled to successively lower temperatures until the liquefaction temperature is reached. Cooling is generally accomplished by indirect heat exchange with one or more refrigerants such as propane, propylene, ethane, ethylene, methane, nitrogen, carbon dioxide, or combinations of the preceding refrigerants (e.g., mixed refrigerant systems).
[0007] In any natural gas liquefaction process, there will be progressive accumulation of buildup upon the interior surfaces of the cryogenic heat exchanger. Such buildup can be caused by water in the form of ice or relatively heavy hydrocarbons present in the gas feed in solid form. The various sections of the cryogenic heat exchanger operate at different temperatures depending upon what stream is passing through a particular section. For example, one section of the cryogenic heat exchanger can operate at an inlet temperature of −35° F. and an outlet temperature of −50° F., while a nearby or contiguous section can operate at an inlet temperature of −147° F. and an outlet temperature of −103° F., while yet another nearby or contiguous section in the cryogenic heat exchanger can operate at an inlet temperature of −147° F. and an outlet temperature of −204° F. Thus, it can be seen that a specific stream containing materials having various freeze points may pass through one or more sections of the unit without forming a buildup, but the same stream may encounter a separate section operating at a lower temperature than the other section(s), and buildup can ultimately result thus adversely affecting the overall heat transfer efficiency of the unit. Build-up of solids in these cryogenic heat exchangers, control valves and other associated equipment can lead to reduced heat transfer, high pressure drop and/or reduced flow resulting in a decrease in LNG production.
[0008] Therefore, a need exists for the removal, or de-riming, of heavy hydrocarbons that precipitate, wax up or freeze in the passages of cryogenic heat exchangers, control valves and other associated equipment.
SUMMARY OF THE INVENTION
[0009] In an embodiment of the present invention, a method of removing buildup in a heat exchanger, the method includes: (a) closing a first inlet valve of pumping vessel, wherein the first inlet valve controls a supply of a solvent into the pumping vessel, wherein the pumping vessel is a positive displacement pumping vessel, wherein the solvent is liquid petroleum gas; (b) closing a first exit valve of the pumping vessel, wherein the first exit valve controls a supply of a solvent exiting the pumping vessel; (c) closing a second inlet valve of the pumping vessel, wherein the second inlet valve controls a supply of a method gas into the pumping vessel, wherein the method gas is capable of exiting with the solvent without negatively impacting the integrity of the solvent, wherein the method gas is a high pressure method gas; (d) continuously opening and closing a second exit valve to maintain pressure within the pumping vessel, wherein the second exit valve controls a supply of the method gas exiting the pumping vessel; (e) opening the first inlet valve to introduce the solvent into the pumping vessel, wherein the pumping vessel includes a pumping vessel housing forming a pumping vessel chamber and a moveable float located within the pumping vessel chamber, wherein the moveable float is attached to the pumping vessel chamber by a mechanical linkage; (f) engaging the moveable float by continuously introducing solvent into the pumping vessel chamber until the solvent reaches a predetermined level, wherein upon reaching the predetermined level the mechanical linkage of the moveable float engages to close the first inlet valve, to close the second exit valve, and to open the second inlet valve; (g) opening the first exit valve of the pumping vessel to discharge the solvent, wherein the discharged solvent is injected into the heat exchanger, wherein the solvent is injected into the heat exchanger at a variable rate; (h) closing the first exit valve of the pumping vessel; and (i) closing the second inlet valve of the pumping vessel.
[0010] In another embodiment of the present invention, a method of removing buildup in a heat exchanger, the method includes: (a) closing a first inlet valve of pumping vessel, wherein the first inlet valve controls a supply of a solvent into the pumping vessel; (b) closing a first exit valve of the pumping vessel, wherein the first exit valve controls a supply of a solvent exiting the pumping vessel; (c) closing a second inlet valve of the pumping vessel, wherein the second inlet valve controls a supply of a method gas into the pumping vessel; (d) continuously opening and closing a second exit valve to maintain pressure within the pumping vessel, wherein the second exit valve controls a supply of the method gas exiting the pumping vessel; (e) opening the first inlet valve to introduce the solvent into the pumping vessel, wherein the pumping vessel includes a pumping vessel housing forming a pumping vessel chamber and a moveable float located within the pumping vessel chamber, wherein the moveable float is attached to the pumping vessel chamber by a mechanical linkage; (f) engaging the moveable float by introducing solvent into the pumping vessel chamber until the solvent reaches a predetermined level, wherein upon reaching the predetermined level the mechanical linkage of the moveable float engages to close the first inlet valve, to close the second exit valve, and to open the second inlet valve; (g) opening the first exit valve of the pumping vessel to discharge the solvent, wherein the discharged solvent is injected into the heat exchanger; (h) closing the first exit valve of the pumping vessel; and (i) closing the second inlet valve of the pumping vessel.
[0011] In yet another embodiment of the present invention, a system for removing buildup in a heat exchanger, the system includes: (a) a pumping vessel, wherein the pumping vessel includes: (i) a pump housing forming a pump chamber, (ii) a moveable float located within the pump chamber, wherein the moveable float is attached to the pump chamber by a mechanical linkage, (iii) a first inlet leading into the pump chamber, wherein the first inlet introduces a solvent into the pump chamber, (iv) a first inlet valve for controlling supply of the solvent into the pump chamber, (v) a first exit, wherein the first exit discharges the solvent from the pump chamber, (vi) a first exit valve for controlling the discharge of solvent exiting the pump chamber, (vii) a second inlet leading into the pump chamber, wherein the second inlet introduces a process gas into the pump chamber, (viii) a second inlet valve for controlling supply of the process gas into the pump chamber, (ix) a second exit, wherein the second exit discharges process gas from the pump chamber, (x) a second exit valve for controlling the discharge of solvent exiting the pump chamber; and (b) a heat exchanger, wherein the first exit and the first exit valve are between the pumping vessel and the heat exchanger, and wherein the heat exchanger is configured to receive the solvent.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] The present invention is shown by way of example and not by limitation in the accompanying figures, in which:
[0013] FIG. 1 is a schematic diagram of one embodiment of the deriming process according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0014] Reference will now be made in detail to embodiments of the invention, one or more examples of which are illustrated in the accompanying drawings. Each example is provided by way of explanation of the invention, not as a limitation of the invention. It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope or spirit of the invention. For instance, features illustrated or described as part of one embodiment can be used in another embodiment to yield a still further embodiment. Thus, it is intended that the present invention cover such modifications and variations that come within the scope of the appended claims and their equivalents.
[0015] A cascaded LNG process uses one or more refrigerant systems for sequentially transferring heat energy from the natural gas stream to the environment where different refrigeration systems may use different refrigerants. Each refrigeration system functions as a heat pump by removing heat energy from the natural gas stream as the stream is progressively cooled to lower and lower temperatures. In so doing, the thermal energy removed from the natural gas stream is ultimately rejected (pumped) to the environment via energy exchange with one or more refrigerants.
[0016] The design of a cascaded refrigeration process involves the balancing of thermodynamic efficiencies and capital costs. In heat transfer processes, thermodynamic irreversibilities are reduced as the temperature gradients between heating and cooling fluids become smaller, but obtaining such small temperature gradients generally requires significant increases in the amount of heat transfer area, major modifications to various process equipment and the proper selection of flow rates through such equipment so as to ensure that both flow rates and approach and outlet temperatures are compatible with the required heating/cooling duty.
[0017] One of the most efficient and effective means of liquefying natural gas is via an optimized cascade-type operation in combination with expansion-type cooling. Such a liquefaction process is comprised of the sequential cooling of a natural gas stream at an elevated pressure, for example about 625 psia, by passage through a multistage propane cycle, a multistage ethane or ethylene cycle, and an open-end methane cycle which utilizes a portion of the feed gas as a source of methane and which includes therein a multistage expansion cycle to further cool the same and reduce the pressure to near-atmospheric pressure. In the sequence of cooling cycles, the refrigerant having the highest boiling point is utilized first followed by a refrigerant having an intermediate boiling point and finally by a refrigerant having the lowest boiling point. As used herein, the term “propane chiller” shall denote a cooling system that employs a refrigerant having a boiling point the same as, or similar to, that of propane or propylene. As used herein, the term “ethylene chiller” shall denote a cooling system that employs a refrigerant having a boiling point the same as, or similar to, that of ethane or ethylene. As used herein, the terms “upstream” and “downstream” shall be used to describe the relative positions of various components of a natural gas liquefaction plant along the flow path of natural gas through the plant.
[0018] Various pretreatment steps provide a means for removing undesirable components, such as acid gases, mercaptan, mercury, and moisture from the natural gas feed stream delivered to the facility. The composition of this gas stream may vary significantly. As used herein, a natural gas stream is any stream principally comprised of methane which originates in major portion from a natural gas feed stream, such feed stream for example containing at least 85 percent methane by volume, with the balance being ethane, higher hydrocarbons, nitrogen, carbon dioxide and a minor amounts of other contaminants such as mercury, hydrogen sulfide, and mercaptan. The pretreatment steps may be separate steps located either upstream of the cooling cycles or located downstream of one of the early stages of cooling in the initial cycle. The following is a non-exclusive listing of some of the available means which are readily available to one skilled in the art: (1) acid gases and to a lesser extent mercaptan are routinely removed via a sorption process employing an aqueous amine-bearing solution; (2) a major portion of the water is routinely removed as a liquid via two-phase gas-liquid separation following gas compression and cooling upstream of the initial cooling cycle and also downstream of the first cooling stage in the initial cooling cycle; (3) mercury is routinely removed via mercury sorbent beds and (4) residual amounts of water and acid gases are routinely removed via the use of properly selected sorbent beds such as regenerable molecular sieves.
[0019] The pretreated natural gas feed stream is generally delivered to the liquefaction process at an elevated pressure or is compressed to an elevated pressure, that being a pressure greater than 500 psia, preferably about 500 psia to about 900 psia, still more preferably about 500 psia to about 675 psia, still yet more preferably about 600 psia to about 675 psia, and most preferably about 625 psia. The stream temperature is typically near ambient to slightly above ambient. A representative temperature range being 60° F. to 138° F.
[0020] As previously noted, the natural gas feed stream is cooled in a plurality of multistage (for example, three) cycles or steps by an indirect heat exchange with a plurality of refrigerants, preferably three. As used herein, the term “heat exchanger” broadly means any device capable of transferring heat from one media to another media, including particularly any structure, e.g., device commonly referred to as a heat exchanger. Thus, the heat exchanger may be a plate-fin, shell-and-tube, spiral core-in-kettle or any other type of heat exchanger. Preferably, the heat exchanger is a brazed aluminum plate-fin type. The overall cooling efficiency for a given cycle improves as the number of stages increases but this increase in efficiency is accompanied by corresponding increases in net capital cost and process complexity. The feed gas is preferably passed through an effective number of refrigeration stages, nominally two, preferably two to four, and more preferably three stages, in the first closed refrigeration cycle utilizing a relatively high boiling refrigerant. Such refrigerant is preferably comprised in major portion of propane, propylene or mixtures thereof, more preferably the refrigerant comprises at least about 75 mole percent propane, even more preferably at least 90 mole percent propane, and most preferably the refrigerant consists essentially of propane.
[0021] Thereafter, the processed feed gas flows through an effective number of stages, nominally two, preferably two to four, and more preferably two or three, in a second closed refrigeration cycle in heat exchange with a refrigerant having a lower boiling point. Such refrigerant is preferably comprised in major portion of ethane, ethylene or mixtures thereof, more preferably the refrigerant comprises at least about 75 mole percent ethylene, even more preferably at least 90 mole percent ethylene, and most preferably the refrigerant consists essentially of ethylene. Each cooling stage comprises a separate cooling zone. As previously noted, the processed natural gas feed stream is combined with one or more recycle streams (i.e., compressed open methane cycle gas streams) at various locations in the second cycle thereby producing a liquefaction stream. In the last stage of the second cooling cycle, the liquefaction stream is condensed (i.e., liquefied) in major portion, preferably in its entirety thereby producing a pressurized LNG-bearing stream. Generally, the process pressure at this location is only slightly lower than the pressure of the pretreated feed gas to the first stage of the first cycle.
[0022] Generally, the natural gas feed stream will contain such quantities of C 2 + components so as to result in the formation of a C 2 + rich liquid in one or more of the cooling stages. This liquid is removed via gas-liquid separation means, preferably one or more conventional gas-liquid separators. Generally, the sequential cooling of the natural gas in each stage is controlled so as to remove as much as possible of the C 2 and higher molecular weight hydrocarbons from the gas to produce a gas stream predominating in methane and a liquid stream containing significant amounts of ethane and heavier components. An effective number of gas/liquid separation means are located at strategic locations downstream of the cooling zones for the removal of liquid streams rich in C 2 + components. The exact location and number of gas/liquid separation means, preferably conventional gas/liquid separators, will be dependant on a number of operating parameters, such as the C 2 + composition of the natural gas feed stream, the desired BTU content of the LNG product, the value of the C 2 + components for other applications and other factors routinely considered by those skilled in the art of the LNG plant and gas plant operation. The C 2 + hydrocarbon stream or streams may be demethanized via a single stage flash or a fractionation column. In the latter case, the resulting methane-rich stream can be directly returned at pressure to the liquefaction process. In the former case, the methane-rich stream can be repressurized and recycled or can be used as fuel gas. The C 2 + hydrocarbon stream or streams or the demethanized C 2 + hydrocarbon stream may be used as fuel or may be further processed such as by fractionation in one or more fractionation zones to produce individual streams rich in specific chemical constituents (e.g., C 2 , C 3 , C 4 and C 5 +).
[0023] The pressurized LNG-bearing stream is further cooled in a third cycle or step referred to as the open methane cycle via contact in a main methane economizer with flash gases (i.e., flash gas streams) generated in this third cycle in a manner to be described later and via expansion of the pressurized LNG-bearing stream to near atmospheric pressure. The flash gasses used as a refrigerant in the third refrigeration cycle are preferably comprised in major portion of methane, more preferably the refrigerant comprises at least about 75 mole percent methane, still more preferably at least 90 mole percent methane, and most preferably the refrigerant consists essentially of methane. During expansion of the pressurized LNG-bearing stream to near atmospheric pressure, the pressurized LNG-bearing stream is cooled via at least one, preferably two to four, and more preferably three expansions where each expansion employs as a pressure reduction means either Joule-Thomson expansion valves or hydraulic expanders. The expansion is followed by a separation of the gas-liquid product with a separator. When a hydraulic expander is employed and properly operated, the greater efficiencies associated with the recovery of power, a greater reduction in stream temperature, and the production of less vapor during the flash step will frequently more than off-set the more expensive capital and operating costs associated with the expander. In one embodiment, additional cooling of the pressurized LNG-bearing stream prior to flashing is made possible by first flashing a portion of this stream via one or more hydraulic expanders and then via indirect heat exchange means employing said flash gas stream to cool the remaining portion of the pressurized LNG-bearing stream prior to flashing. The warmed flash gas stream is then recycled via return to an appropriate location, based on temperature and pressure considerations, in the open methane cycle and will be recompressed.
[0024] When the pressurized LNG-bearing stream, preferably a liquid stream, entering the third cycle is at a preferred pressure of about 550-650 psia, representative flash pressures for a three stage flash process are about 170-210, 45-75, and 10-40 psia. Flashing of the pressurized LNG-bearing stream, preferably a liquid stream, to near atmospheric pressure produces an LNG product possessing a temperature of about −240° F. to −260° F.
[0025] The liquefaction process may use one of several types of cooling which include but is not limited to (a) indirect heat exchange, (b) vaporization, and (c) expansion or pressure reduction. Indirect heat exchange, as used herein, refers to a process wherein the refrigerant cools the substance to be cooled without actual physical contact between the refrigerating agent and the substance to be cooled. Specific examples of indirect heat exchange means include heat exchange undergone in a shell-and-tube heat exchanger, a core in-kettle heat exchanger, and a brazed aluminum plate-fin heat exchanger. The physical state of the refrigerant and substance to be cooled can vary depending on the demands of the system and the type of heat exchanger chosen. Thus, a shell-and-tube heat exchanger will typically be utilized where the refrigerating agent is in a liquid state and the substance to be cooled is in a liquid or gaseous state or when one of the substances undergoes a phase change and process conditions do not favor the use of a core-in-kettle heat exchanger. As an example, aluminum and aluminum alloys are preferred materials of construction for the core but such materials may not be suitable for use at the designated process conditions. A platefin heat exchanger will typically be utilized where the refrigerant is in a gaseous state and the substance to be cooled is in a liquid or gaseous state. Finally, the core-in-kettle heat exchanger will typically be utilized where the substance to be cooled is liquid or gas and the refrigerant undergoes a phase change from a liquid state to a gaseous state during the heat exchange.
[0026] Vaporization cooling refers to the cooling of a substance by the evaporation or vaporization of a portion of the substance with the system maintained at a constant pressure. Thus, during the vaporization, the portion of the substance which evaporates absorbs heat from the portion of the substance which remains in a liquid state and hence, cools the liquid portion.
[0027] Finally, expansion or pressure reduction cooling refers to cooling which occurs when the pressure of a gas, liquid or a two-phase system is decreased by passing through a pressure reduction means. In one embodiment, this expansion means is a Joule-Thomson expansion valve. In another embodiment, the expansion means is either a hydraulic or gas expander. Because expanders recover work energy from the expansion process, lower process stream temperatures are possible upon expansion.
[0028] As previously discussed the present invention focuses on the removal or deriming of the progressive accumulation of buildup, such as water in the form of ice and relatively heavy hydrocarbons present in the gas feed in solid form, upon the interior surfaces of the cryogenic heat exchanger.
[0029] Referring to FIG. 1 , a pumping vessel 20 provides a mechanism for injecting solvent into the cryogenic heat exchanger 10 . The pumping vessel includes a first inlet valve 22 for controlling supply of solvent into the pumping vessel, a first exit valve 24 for solvent exiting the pumping vessel, a second inlet valve 26 for controlling supply of process gas into the pumping vessel, and a second exit valve 28 for process gas exiting the pumping vessel.
[0030] The process begins with a minimal amount of solvent in the pump chamber of the pumping vessel. FIG. 1 depicts this minimal amount of solvent via line 11 . The first inlet valve 22 , the second inlet valve 26 , and the first exit valve 24 are all in closed positions, while the process gas exit valve 28 is continuously opening and closing as necessary to maintain appropriate pressure within the pumping vessel 20 . The first inlet valve 22 is then open to allow the solvent to enter the pumping vessel 20 via conduit 2 in an effort to fill the vessel. As the pumping vessel 20 chamber fills with solvent, a float within the pump chamber, not pictured, begins to rise as the amount of deriming solvent increases. When the float reaches a predetermined level, level 12 in FIG. 1 , the float operates as a snap-action mechanical linkage to close the first valve 22 , to then close the second valve 28 , and to then open the second inlet valve 26 allowing for entry of the process gas via conduit 6 in an effort to pressurize the vessel. The snap-action mechanical linkage ensures a rapid changeover from filling to pumping. Thus, as the pressure inside the pump increases above the back pressure, the solvent is forced through the first exit valve 24 and injected into the cryogenic heat exchanger 10 via conduit 12 . After discharge, the first exit valve 24 is closed followed by the process gas inlet valve 26 thus placing the vessel back in pressure control.
[0031] In an embodiment, the pumping vessel 20 is a positive displacement pump. In another embodiment, the pumping vessel is a blowcase. In yet another embodiment, the pumping vessel is a steam condensate pump. In a further embodiment, the pumping vessel is a mechanical pressure powered pump.
[0032] The process gas utilized in the pumping vessel is capable of co-existing with the deriming solvent without negatively impacting the integrity of the solvent. In an embodiment, a high pressure process gas is utilized.
[0033] As previously discussed, the injection of the solvent into the cryogenic heat exchanger assists in the alleviation and elimination of progressive accumulation of buildup within the cryogenic heat exchanger, while allowing the deriming solvent to be delivered to the cryogenic heat exchanger at a variable rate, i.e., continuous or intermittent injection. In an embodiment, the injection can be provided as a slug for high rate injection, i.e., slug deriming. In another embodiment, the injection can be provided as metered into the system. In an embodiment, if the injection is provided as metered into the system a needle valve can be utilized, or a flow control valve can be utilized or any other control system to provide a relatively constant time-averaged rate of injection for continuous deriming of the heat exchanger.
[0034] In an embodiment, the solvent is a deriming solvent. In another embodiment, the solvent is liquid hydrocarbon. In another embodiment, the solvent is liquid petroleum gas (LPG). However, other liquid hydrocarbons which can be expected to be suitable for deriming the interior surfaces of the cryogenic heat exchanger are also of significant importance in the practice of this invention. For example, suitable solvent can include liquefied gas mixtures containing varying fraction of approximately 0.1 to approximately 80 volume percent or higher methane, ethane, propane, butane, pentane and hexane from distillation.
[0035] The preferred embodiment of the present invention has been disclosed and illustrated. However, the invention is intended to be as broad as defined in the claims below. Those skilled in the art may be able to study the preferred embodiments and identify other ways to practice the invention that are not exactly as described in the present invention. It is the intent of the inventors that variations and equivalents of the invention are within the scope of the claims below and the description, abstract and drawings not to be used to limit the scope of the invention
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The invention relates to a method and apparatus relate for the liquefaction of natural gas. In another aspect, the present invention concerns the deriming the interior surfaces of a cryogenic heat exchanger employed in the liquefaction of natural gas. In another aspect, the present invention concerns the utilization of a pump to derim the interior surfaces of a cryogenic heat exchanger.
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FIELD OF THE INVENTION
[0001] The invention relates generally to chemical dispensing systems for laundry, ware-wash, and healthcare, and more particularly to systems and methods for automatic control of product dispensing in a chemical dispensing system.
BACKGROUND OF THE INVENTION
[0002] The dispensing of liquid chemical products from one or more chemical receptacles is a common requirement of many industries, such as the laundry, textile, ware wash, healthcare instruments, and food processing industries. For example, in an industrial laundry facility, one of several operating washing machines will require, from time to time, aqueous solutions containing quantities of alkaloid, detergent, bleach, starch, softener and/or sour. Increasingly, such industries have turned to automated methods and systems for dispensing chemical products. Such automated methods and systems provide increased control of product use and reduce human contact with potentially hazardous chemicals.
[0003] Contemporary automatic chemical dispensing systems used in the commercial washing industry typically rely on pumps to deliver liquid chemical products from bulk storage containers. Generally, these pumps deliver raw product to a washing machine via a flush manifold, where the product is mixed with a diluent, such as water, that delivers the chemical product to the machine. A typical chemical dispensing system used to supply a washing machine will include a controller that is coupled to one or more peristaltic pumps in a pump-stand by a plurality of dedicated signal lines. The controller will also typically be coupled to a washing machine interface by another plurality of dedicated signal lines, so that the controller is provided with signals indicating the operational state of the machine. In operation, the machine interface transforms high voltage trigger signals generated by the washing machine into lower voltage signals suitable for the controller, and transmits these low voltage trigger signals to the controller over the set of dedicated signal lines, which are typically in the form of a multi-conductor cable. In response to these individual trigger signals, the controller will individually activate one or more of the pump-stands over another set of dedicated lines so that the pumps dispense a desired amount of a chemical product into the flush line. The chemicals are then are mixed with a dilutant before being delivered to the machine.
[0004] In the chemical dispensing system described above, the controller is connected to each washing machine trigger signal output and pump by a dedicated line, and the controller directly activates and deactivates each of the pumps. This arrangement, while generally satisfactory for its intended purpose, places practical limits on how many trigger signals and pumps can be connected to a single controller and creates a need for large numbers of wires and controller input ports. Installation of these types of systems can be cumbersome since installers must keep track of each signal line and ensure that the each line couples the proper controller port to the proper trigger signal source or pump. An incorrect connection may result in the wrong chemical being dispensed at the wrong time by the system, and may not be immediately apparent, resulting in many incorrectly processed loads and resulting monetary losses. Moreover, because the controller is merely switching the pumps on and off for an amount of time expected to provide a desired amount of chemical to the flush manifold, the controller receives no feedback regarding whether the pump is actually dispensing the amount of product desired.
[0005] Chemical dispensing systems employed with commercial washing machines typically employ peristaltic pumps to minimize both operator and system component contact with the chemical products, which are often corrosive and toxic. Peristaltic pumps of this type include a flexible tube (or squeeze tube) and a rotor with one or more rollers located in a pump chamber. The one or more rollers compress a section of the squeeze tube against a wall of a pump chamber, pinching off the section of squeeze tube. When the rotor is rotated, the location of the pinched section of the squeeze tube moves along the length of the tube, thereby forcing, or pumping, fluid through the tube. The amount of fluid pumped per unit time tends to vary from pump to pump, depending on multiple variables such as the speed with which the rotor turns, the interior diameter of the squeeze tube, and the viscosity of the product being dispensed. Therefore, system installers must perform calibration measurements on each pump so that the system controller dispenses accurate amounts of product. This requirement for calibrating each pump during installation greatly increases installation time and expense.
[0006] Squeeze tubes are also subject to wear over time from the repeated compression and pulling of the rollers, which causes the volume of chemical pumped by the pump-stand to vary over time. Worn out squeeze tubes must also be periodically replaced to prevent tube failure. Squeeze tube replacement can be a cumbersome endeavor, as chemical product often leaks from the feed lines when the seal is broken between the squeeze tube and feeder tubes. In addition to causing a loss of product and undesirably exposing workers to potentially hazardous chemicals, the spilled product may also contaminate the surfaces of the squeeze tube and pump chamber. If the chemical product is not sufficiently cleaned from these surfaces, the resulting sticky residue can cause the roller to pull the squeeze tube through the pump chamber so that the tube becomes damaged or tangled, resulting in pump failure and further potential product spills. In addition, because the controller cannot determine that the pump is not dispensing the correct amount of product, any processed wash loads that rely on the failed pump will have to be re-processed. Further, because the timing of the pump failure may be difficult to determine, multiple wash loads may have to be reprocessed.
[0007] Therefore, there is a need in the art for improved chemical dispensing system components and methods that more accurately and reliably control the dispensing of chemical products into washing machines, and that reduce the maintenance burden and number of potential failure modes associated with peristaltic pumps.
SUMMARY OF THE INVENTION
[0008] In a first aspect of the invention, a chemical dispensing system controller includes a plurality of serial data bus interfaces that allow the system controller to communicate with other chemical dispensing system components over one or more intelligent networks. To this end, the system controller may include serial data bus interfaces that provide communications between the system controller and a plurality of pump controllers, machine interfaces, network gateways, as well as other system controllers. The system controller may also include additional serial bus interfaces to accommodate future system expansion. By communicating over serial data buses instead of using dedicated signaling lines, the system controller may reduce the number of physical connections required between the dispensing system components, thereby increasing system reliability and reducing installation time. The flexibility provided by digital communications over the serial data buses also provides additional advantages to the chemical dispensing system, such as providing support for more intelligent system components as well as future system improvements, the addition of new features, and system expansion.
[0009] To support networking functions between the system controller and the pump-stand, each pump includes a pump controller with a user selectable serial data bus address. The system controller controls the timing and amounts of chemicals dispensed to the washing machine by communicating with individual pump controllers connected to the pump controller serial data bus interface using the user selectable addresses. The pump controller provides several advantages to the chemical dispensing control system in addition to supporting the system controller networking function, such as improved dispensing accuracy and pump status monitoring.
[0010] In a second aspect of the invention, the pump controller may be loaded with pump calibration data at the factory. The pump calibration data is accessible to the pump and system controllers and is used to calculate pump run times and/or the number of pump rotor rotations necessary to deliver a desired amount of chemical product. Advantageously, by loading pump calibration data into the pump controller at the factory, the need to perform pump-stand calibrations during installation is reduced or eliminated, thereby reducing installation time and expense.
[0011] In a third aspect of the invention, the chemical dispensing system tracks the operational time and/or number of operational cycles on each of the squeeze tubes installed in the pumps. Using test data regarding the expected service life of the squeeze tube, the chemical dispensing system estimates the remaining service life of the tube from aging and wear based on the operational conditions (e.g., age, type of chemicals pumped, amount of chemicals pumped, etc.) experienced by the squeeze tube. The chemical dispensing system may then report out the estimated remaining tube life, as well as provide an indication to system operators when a squeeze tube should be replaced because the squeeze tube is nearing the end of its useful service life. Tracking estimated remaining service life may also provide additional operational benefits and advantages to the dispensing system.
[0012] For example, to improve produce dispensing accuracy, the chemical dispensing system may adjust pump activation periods for a specific output based on expected changes in pump capacity due to estimated wear and aging of the squeeze tube. To this end, the pump controller may increase the amount of time the pump is activated for a given amount of product to be dispensed as the squeeze tube ages to compensate for an expected reduction in pump capacity. The pump controller may thereby improve pump dispensing accuracy over the life of the squeeze tube. When the squeeze tube is replaced, the time and usage tracking in the pump controller may be reset by a system operator through a user interface on the system controller. The system controller may also provide an interface that allows the system operator to update the pump calibration data based on a new pump calibration.
[0013] In a fourth aspect of the invention, the system controller controls the amount and type of chemical product dispensed by sending data addressed to the pump controller for the pump from which a desired amount of chemical is to be dispensed. The data includes data indicative of the amount of chemical product to be dispensed, which the pump controller uses to determine the amount of time and/or number of rotor rotations for which to activate the pump. The pump controller may also use stored calibration data and/or wear data for the squeeze tube to adjust the pump activation period. In an alternative embodiment, the system controller may retrieve the calibration data from the pump controller and use the calibration data to determine an activation period for the pump. In either case, once the required activation period is determined and communicated to the pump controller, the pump controller activates the pump for the determined period, thereby supplying the desired amount of chemical product to the washing machine.
[0014] Advantageously, by communicating the amount of product to be dispensed to the pump controller rather than directly activating and deactivating the pump, the pump may more accurately dispense the desired amount of chemical product. More advantageously, because the pump controller controls activation of the pump locally, if communication is lost between the system controller and pump controller after activation of the pump (for example, due to a loose or intermittent connection), the pump controller can still dispense the desired amount of product. This is in contrast to a pump activated directly by a system controller, which might stop dispensing chemical product prematurely upon loss of communications with the system controller, or worse yet, might continue running indefinitely if communications are lost between the time the pump is activated and the time the deactivation signal is sent.
[0015] To further improve the accuracy of the amount of product dispensed, the pump controller may be coupled to one or more temperature sensors that provide signals indicating the temperature of the chemical product that the pump is dispensing. Advantageously, this may improve the accuracy of the chemical dispensing over a range of temperatures. For example, if a container of chemical product that was recently delivered (or that is stored in an unheated area) is coupled to the pump, the temperature of the product could be substantially different from the temperature of the product used to calibrate the pump. To account for the effect of viscosity on the amount of product dispensed, the pump controller may use information regarding the temperature of the product to calculate the viscosity of the product, and adjusts pump activation periods accordingly.
[0016] In a fifth aspect of the invention, each pump controller may include a detection circuit that allows the pump controller to determine if the product container to which it is coupled is running low on product. To this end, the pump controller may include ports which may be coupled to product level probes that provide signals indicative of the amount of chemical product left in a product container coupled to the pump. In response to sensing that the product is running low, the pump controller may activate local alarms (such as a flashing LED or buzzer) and/or communicate the product level condition to the system controller over the serial data bus. In response to receiving a low level product condition message from the pump controller, the system controller may also activate a local alarm, and/or send an alarm message to the system operator through a network gateway.
[0017] To provide an out of product indication to the system, the pump controller may begin tracking the amount of chemical product dispensed beginning from the time at which a low level indication is received from a product level probe. If the low level indication is not cleared by refilling or replacing the container before a predetermined amount of additional product is dispensed, the pump controller may stop activating the pump and inform the system controller that the product has run out. Advantageously, this allows the chemical dispensing system to keep operating up until the point where a chemical product is about to run out, but prevents the system from operating without sufficient chemical product to properly process wash loads.
[0018] In an alternative embodiment, the pump may include an integrated out-of-product detection capability. This integrated out-of-product detection capability includes conductive plastic inserts in the flow path of the product so that the conductive plastic inserts are in contact with product passing through the pump. The conductive plastic inserts are electrically coupled to the detection circuit in the pump controller. The detection circuit is sensitive to the impedance between the inserts so that when product is present in the line between the inserts, the impedance presented causes the detection circuit to provide an indication to the pump controller that product is present. However, when product is not present in the line, such as if the pump begins drawing air from an empty chemical product container, the impedance between the conductive plastic inserts increases. This increase in impedance between the conductive plastic inserts, in turn, causes the detection circuit to provide an indication to the pump controller that the chemical product has run out. In response, the pump controller stops activating the pump and informs the system controller that the product has run out. Advantageously, this provides an additional mechanism that prevents the chemical dispensing system from operating when a chemical product has run out, thereby preventing the system from operating when there is insufficient chemical product to properly process wash loads. The pump controller may also activate local or remote alarms indicating an out product condition so that the condition is brought the attention of the system operator.
[0019] The system controller may include a selectable alarm notification feature that allows the system operator to select the types of alarms that are activated, as well as the time and duration of the alarms, based on the condition causing the alarm. Advantageously, this feature allows the system operator to customize the type of notification based on the perceived severity of the alarm. For example, alarms caused by conditions that do not immediately affect the performance of the system (such as low level alarms) may be logged in a productivity report maintained by the system controller, or could trigger a notification message sent through the network gateway to an e-mail address. Other more severe alarms (such as out of product alarms) may be configured to provide a more urgent indication, such as audible indicators (e.g., a buzzer) and/or visual indicators (e.g., a strobe light) at the system controller and/or pump-stand location.
[0020] In a sixth aspect of the invention, the pump controller provides a selectable flush manifold status monitoring feature. To this end, the pump controller includes an electrical input port that is operatively coupleable to one or more sensors in the flush manifold. The sensors (e.g., a flow switch) provide an indication of whether the flush manifold is ready to receive a dispensed chemical product. If the flush manifold is not ready to receive the dispensed chemical (e.g., the flow switch signal indicates that there is insufficient flow of diluent through the flush manifold), the pump controller refrains from activating the pump, and provides local and/or remote alarm notifications indicating the problem encountered.
[0021] In seventh aspect of the invention, the pump includes a pump chamber lid interlock system. The interlock system includes a sensor that provides a signal to the pump controller indicating the position of the pump chamber lid. For example, a magnet located in the pump chamber lid and a Hall Effect sensor located in the pump housing. In response to receiving a signal indicating that the pump chamber lid is open, the pump controller disables the pump. Advantageously, the pump chamber lid interlock system may thereby prevent injuries from pinched fingers and damage to the pump that may result if the pump is activated while a system operator is, for example, replacing a squeeze tube.
[0022] In an eighth aspect of the invention, the pump includes a housing that includes integral input and output channels and a motor having a horizontal orientation. The input end of the squeeze tube is coupled to a product supply line by the integral input channel, and the output end of the squeeze tube is coupled to a product delivery line by the integral output channel. The squeeze tube is thereby isolated by the pump housing from mechanical forces present on the supply lines. The squeeze tube is fluidically coupled to the input and output channels by 90 degree elbows so that the squeeze tube is oriented in a horizontal orientation. The 90 degree elbows are free to pivot inside the integral channels, and thereby allow axial motion at the ends of the squeeze tube. This axial motion is believed to further reduce mechanical stresses on the squeeze tube when the pump rotor is in motion, potentially extending squeeze tube service life. The 90 degree elbows also facilitate removal and replacement of the squeeze tube by allowing the squeeze tube to be in a horizontal position at a high point in the chemical product supply path. Gravity thus urges the chemical product to retreat back into the supply lines when the squeeze tube assembly is removed, reducing the likelihood of a spill.
[0023] The horizontal orientation of the motor facilitates positioning the rotor in a proper relationship with the horizontally oriented squeeze tube, and improves pump packaging. In an embodiment of the invention, the integral input and output channels are located in a back side of the pump housing so that the supply lines are positioned out of the way, and to facilitate use of European industry standard DIN rail system to secure the pumps comprising the pump stand to a vertical surface, such as a wall.
BRIEF DESCRIPTION OF THE DRAWINGS
[0024] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with a general description of the invention given above, and the detailed description given below, serve to explain the invention.
[0025] FIG. 1 is an illustration of an exemplary chemical dispensing system including a system controller, pump-stand, and machine interface.
[0026] FIG. 2 is a schematic diagram of the chemical dispensing system in FIG. 1 illustrating the interconnectivity between the system controller, machine interface, pumps, washing machine, and chemical product containers in an embodiment of the invention where the system controller located with the washing machine.
[0027] FIG. 3 is a schematic diagram of the chemical dispensing system in FIG. 2 with the system controller relocated to the pump-stand.
[0028] FIG. 4 is a schematic illustrating details of the system controller.
[0029] FIG. 5 is a schematic illustrating details of the pump including a pump controller and motor, as well as sensors and indicators associated with operation of the pump controller.
[0030] FIG. 6A is a detailed schematic of a detection circuit shown in FIG. 5 including an oscillator with an input coupled to a probe assembly.
[0031] FIG. 6B is a schematic of the detection circuit in FIG. 6A with a high impedance being provided by the probe assembly showing the oscillator in an oscillating state.
[0032] FIG. 6C is a schematic of the detection circuit in FIG. 6A with an impedance being provided by the probe assembly that causes the oscillator to be in a different state to include a non-oscillating state.
[0033] FIG. 7 is a schematic illustrating additional details of the machine interface presented in FIGS. 1-3 .
[0034] FIG. 8 is an isometric view of the pump illustrating features of the pump housing and pump components.
[0035] FIG. 9 is a cross-sectional diagram of the pump in FIG. 8 illustrating the integral input and output channels.
[0036] FIG. 10 is a top view of the pump illustrating the squeeze tube, rotor, and pump chamber.
[0037] It should be understood that the appended drawings are not necessarily to scale, presenting a somewhat simplified representation of various features illustrative of the basic principles of the invention. The specific design features of the sequence of operations as disclosed herein, including, for example, specific dimensions, orientations, locations, and shapes of various illustrated components, will be determined in part by the particular intended application and use environment. Certain features of the illustrated embodiments have been enlarged or distorted relative to others to facilitate visualization and a clear understanding. In particular, thin features may be thickened, for example, for clarity or illustration.
DETAILED DESCRIPTION OF THE INVENTION
[0038] Embodiments of the invention provide a networked control system for dispensing chemical products in commercial washing machine applications that assists in overcoming the difficulties with contemporary chemical dispensing systems. In an embodiment of the invention, a system controller serves as a master controller and is linked via a plurality of serial data buses the other system nodes. The serial data bus interfaces provide an increased communications capability between the system controller and the system nodes as compared to conventional systems. The serial data buses thereby support adding intelligence to system nodes so that control functions may be distributed among the system nodes rather than concentrated in the system controller. By way of example, each pump controlled by the system includes a pump controller, which enables chemical product dispensing to be controlled locally in each pump based on commands received from the system controller over the serial data bus.
[0039] The serial data bus network allows the system controller to query the operational status of each of the other system components (such as a machine interface or any of a plurality of pump-stands) to determine if the system is ready to dispense chemicals before issuing commands. The serial data bus also provides power to network components so that additional nodes may be added to the network by simply daisy-chaining a new node to an existing node. This allows, for example, an additional pump to be added to an existing group of pumps comprising a pump-stand by merely coupling the new pump to the end of the chain of pumps with a jumper.
[0040] The system controller provides a user interface, stores process formulas, and displays system alarms and status indicators, as well as serving as the master controller for the serial data busses. To dispense chemical products according to a stored formula (e.g., a product dispensing profile for a particular process), the system controller sends data to one or more the pumps indicting the amount of chemical product that the pump stand is required to dispense. The system controller also periodically interrogates the pumps to verify that the pumps are operating properly. To this end, the system controller will typically query the status of a network node before issuing a command. The system controller may thereby obtain positive verification that the node is operating properly before issuing a command. The system controller may also include a serial data port configured to communicate with an optional network gateway. When present, the network gateway provides a data link between the system controller and an outside network, such as the Internet, so that system operators may communicate with one or more system controllers from a remote location.
[0041] To support the serial data bus network, each pump-stand includes a pump controller that provides local control of the pump motor and enables a data link process with the system controller. To this end, the pump controller includes a user selectable address that allows the system controller to address each pump controller individually over the shared serial data bus. The pump controller provides intelligence to the pump that supports more accurate dispensing of chemical product based on stored calibration data, monitoring and reporting of pump status, chemical product level monitoring, control of flush manifold operation (if present), and transmission of alarms to the system controller.
[0042] Referring now to the drawings, FIGS. 1-3 illustrate an exemplary chemical dispensing system 10 shown in two typical deployment configurations with a washing machine 11 , which may be a laundry machine, a ware-wash machine, a healthcare wash, or any other type of machine that uses dispensed chemicals. One of ordinary skill in the art will recognize that this system 10 is only for illustration purposes and that embodiments of the invention may be used with other configurations of the chemical dispensing system 10 . The base configuration of the chemical dispensing system 10 includes a system controller 12 coupled to a plurality of pumps 14 a - 14 c comprising pump-stand 15 by a pump serial data bus 16 . For illustrative purposes, FIGS. 1-3 show a system with 3 pumps 14 a - 14 c . However, it is understood that other numbers of pumps may be used, and the invention is not limited to any specific number of pumps. The pumps 14 a - 14 c each include a pass-through serial data bus connector 18 ( FIG. 5 ) so that the pumps 14 a - 14 c may be connected in a daisy-chain configuration on the pump-stand 15 . Each pump 14 a - 14 c is thereby connected to an adjacent pump by a jumper 22 so that the pumps 14 a - 14 c are each electrically coupled to the pump serial data bus 16 . The pump serial data bus 16 thus includes multiple jumpers 22 and pass-through connectors 18 . In an embodiment of the invention, jumpers 22 may be comprised of a printed circuit board (PCB) encapsulated in plastic to facilitate quick connections between pumps 14 a - 14 c and power supply 20 .
[0043] System power is supplied by a power supply 20 mounted to the pump-stand 15 near one end of the chain of pumps 14 a - 14 c . The power supply 20 may be coupled to the pump serial data bus 16 by connecting the output of the power supply 20 to one end of the pass-though connector 18 in the end pump, shown here as the left most pump 14 a . The power supply 20 is thereby coupled to the pumps 14 a - 14 c and the system controller 12 by the serial data bus 16 . In a preferred embodiment, the pumps 14 a - 14 c , and power supply 20 may be mounted to a DIN rail 28 on the pump stand 15 , although the invention is not so limited, and other mounting locations and methods may be used.
[0044] To obtain data concerning the operational status of the washing machine 11 , the system controller 12 is coupled to a machine interface 24 by a machine interface serial data bus 26 . Typically, the system controller 12 will be located near (or mounted to) the washing machine 11 as shown in FIGS. 1 and 2 , but the system controller 12 may also be located remotely from the washing machine 11 as shown in FIG. 3 . For example, in the alternative embodiment illustrated in FIG. 3 , the system controller 12 is mounted to the DIN rail 24 so that the system controller 12 , pumps 14 a - 14 c and power supply 20 are all affixed to the pump-stand 15 by the DIN rail 28 .
[0045] The pump-stand 15 is configured to provide product to the washing machine 11 from various chemical storage containers 30 , 32 , 34 , each of which is fluidically coupled to one of pumps 14 a - 14 c by a product supply line 36 . Typically, the output of each pump 14 a - 14 c is fluidically coupled to a flush manifold 42 by flush manifold supply lines 44 as shown in FIGS. 1-3 . However, the pumps 14 a - 14 c may also be fluidically coupled directly to the washing machine 11 so that undiluted product is delivered to the machine 11 . In embodiments including the flush manifold 42 , an output of the flush manifold 42 is coupled to the washing machine 11 by a machine supply line 45 , and an input of the flush manifold 42 is coupled to a diluent source 46 by a diluent valve 48 . The diluent valve 48 may be electrically coupled to one or more of the pumps 14 a - 14 c , ( FIG. 5 ) so that the chemical dispensing system 10 can control delivery of product to the washing machine 11 by regulating the flow of diluent through the flush manifold 42 .
[0046] The power supply 20 is typically mounted on the DIN rail 28 next to a pump 14 a - 14 c , although other mounting locations may be used. The power supply 20 is connected to source of AC line voltage (not shown) and provides a DC voltage (such as to 24 VDC) suitable for powering system controller 12 , pumps 14 a - 14 c , and machine interface 24 . When mounted on the DIN rail 28 , the power supply 20 will typically be coupled to either the left side of pass-through connector 18 of rightmost pump 14 a , (as shown); or to the right side of pass-through connector 18 of the leftmost pump 14 c . Power is thereby distributed to the system controller 12 and pumps 14 a - 14 c via the serial data bus 16 . To this end, the serial data bus 16 may include power and ground conductors, as well as one or more data conductors. In an embodiment of the invention, the pump serial data bus 16 includes a power conductor, a ground conductor, a positive data conductor, and a negative data conductor. The data conductors thereby form a balanced, or differential, serial data transmission line. The system controller 12 , in turn provides power to the machine interface 24 over the machine interface serial data bus 26 , which is typically configured to have the same conductor layout as the pump serial data bus 16 . Advantageously, the pass-through connectors 18 and pump serial data bus configuration make adding additional pumps to the pump-stand 15 a simple process, thereby facilitating the addition of additional chemical products to the chemical dispensing system 10 .
[0047] Some embodiments of the invention may also include probe assemblies 50 operatively disposed in containers 30 , 32 , 34 . The probe assemblies 50 , in turn, may be electrically coupled to a detection circuit 52 ( FIG. 5 ) in the pump 14 a - 14 c that dispenses product from the container 30 , 32 , 34 in which the probe assembly 50 is located. Probe assemblies 50 may be configured to provide a signal to the detection circuit 52 indicative of the level of product in the container 30 , 32 , 34 so that the pumps 14 a - 14 c may monitor product levels in their associated containers 30 , 32 , 34 . Probe assemblies 50 are known in the art and typically include one or more conductive probes that present different impedances to the detection circuit 50 depending on whether the probe assembly 50 is in contact with product. Suitable probe assembles and detection circuits are described in U.S. patent application Ser. No. 13/164,878, entitled “System and Method for Product Level Monitoring in a Chemical Dispensing System”, Attorney Docket No. NOVC-23, the disclosure of which is incorporated herein by reference in its entirety.
[0048] Referring now to FIG. 4 and in accordance with an embodiment of the invention, the system controller 12 includes a processor 54 , memory 56 , an input/output (I/O) interface 58 , a user interface 60 , a system controller voltage supply circuit 62 , and a machine interface power supply output circuit 64 . The I/O interface 58 is communicatively coupled to the processor 54 and employs a suitable communication protocol for communicating with the serial data busses, and. The processor 54 may thereby communicate through the I/O interface 58 to the machine interface 24 via the machine interface serial data bus 26 , the pumps 14 a - 14 c (shown as a single pump for purposes of illustration) through pump serial data bus 16 , and a network gateway 68 via a network gateway serial data bus 70 . The system controller 12 may also include one or more additional serial data bus interfaces 72 to accommodate future system expansion. The serial buses may be connected to the I/O interface 58 (as well as the various network nodes) though serial bus interfaces, each of which includes a suitable multi-pin connector 74 .
[0049] Processor 54 may be a microprocessor, microcontroller, programmable logic or any other suitable device that manipulates signals based on operational instructions, which may be stored in memory 56 . The memory 56 may be a single memory device or a plurality of memory devices including but not limited to read-only memory (ROM), random access memory (RAM), volatile memory, non-volatile memory, static random access memory (SRAM), dynamic random access memory (DRAM), flash memory, cache memory, and/or any other device capable of storing digital information. The memory 56 may also be integrated with the processor 54 .
[0050] The processor 54 executes or otherwise relies upon computer program code, instructions, or logic (collectively referred to as program code) to execute the functions of the system controller 12 . To this end, a system controller application 66 may reside in memory 56 and may be executed by the processor 54 . The system controller application 66 controls and manages the chemical dispensing system 10 by communicating with other system components via the I/O interface 58 and serial data buses 16 , 26 , 70 . The system controller application 66 may thereby obtain information regarding the operational status of the washing machine 11 from the machine interface 24 , and in response, causes the pumps 14 a - 14 c to dispense chemicals in a controlled way.
[0051] The user interface 60 may be operatively coupled to the processor 54 of the system controller 12 in a known manner. The user interface 60 includes output devices, such as alphanumeric displays, one or more touch screens, light emitting diodes (LEDs), acoustic transducers, and/or any other suitable visual and/or audio indicators; and input devices and controls, such as the aforementioned touch screen, an alphanumeric keyboard, a pointing device, keypads, pushbuttons, control knobs, etc., capable of accepting commands or input from the system operator and transmitting the entered input to the processor 54 . The user interface 60 thereby provides a mechanism by which the system operator may enter new washing process formulas, set and/or deactivate alarms, update calibration data, retrieve and view system data (such as amounts of product dispensed and number and type of wash loads run) and otherwise operate and manage the chemical dispensing system 10 .
[0052] The system controller voltage supply 62 receives power from the power supply 20 via the pump serial data bus 16 . The system controller voltage supply may contain circuits, such as voltage regulators, that condition and adjust the voltage received from the power supply 20 , thereby providing suitable voltages for running the processor 54 and other system controller components. The machine interface power supply output circuit 64 may receive power from the system controller voltage supply 62 , or directly from the power supply 20 via the pump serial data bus 16 . The machine interface power supply circuit 64 may condition the power before transmitting it to the machine interface 24 ; or the machine interface power supply circuit 64 may merely pass the power received from the power supply 20 on to the machine interface 24 over the machine interface serial data bus 26 without significant alteration.
[0053] The network gateway 68 may be a computer equipped to provide an interface between the system controller 12 and an external network 76 , such as the Internet. To this end, the network gateway 68 may include a network gateway application running on a processor that performs protocol translation, converts data rates, and/or provides any other functions necessary to provide interoperability between the chemical dispensing system and the external network. The network gateway 68 may thereby allow computers or other communication devices that are attached to the external network 76 to communicate with the system controller 12 so that system operators may remotely control and monitor the chemical dispensing system 10 . The network gateway 68 may also be configured to address multiple system controllers 12 over a single network gateway serial data bus 70 .
[0054] Referring now to FIGS. 5 and 6 A- 6 C, each pump 14 a - 14 c includes a pump controller 78 in communication with a motor 80 . The pump controller 78 may also be in communication with the detection circuit 52 , internal and external temperature sensors 82 , 84 , a plurality of status indicator LEDs 86 , a local alarm buzzer 88 , a mute switch 90 , a flow sensor 96 , a pump chamber lid sensor 98 , address selector switch 99 , pump prime switch 101 , and a valve driver circuit 103 . The pump controller 78 may also include a pump controller voltage supply 105 that provides suitable voltage levels for running the controller components. The motor 80 may be a brushless direct current (BLDC) electric motor coupled to a rotor 100 by a transmission 102 . The rotor 100 includes one or more rollers 104 and is positioned in a pump chamber 106 with a squeeze tube 108 . The rotor 100 , pump chamber 106 , and squeeze tube 108 are further configured so that when torque is applied to the rotor 100 by the motor 80 , the rotor 100 rotates in such a way that the rollers 104 compress the squeeze tube 108 against a side wall of the pump chamber 106 in a progressive fashion that causes fluid to be urged through the squeeze tube 108 .
[0055] So that the pump 14 a - 14 c may dispense product, one end of the squeeze tube 108 is coupled to an integral input channel 110 , and the other end of the squeeze tube 108 is coupled to an integral output channel 112 . The integral input and output channels 110 , 112 are in turn fluidically coupled to the product supply and flush manifold supply lines 36 , 44 , respectively. Activating the motor 80 thereby causes fluid to be drawn into the squeeze tube 108 from the product supply line 36 via the integral input channel 110 and expelled into the flush manifold supply line 44 via the integral output channel 112 . Product may thereby be conveyed from the product container 30 , 32 , 34 to the flush manifold 42 by pumps 14 a - 14 c.
[0056] Similarly as described with respect to the system controller 12 , the pump controller 78 includes a processor 114 , memory 116 , and an I/O interface 118 that provides a communications link between the pump controller processor 114 and the pump serial data bus 16 via the pass-through connector 18 . The pump controller processor 114 may be further operatively coupled to detection circuit 52 , motor 80 , internal and external temperature sensors 82 , 84 , status indicator LEDs 86 , local alarm buzzer 88 , mute switch 90 , flush manifold flow sensor 96 , pump chamber lid sensor 98 , address selector switch 99 , pump prime switch 101 , and valve driver circuit 103 .
[0057] Memory 116 may contain a pump controller application 120 comprised of program code that, when executed by the processor 114 , causes the pump controller 78 to provide local motor control and support a data link process that allows the system controller 12 and pump controller 78 to communicate over the pump serial data bus 16 . The address selector switch 99 may be any suitable switch, such as a rotational selector switch or dip switch that is accessible from the outside of the pump 14 a - 14 c . Advantageously, the address selector switch 99 thereby provides a quick and easy means to visually identify the current address of each pump controller 78 in the network.
[0058] Each pump controller 78 that is sharing the pump serial data bus 16 has a unique address that is set on the address selector switch 99 prior to applying power to the pumps 14 a - 14 c . The pump controller application 120 reads the address selector switch at power up and loads the network address into memory 116 . Once the pump controller application 120 has loaded the network address into memory, the network address will remain fixed so long as the pump controller 78 is under power. Advantageously, this feature reduces the risk of the pump controller's network address being changed inadvertently while the system 10 is in operation, which could result in more than one pump controller 78 having the same network address. To change the network address of the pump controller 78 , the system operator must power down the pump stand 15 , change the configuration of the address selector switch 99 , and reapply power so that the new address is loaded by the pump controller application 120 .
[0059] The pump prime switch 101 , when enabled, provides an automated pump priming function. To prevent inadvertent activation of the priming function, the operation of the pump prime switch 101 may have to be enabled in the system controller 12 through a password protected menu accessed through the system controller user interface 60 . Enabling the pump prime function in the system controller 12 causes the system controller application 66 to set a priming feature enable flag in the pump controller 78 . In response to sensing that the pump prime switch 101 has been activated, the pump controller application 120 checks the priming feature enable flag. If the flag is set, the pump controller application 120 activates the motor 80 for a sufficient amount of time to ensure that the supply lines 36 , 44 and pump 14 a - 14 c are primed with product. In contrast, if the feature enable flag is not set, the pump controller application 120 may simply ignore the state of the pump prime switch 101 .
[0060] The pump chamber lid sensor 98 provides a signal indicative of the position of a pump chamber lid 178 ( FIG. 9 ) to the processor 114 . To this end, the lid sensor 98 may include a magnet 122 and a Hall Effect sensor 124 configured to provide a first signal to the processor 114 when the lid 178 is in an open position, and a second signal to the processor 114 when the lid 178 is in a closed position. To reduce the risk of damage to the pump 14 a - 14 c as well as injury to the system operator, the pump controller application 120 checks the pump chamber lid sensor signal before activating the motor 80 . If the signal indicates that the pump chamber lid 178 is in a closed position, the pump controller application 120 will activate the motor in the normal manner. However, in response to a signal indicating that the pump chamber lid 178 is in an open position, the pump controller application 120 may disable the motor 80 as well as provide an indication to the system controller 12 that the motor 80 is not in a condition to be activated.
[0061] The detection circuit 52 supports a low level detection feature, which may be enabled in the pump controller application 120 by activating the feature through the system controller user interface 60 . The detection circuit 52 includes in input port coupleable to the probe assembly 50 through a probe assembly connector 126 , which may be located on the bottom of the pump 14 a - 14 c . The detection circuit 52 includes a low frequency oscillator that includes an active element, or oscillator 128 ( FIGS. 6A-6C ) and a load element 130 . The oscillator 128 may include a CMOS inverter or any other suitable device capable of producing an oscillation when coupled to load element 130 . Load element 130 may be a resistor-capacitor (RC) circuit or some other suitable circuit that provides a suitable load or feedback to the oscillator 128 to cause the oscillator 128 to oscillate. The detection circuit 52 produces an oscillation when a high impedance electrical load is present on the input to the probe assembly connector 126 , such as an electrical load with an impedance greater than 5 megohms. The detection circuit 52 thereby provides a low frequency oscillation signal when the quality factor of the oscillator 128 is sufficiently unaltered by the electrical load from a probe assembly 50 that is not in contact with a monitored product. When an electrical load that has a high impedance is coupled to the input 126 , the oscillator 128 comprising detection circuit 52 is tuned to oscillate at a nominal operating frequency, such as about 10 Hz, for example. The pump controller application 120 may thereby determine if there is sufficient product remaining to contact the probe assembly 50 by monitoring the output of the detection circuit 52 for an oscillation.
[0062] A pair of conductive probes 132 , 134 comprising the probe assembly 50 may be connected to the detection circuit 52 . The probe assembly 50 is connected across the input 126 of the detection circuit 52 so that one probe 132 is connected to one side of load element 130 and the other probe 134 is connected to the other side of load element 132 , which may also be coupled to a reference ground 136 . When the probe assembly 50 is suspended in air, such as when the product in the monitored container 30 , 32 , 34 has dropped below the probe assembly 50 , the impedance of the probe assembly 50 as seen by the detection circuit 52 has a low loading effect on the oscillator 128 . The quality factor of the oscillator 128 is thus relatively unaffected by the presence of the probe assembly 50 so that the detection circuit 52 outputs a time varying voltage signal at the nominal frequency as illustrated in the schematic diagram of FIG. 6B .
[0063] However, when one or both of the probes 132 , 134 are in contact with a conductive solution, an impedance 138 from the probes 132 , 134 is seen by the detection circuit 52 . A typical impedance between the probes 132 , 134 when in contact with product will be between 10 kilohms and 1 megohms. The impedance 138 will lower the quality factor of the oscillator 128 , which changes the operating parameters of the oscillator 128 due to the parallel loading effect of the probe assembly 50 . These changed parameters will cause the oscillator 128 to oscillate at a frequency different from the nominal frequency or to cease oscillating depending on the load presented by the probe assembly 50 , as illustrated in the schematic diagram of FIG. 6C . Thus, in response to being coupled to a probe assembly 50 that is in contact with product, the detection circuit 52 will output a signal having a different frequency or that stops varying altogether, such a constant voltage at ground potential. This change in the output of the detection circuit 52 thereby provides an indication to the processor 114 of the presence or absence of product at the probe assembly 50 .
[0064] The status indicator LED's 86 may include a first LED that provides a visual indication that the pump 14 a - 14 c is powered, a second LED that provides an indication of the presence of data traffic on the pump serial data bus 16 , a third LED to indicate if a local error is active, and a fourth alarm LED that provides an indication of the level of product detected by the pump controller application 120 . The power and data traffic status indicator LEDs may be coupled to and activated by the processor 114 , or may be directly tied to a pump power supply and/or data lines as the case may be. The alarm LED may be used to indicate a variety of conditions. By way of example, the pump controller application 120 may cause the alarm LED to flash when a probe assembly 50 is coupled to the detection circuit and the product level feature is active to provide an indication of such to the system operator. In response to detecting a low product condition, the pump controller application 120 may cause the alarm LED to be illuminated continuously so that the system operator is provided with a visual indication of the low product level condition.
[0065] The pump controller application 120 may also be configured to activate the local alarm buzzer 88 in response to detecting a low product level condition. The system operator may cause the pump controller application 120 to silence the alarm buzzer 88 by pressing mute switch 90 . In some embodiments, the pump controller application 120 may send an alarm message to the system controller 12 in response to a status query so that the system controller 12 may activate an alarm or otherwise report to the system operator that an alarm condition exists at the pump-stand 15 . The pump controller application 120 may be configured to provide different mute responses depending on how long or how many times the mute switch 90 is activated. By way of example, in some embodiments of the invention, the first time the mute switch 90 is pressed, the alarm might be silenced for a short period, such as an hour. If the mute switch 90 is held down for a length of time, such as 3-4 seconds, the alarm might be silenced for a longer period, such as a weekend. To provide an indication that the local alarm buzzer 88 has been muted, the local alarm LED may be made to flash at a slower rate than normal. The rate of flashing may be further adjusted so that the local alarm LED flashes at a slower rate when a long duration alarm silencing period has been activated (such as a weekend) than when a short duration silencing period has been activated (such as an hour).
[0066] The pump-stand 15 may be configured to deliver product directly to the washing machine 11 , or the product may be dispensed into the flush manifold 42 and delivered to the machine 11 by a diluent, which is the configuration illustrated in FIGS. 1 - 3 . When the pump-stand 15 is deployed with flush manifold 42 , a flush-flow control feature may be activated in the pump controller application 120 of at least one of the pumps 14 a - 14 c associated with the system controller 12 . As with the previous optional features, the flush-flow feature is activated in the pump controller application 120 through the user interface 60 of the system controller 12 . Typically, the flush flow feature is only activated in one pump 14 a - 14 c per pump-stand 15 , with the system controller 12 controlling the flush manifold 42 by addressing flush manifold related commands to the pump controller 78 that is coupled to the diluent valve 48 . In order to provide sufficient drive current and voltages to the diluent valve 48 , the processor 114 may be coupled to the diluent valve 48 by a valve circuit driver 103 . In cases where the valve circuit driver 103 is not coupled to the diluent valve 48 , the valve circuit driver output port 140 may be used to provide a switched voltage output, such as a 24 VDC switched output, for activating external alarms or other uses.
[0067] The pump controller application 120 may also monitor the flow sensor 96 , which provides a signal indicative of the rate that diluent is flowing through the flush manifold 42 . The pump controller application 120 may thereby make determinations concerning the dispensing of product into the flush manifold 42 based on whether there is sufficient diluent flow to deliver the product to the washing machine 11 . The pump controller application 120 may also report alarm conditions to the system controller 12 if the detected diluent flow rate deviates from an acceptable level.
[0068] Referring now to FIG. 7 , the machine interface 24 includes a processor 142 that is operatively coupled to a memory 144 , an I/O interface 146 , a trigger signal interface 148 , and a display 150 . A machine interface voltage supply 152 is coupled to and receives power from the machine interface serial data bus 26 , and includes voltage regulation circuits that provide suitable voltages to the circuits comprising the machine interface 24 . The trigger signal interface 148 is coupled to trigger signals in the washing machine 11 by optical isolators 154 a - 154 n , which provide galvanic isolation between the high voltage triggers in the washing machine 11 and the other chemical dispensing system components. In an embodiment of the invention, there may be 10 trigger signals, with each signal being coupled to the trigger signal interface by an optical isolator 154 a - 154 n.
[0069] Memory 144 may contain a machine interface application 156 comprised of program code that, when executed by the processor 142 , causes the machine interface 24 to determine the operational state of the washing machine 11 based on machine trigger signals detected by the processor 142 via the trigger signal interface 148 . The machine interface application 152 may also handle the networking and messaging functions required to communicate with the system controller 12 over the machine interface serial data bus 26 . To this end, the I/O interface 146 may employ a suitable communication protocol for communicating over the machine interface serial data bus 26 . In an embodiment of the invention, the machine interface 24 is configured as a slave module, and will only respond back to the system controller 12 in response to being queried by the system controller 12 .
[0070] The trigger signal interface 148 works cooperatively with optical isolators 154 a - 154 n to convert the local high voltage trigger signals received from the washing machine 11 into signals suitable for coupling to the processor 144 . The machine interface application 156 determines the state of the washing machine 11 based on the detected trigger signals, and may store time stamped trigger signals in memory 144 for later use and reporting. In response to a query from the system controller 12 , the machine interface application 152 communicates the determined state of the machine 11 and/or detected triggers to the system controller application 66 . In response to the washing machine state (e.g., beginning wash cycle), the system controller application 66 may, in turn, cause the pump controller application 120 to dispense product to the washing machine 11 (e.g., dispense 100 milliliters of detergent). The machine interface display 150 may include an electronic membrane overlay having LEDs that are illuminated by the machine interface application 156 to indicate the particular triggers that have been detected and qualified. The display 150 may also include an additional LED that is illuminated to indicate the presence of data traffic on the machine interface serial data bus.
[0071] With reference to FIGS. 8-10 , in which like reference numerals refer to like features in FIGS. 1-7 and in accordance with an embodiment of the invention, the representative pump 14 a - 14 c includes a housing 158 having a pump chamber 106 , an integral input channel 110 , and an integral output channel 112 . The rotor 100 and squeeze tube 108 are positioned in the pump chamber 106 , and the rotor 100 includes rollers 104 configured to compress the squeeze tube 108 against a sidewall 160 of the pump chamber 106 . The squeeze tube 108 has a first end coupled to the integral input channel 110 by an inlet fitting 162 and a second end coupled to the integral output channel 112 by an outlet fitting 164 . The inlet and outlet fittings 162 , 164 include a 90 degree elbow so that the squeeze tube 108 is oriented in a plane perpendicular to the integral input and output channels 110 , 112 . Each fitting 162 , 164 includes upper and lower o-rings 166 , 168 that provide a fluid-tight seal between the fitting 162 , 164 and its respective integral channel 110 , 112 . Advantageously, the o-rings 162 , 164 allow the fittings 162 , 164 to pivot axially, which may reduce lateral bending forces on the squeeze tube 108 at the squeeze tube/fitting connection points.
[0072] The pump controller 78 and associated circuits are mounted in a lower cavity 170 near the bottom of the pump housing 158 to facilitate access to the various electrical connectors associated with the pump controller 78 . The pump motor 80 and transmission 102 are stacked vertically in a central cavity 172 , so that the motor 80 has a horizontal orientation. The transmission 102 may provide speed and torque conversion between the motor 80 and rotor 100 so that the rotor rotates at a desirable speed. In an alternative embodiment of the invention, the transmission 102 may be omitted and the motor 80 directly coupled to the rotor 100 . The motor 80 may be a brushless DC motor, and may include an integrated motor controller (not shown) that provides signals indicative of the motor speed in rotations per minute to the pump controller processor 114 . Advantageously, the integrated motor controller thereby allows the pump controller application 120 to determine and report motor status (such as a locked rotor condition) as well as precisely measure product volume dispensing by tracking the speed and/or number of rotations of the rotor 100 .
[0073] The product and flush manifold supply lines 36 , 44 are coupled to the integral input and output channels 110 , 112 by plastic inserts 174 , 176 , respectively. Plastic inserts 174 and 176 may include a threaded upper end configured to engage the lower ends of the integral input and output channels 110 , 112 . The plastic inserts 174 , 176 each include a barbed lower end that provides a fluid tight seal when coupled to the product and flush manifold supply lines 36 , 44 . In an embodiment of the invention, the plastic inserts 174 , 176 may be comprised of a conductive plastic, such as carbon impregnated polypropylene. In this alternative embodiment, the conductive plastic inserts 174 , 176 may be electrically coupled to the detection circuit 52 and thereby serve as integrated conductive probes 132 , 134 that provide an out-of-product indication to the detection circuit 52 .
[0074] The pump chamber lid 178 may be comprised of transparent plastic that allows system operators to view the operation of rotor 100 and squeeze tube 108 . The magnet 122 is positioned within the pump chamber lid 178 so that when the lid 178 is closed, the magnet 122 causes the Hall Effect sensor 124 to change its output, indicating to the pump controller application 120 that the pump chamber lid 178 is in a closed position. When the pump chamber lid 178 is opened, the change the magnetic field in the region of the Hall Effect sensor 124 causes the Hall Effect sensor to provide a signal to the pump controller application 120 that indicates the lid 178 is not closed. In response, the pump controller application 120 may disable the motor 80 to reduce the risk of injury to system operators and/or damage to the squeeze tube 108 from fingers or other objects becoming entangled with the rotor 100 .
[0075] In operation, the system controller 12 may be configured as a master, and the machine interface 24 and pump controllers 78 configured as slaves. Using this master/slave configuration, the machine interface 24 and pump controllers 78 only communicate with the system controller 12 in response to a query or other message from the system controller 12 . This master/slave arrangement thus ensures that only one system node transmits data over their associated serial data bus at a time. Process formulas are programmed into the system controller 12 over the user interface 60 , and the system operator selects which chemical dispensing process formula the system controller 12 will implement based on the type of load the washing machine 11 is processing. The system controller 12 is thus the master controller in the network and handles all of the process formulas and any required mathematical calculations, as well as providing a human-machine interface to the chemical dispensing system 10 .
[0076] Operations in the chemical dispensing system 10 are initiated by the system controller 12 querying the status of the machine interface 24 . To this end, the system controller application 66 sends a status query message to the machine interface 24 over the machine interface data bus 26 . The machine interface application 156 responds to the status query message with a status update that includes data regarding any qualified triggers that have been logged by the machine interface 24 since the last query message the system controller 12 . In response to the content of the machine controller response message, the system controller application 66 determines the state of the washing machine 11 . Based on the state of the washing machine 11 and the process formula selected by the system operator, the system controller application 66 further determines which product, if any, needs to be dispensed as well as how much of the product should be dispensed. All pump operations are thus ultimately dependent on the qualified triggers, which are processed locally by the machine interface 24 and sent to the system controller 12 by the machine interface 24 when prompted.
[0077] If the washing machine 11 is in a state requiring product to be dispensed (e.g., beginning a wash load), the system controller application 66 queries the status of the pump 14 a - 14 c associated with the container 30 , 32 , 34 holding the product to be dispensed. To this end, the system controller application 66 sends a query message addressed to the pump controller 78 associated with the product to be dispensed over the pump serial data bus 16 . The pump controller application 120 responds to the query message by reporting back pump status, including any out of product or other system alarms, which (if present) are displayed by the system controller 12 .
[0078] If the pump controller application 120 response indicates that the pump 14 a - 14 c is ready to dispense product, the system controller application 66 will determine the amount of product that is to be dispensed, and communicate this to the pump controller application 120 . Advantageously, by sending data to the pump 14 a - 14 c that allows the pump controller 78 to determine a required run time rather than merely a pump OFF/ON command (as is conventional), the system 10 ensures that the motor 80 will not run continuously if the system controller 12 loses communication with the pump controller 78 after the motor 80 has been activated.
[0079] In response to receiving the dispense product message from the system controller 12 , the pump controller application 120 checks the pump status to verify that the pump 14 a - 14 c is ready to dispense product (i.e., there are no active alarms that would preclude dispensing product), and activate the motor 80 for an amount of time or number of rotations calculated to dispense the required amount of product. The pump controller 78 may accumulate the total motor activation time and/or number of rotations (collectively referred to as an activation period) and store this value in memory 116 . The accumulated activation period value may be used in estimating remaining squeeze tube service life and/or a deterioration in pump flow rate due to wear on the squeeze tube 108 . The pump controller application 120 may also open the diluent valve 48 (when present) for an amount of time sufficient to flush the product into the washing machine 11 , and may monitor the flow sensor 96 to ensure that sufficient diluent flow is present. In response to the pump controller application 120 determining that the required amount of product has been delivered to the washing machine 11 , the application 120 notifies the system controller 12 that the dispensing operation is complete. If the pump controller application 120 determines that the required amount of product was not delivered to the washing machine 11 , the application 120 may send an alarm or other error message to the system controller 12 so that the system controller 12 can notify the system operator.
[0080] To increase the reliability of communications over the serial data bus network, the system controller 12 may make several attempts to deliver data packets to the system nodes if no response is received to earlier transmissions. The machine interface and pump serial data bus protocols may include both acknowledge (ACK) and negative-acknowledge (NACK) response messages to fully validate system node operation, and may also include cyclic redundancy checking (CRC) to further ensure data robustness.
[0081] The system controller 12 may periodically interrogate the pumps 14 a - 14 c to monitor the performance of the motor 80 , squeeze tube 108 , and any other system errors or alarms. By way of example, the pump controller 78 may track the amount of pump activation time and/or number of rotations to which the squeeze tube 108 has been subjected and use this data to estimate the remaining service life of the squeeze tube 78 . The system controller 12 may obtain operational data from the pump controller 78 regarding the estimated remaining squeeze tube service life and display this data in a squeeze tube life menu over the user interface 60 . The system controller 12 may also include a menu selection that allows the system operator to reset the percentage of life remaining statistic for an individual pump 14 a - 14 c when that pump's squeeze tube 108 is replaced. The system controller 12 may also generate system maintenance alerts or alarms based on this squeeze tube percentage of life remaining exceeding a lower threshold (e.g., below 5%), which may be settable by the system operator. Advantageously, by closely monitoring the percentage of life remaining, the system controller 12 and/or pump controller 78 may adjust the run time of the motor 80 to compensate for reductions in the volume of product dispensed due to tube wear. More advantageously, by actively monitoring squeeze tube life, the replacement schedules for squeeze tubes 108 may be extended while simultaneously reducing the risk of squeeze tube failure, thereby reducing overall system maintenance costs.
[0082] While the present invention has been illustrated by a description of one or more embodiments thereof and while these embodiments have been described in considerable detail, they are not intended to restrict or in any way limit the scope of the appended claims to such detail. Additional advantages and modifications will readily appear to those skilled in the art. For example, as is understood by a person having ordinary skill in the art, the various functions and methods described herein may be distributed between the system, pump, and machine interface controllers in various ways and combinations, so that any controller in the system may perform functions currently ascribed to another controller. The invention in its broader aspects is therefore not limited to the specific details, representative apparatus and method, and illustrative examples shown and described. Accordingly, departures may be made from such details without departing from the scope of the general inventive concept.
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System and method for dispensing product to a washing machine. A chemical dispensing system includes a system controller, machine interface, and pump controller that communicate through serial data buses. The system controller provides a user interface, retrieves washing machine status information from the machine interface, and issues product dispensing commands to the pump controller. The pump controller monitors pump status and dispenses product in response to commands from the system controller. The pump controller: (1) determines pump activation periods based on calibration data stored in a pump controller memory; (2) tracks pump usage and adjusts the activation period to compensate for pump wear as the pump ages; (3) disables the pump if conditions exists that preclude operating the pump; (4) monitors product levels, and (5) reports pump status to the system controller. Integral channels are included in the pump housing to provide stress relief to a squeeze tube.
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This application is related to the commonly assigned applications: "Ink-jet Printing System with Off-Axis Ink Supply and High Performance Tubing," Ser. No. 08/706,061 now abandoned, "Compliant Ink Interconnect Between Print Cartridge and Carriage", Ser. No. 08/706,045 filed on Aug. 30, 1996, and "Fluidic Delivery System with Tubing and Manifolding for an Off-Axis Printing System," Ser. No. 08/706,060 filed on Aug. 30, 1996, the entire contents of which are herein incorporated by reference.
TECHNICAL FIELD OF THE INVENTION
This invention relates to ink-jet printers, and more particularly to a printing system employing off-carriage ink supplies connected to a carriage mounted pen via tubing and manifolding and still more particularly to an off-carriage ink supply system employing high performance tubing.
BACKGROUND OF THE INVENTION
Thermal inkjet hardcopy devices such as printers, graphics plotters, facsimile machines and copiers have gained wide acceptance. These hardcopy devices are described by W.J. Lloyd and H.T. Taub in "Ink Jet Devices," Chapter 13 of Output Hardcopy Devices (Ed. R.C. Durbeck and S. Sherr, San Diego: Academic Press, 1988) and U.S. Pat. Nos. 4,490,728 and 4,313,684. The basics of this technology are further disclosed in various articles in several editions of the Hewlett-Packard Journal [Vol. 36, No. 5 (May 1985), Vol. 39, No. 4 (August 1988), Vol. 39, No. 5 (October 1988), Vol. 43, No. 4 (August 1992), Vol. 43, No. 6 (December 1992) and Vol. 45, No. 1 (February 1994)], incorporated herein by reference. Inkjet hardcopy devices produce high quality print, are compact and portable, and print quickly and quietly because only ink strikes the paper.
An inkjet printer forms a printed image by printing a pattern of individual dots at particular locations of an array defined for the printing medium. The locations are conveniently visualized as being small dots in a rectilinear array. The locations are sometimes "dot locations", "dot positions", or pixels". Thus, the printing operation can be viewed as the filling of a pattern of dot locations with dots of ink.
Inkjet hardcopy devices print dots by ejecting very small drops of ink onto the print medium and typically include a movable carriage that supports one or more printheads each having ink ejecting nozzles. The carriage traverses over the surface of the print medium, and the nozzles are controlled to eject drops of ink at appropriate times pursuant to command of a microcomputer or other controller, wherein the timing of the application of the ink drops is intended to correspond to the pattern of pixels of the image being printed.
The typical inkjet printhead (i.e., the silicon substrate, structures built on the substrate, and connections to the substrate) uses liquid ink (i.e., dissolved colorants or pigments dispersed in a solvent). It has an array of precisely formed orifices or nozzles attached to a printhead substrate that incorporates an array of ink ejection chambers which receive liquid ink from the ink reservoir. Each chamber is located opposite the nozzle so ink can collect between it and the nozzle. The ejection of ink droplets is typically under the control of a microprocessor, the signals of which are conveyed by electrical traces to the resistor elements. When electric printing pulses heat the inkjet firing chamber resistor, a small portion of the ink next to it vaporizes and ejects a drop of ink from the printhead. Properly arranged nozzles form a dot matrix pattern. Properly sequencing the operation of each nozzle causes characters or images to be printed upon the paper as the printhead moves past the paper.
The ink cartridge containing the nozzles is moved repeatedly across the width of the medium to be printed upon. At each of a designated number of increments of this movement across the medium, each of the nozzles is caused either to eject ink or to refrain from ejecting ink according to the program output of the controlling microprocessor. Each completed movement across the medium can print a swath approximately as wide as the number of nozzles arranged in a column of the ink cartridge multiplied times the distance between nozzle centers. After each such completed movement or swath the medium is moved forward the width of the swath, and the ink cartridge begins the next swath. By proper selection and timing of the signals, the desired print is obtained on the medium.
Color inkjet hardcopy devices commonly employ a plurality of print cartridges, usually either two or four, mounted in the printer carriage to produce a full spectrum of colors. In a printer with four cartridges, each print cartridge contains a different color ink, with the commonly used base colors being cyan, magenta, yellow, and black. In a printer with two cartridges, one cartridge usually contains black ink with the other cartridge being a tri-compartment cartridge containing the base color cyan, magenta and yellow inks. The base colors are produced on the media by depositing a drop of the required color onto a dot location, while secondary or shaded colors are formed by depositing multiple drops of different base color inks onto the same dot location, with the overprinting of two or more base colors producing the secondary colors according to well established optical principles.
For many applications, such as personal computer printers and fax machines, the ink reservoir has been incorporated into the pen body such that when the pen runs out of ink, the entire pen, including the printhead, is replaced.
However, for other hardcopy applications, such as large format plotting of engineering drawings, color posters and the like, there is a requirement for the use of much larger volumes of ink than can be contained within the replaceable pens. Therefore, various off-board ink reservoir systems have been developed recently which provide an external stationary ink supply connected to the scanning cartridge via a tube. The external ink supply is typically known as an "off-axis," "off-board," or "off-carriage" ink supply. While providing increased ink capacity, these off-carriage systems also present a number of problems. The space requirements for the off-carriage reservoirs and tubing impact the size of the printer, with consequent cost increase. Moreover, pressure drops through the tubing can reduce printer throughput and affect printing quality. Another problem is that of vapor losses from the tubing and air diffusion into the tubing system. In the past, tubing such as LDPE (low density polyethylene) has been used, since it is a low modulus material which is easy to bend. This low modulus material suffers from relatively high vapor losses out of the tube and air diffusion into the tube. As a result of the vapor losses, the ink can change properties, degrading print quality and eventually causing tube or printhead clogging. As a result of air ingestion, the printhead can fill with air. During thermal fluctuations, the air can expand, causing printhead drool. In addition, the air can cause printhead starvation. Further problems include the force exerted on the carriage by the tubing, and the stresses on the tubing that tends to cause buckling or fatigue failures. These problems are exacerbated with a low end off-carriage printing system with its relatively small form factor.
It would therefore be an advantage to provide a compact, low end off-carriage printing system.
It would further be advantageous to provide such a printing system which permits high throughput printing, with relatively high flow rates through the tubing.
Still other advantages would be provided by an off-carriage printing system with high reliability due to low vapor losses and air diffusion, yet with minimal tubing pressure drops while minimizing the force exerted by the tubing on the carriage to maintain accurate printhead alignment.
SUMMARY OF THE INVENTION
An off-carriage printing system with high performance tubing is described. The printing system includes a media transporting system for transporting a print medium along a medium path to a print area, a scanning carriage for holding a printing structure including a printhead, and a scanning apparatus for scanning the carriage along a scanning axis transverse to the media path at the print area. The system further includes a fixed off-carriage ink supply station including an ink reservoir. A fluid conduit for the flow of ink, interconnects between the ink reservoir of the fixed ink supply station and the printing structure, the fluid conduit including a length of hollow flexible multiple layer tubing routed such that a flexible loop is formed therein. The multiple layer tubing comprises at least one inner barrier layer to water vapor transmission from the ink, at least one barrier layer to oxygen permeability, and at least one outer barrier layer to water vapor transmission from the atmosphere.
BRIEF DESCRIPTION OF THE DRAWING
These and other features and advantages of the present invention will become more apparent from the following detailed description of an exemplary embodiment thereof, as illustrated in the accompanying drawings, in which:
FIG. 1 is a graph showing results of characterization efforts of flow rates as a function of tube diameter for exemplary 3 centipoise ink.
FIG. 2 is a simplified schematic diagram of a printer cartridge connected via a length of tubing to an off-carriage ink reservoir represented as a flaccid bag, with an air bubble in the tubing to illustrate an air diffusion problem addressed by an aspect of the invention.
FIG. 3 is a cross-sectional view of the fluid conduit of the present invention.
FIG. 4 is a perspective view of a color ink-jet printer embodying the invention, with its cover removed.
FIG. 5 is a simplified, partial top view of the printer of FIG. 4, showing a routing of the ink supply tubes from the off-carriage ink reservoirs to the carriage-mounted ink cartridges.
FIG. 6 is a cross-sectional view of a fluid conduit set of the printing system of FIG. 4, taken along line 6--6 of FIG. 4.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
An exemplary application for this invention is in an off-carriage ink delivery system for either a low end printing system or a large format printer. In the exemplary system, a scanning carriage moves a print head that fires ink drops in a dot matrix pattern onto a paper or other print medium. The print head is in fluid communication with a replaceable ink supply which is releasably mounted in a fixed ink supply station. Objectives of this system include the following:
(1) to provide an off-carriage ink delivery system for either a compact, low end printing system or a large format printing system;
(2) to allow high throughput printing, with high flow rates through the tubing;
(3) to minimize pressure drops through the tubing;
(4) to maintain accurate print head alignment, by minimizing the forces exerted by the tubing on the print head carriage; and
(5) most importantly, to provide high reliability, through very low vapor losses out of the fluid conduit and very low air diffusion into the fluid conduit.
The tubing requirements add to the difficulty of meeting these objectives. In order to minimize pressure drops, tubing with diameters larger than 0.050 inch ID (inner diameter) are desired, with a preferred inner diameter of 0.094 inches ID or larger for minimizing pressure drops. FIG. 1 is a graph showing results of characterization efforts of flow rates as a function of tube diameter for exemplary 3 centipoise ink. Moreover tube fitments become difficult when the diameter is below 0.0625 (1/16) inches. Smaller tubes are desired in order to allow for tube routing, since larger tubes exert more force and tend to kink when bent around tight corners.
The effect of larger diameters and high modulus tubing materials has two deleterious effects. First, it sets a low limit on the radius of the tubing, which impacts printer size. Going below a certain bend radius increases the force exerted by the tubing on the carriage, which will adversely affect carriage alignment. In addition, the low bend radius can result in tubing buckling or fatigue failures. This militates toward smaller diameter tubing.
The tubing used in the ink delivery system should meet several objectives. It should have a very low vapor transmission rate (VTR) and very low air diffusion. The tubing modulus should be minimized to the extent possible while meeting the other objectives to minimize the force exerted on the carriage. The tubing should operate for many cycles of the carriage scanning back and forth, e.g. for millions of cycles for some applications, without failure. Finally, the tubing should be very low cost.
Air diffusion into the tubing is a more difficult problem to eliminate than that of volatiles escaping from the tubing and the ink partially concentrating and even partially drying in the tubing. Air ingestion is the growth of bubbles that are pre-existing in the tubing that is in fluid communication with a flaccid bag. The problem is illustrated in FIG. 2. Consider ink held in a flaccid closed bag A, and connected to a printing cartridge B through a tube C with an air bubble D. The outside atmosphere, the total pressure in the bag, and the bubble total pressure are equalized (assume they are level and static):
P.sub.tot,tube =P.sub.tot,bag =P.sub.tot,outside
Now, total pressure equals air (primarily oxygen and nitrogen, not counting vapors) pressure plus partial pressure of vapor:
P.sub.tot,tube =P.sub.air,tube +P.sub.vapor,tube =P.sub.air,outside +P.sub.vapor,outside
Thus,
(P.sub.air,outside -P.sub.air,tube)=(P.sub.vapor,tube -P.sub.vapor,outside)
Now, the vapor air in the tube is fully saturated; however, the pressure of vapor outside may vary. In Arizona, for example, the vapor pressure may be very low. In Florida, it would typically be very high. In very dry environments, such as Arizona, the diffusion rate of air can be very high. With low performance tubing materials, the tubes can fill with air in a few days. The air in the tubing will be drawn into the print cartridge, causing starvation of the printhead or dysfunction of the regulator.
There are many polymeric materials that have low oxygen permeability as described below. Unfortunately they are highly crystalline and hence very stiff. Also to make a tube kink resistant the wall thickness must be increased. Both of these factors means that it is very difficult for a tube that is made of a single material to meet the simultaneous requirements of low permeability and high flexibility.
In accordance with the present invention, a multi layer tubing has been employed in a printing system which meets the above objectives. Shown in FIG. 3 is a presently preferred multi layer material tubing having three concentric layers suitable for meeting the above specifications. The multi layer material tubing has an inside diameter of between 0.100 and 0.180 inches or between 0.100 and 0.200 inches. Layer 70 is low density polyethylene (LDPE), or any other Polyolefin. These materials are chemically compatible with most inks for inkjet printers. This layer acts as the primary water vapor barrier. Layer 70 has a thickness of approximately 0.015 to 0.050 inches inch to 0.03 inch. Other suitable materials for layer 70 are high density polyethylene and polypropylene.
Layer 72 is a tie layer which functions as an "adhesive" to adhere layer 70 to layer 74. This tie layer is only required if the materials of layer 70 and layer 74 are not compatible with each other. A suitable adhesive for layer 72 when layer 70 is LDPE and layer 74 is ethylene vinyl alcohol (EVOH) is "BYNEL" which is sold by DuPont. Suitable adhesive materials for two incompatible layers are well known to those skilled in the art. Layer 72 is approximately 0.0005 to 0.0015 inches in thickness.
Layer 74 is ethylene vinyl alcohol (EVOH). This material has extremely low oxygen permeability and acts as an oxygen barrier material. However, EVOH is hygroscopic and when it absorbs water it loses its low oxygen permeability.
Accordingly, water vapor transmission into EVOH must be prevented. Layers 70 and 78 provide water vapor protection from the ink and the atmosphere, respectively. Layer 74 has a wall thickness in the range of 0.0005 inch to 0.0100 inch, and in one embodiment is approximately 0.001 to 0.005 inches in thickness to meet oxygen permeability specifications. Another suitable material for layer 74 is Polyvinylidene Chloride copolymer (PVDC).
Layer 76 is a tie layer which functions as an "adhesive" to adhere layer 74 to layer 78. This adhesive layer is only required if the materials of layer 74 and layer 78 are not compatible with each other. A suitable adhesive for layer 76 when layer 74 is ethylene vinyl alcohol (EVOH) and layer 78 is ethylene vinyl acetate (EVA) is "BYNEL." Other suitable adhesive materials are well known to those skilled in the art. Layer 76 is approximately 0.0005 to 0.0015 inches in thickness. If layers 70 and 78 are chemically similar to each other, the same material to be used as the tie material in layers 72 and 76.
Layer 78 is Ethylene Vinyl Acetate (EVA). Layer 78 performs two functions, first to protect layer 76 from exterior moisture and second to build up the thickness of the tube to prevent kinking of the tube in use. EVA is inexpensive and it is available with a low modulus of elasitisity which makes it very flexible. Layer 78 has a wall thickness in the range of 0.008 inch to 0.012 inch, and in one embodiment thickness of from 0.005 to 0.020 inches. Other suitable materials for layer 78 are LDPE high density polyethylene and polypropylene.
The tubing is manufactured using known extrusion processes for making tubing. There are typically additional standard polymer materials added to aid in the extrusion process or provide additional important properties such as flexibility; the addition of such materials is known in the art.
Turning now to FIG. 4, a perspective view is shown of an exemplary embodiment of an ink-jet printer embodying the invention, with its cover removed. Generally the printer 10 includes a tray 12A for holding an input supply of paper or other print media. When a printing operation is initiated, a sheet of paper is fed into the printer using a sheet feeder, and then brought around in a U direction to travel in the opposite direction toward output tray 12B. The sheet is stopped in a print zone 14, and a scanning carriage 16, containing one or more print cartridges 18, is then scanned across the sheet for printing a swath of ink thereon. After a single scan or multiple scans, the sheet is then incrementally shifted using a stepper motor and feed rollers (not shown in FIG. 4) to a next position within the print zone 14, and carriage 16 again scans across the sheet for printing a next swath of ink. When printing on the sheet is complete, the sheet is forwarded to a position above the tray 12B, held in that position to ensure the ink is dry, and then released.
Alternate embodiments of the printer include those with an output tray located at the back of the printer 10, where the sheet of paper is fed through the print zone 14 without being fed back in a U direction.
The carriage 16 scanning mechanism may be conventional, and generally includes a slide rod 22, along which carriage 16 slides, and a coded strip 24 which is optically detected by a photo detector in carriage 16 for precisely positioning carriage 16. A stepper motor (not shown), connected to carriage 16 using a conventional drive belt and pulley arrangement, is used for transporting carriage 16 across print zone 14.
Novel features of the inkjet printer 10 relate to the ink delivery system for delivering ink to the print cartridges 18 from an off-carriage ink supply station 30 containing replaceable ink supply cartridges 31, 32, 33 and 34. For color printers, there will typically be a separate ink supply station for black ink, yellow ink, magenta ink, and cyan ink. Since black ink tends to be depleted most rapidly, the black ink supply 34 has a larger capacity than the capacities of the other ink supplies 31-33.
A tubing set 36 of four tubes 38, 40, 42 and 44 carry ink from the four off-carriage ink supply cartridges 31-34 to the four print cartridges 18. In accordance with the invention, the tubes 38-44 comprise the multi layer tube as described above. Such tubing materials provide the necessary barrier to air diffusion, and meet the other criteria discussed above for the tubing.
FIG. 5 is a top view of the printer 10 of FIG. 4. This shows the tube routing of the tubing set 36 according to a further aspect of the invention. The tube routing is designed to accommodate the tubing set while minimizing the space needed for the tubing set 36 to follow the carriage 16 along its scanning path. In this exemplary embodiment, the tubes 38-44 are secured together in a flat ribbon intermediate the tube ends. This can be achieved by a flexible tubing carrier 46, fabricated of a flexible plastic material with tube-receiving channels 46A-46D formed therein, sized so that the individual tubes snap fit into the channels, as shown in FIG. 6. An exemplary material for fabrication of the tube carrier is polyurethane. Alternatively, the four tubes 38-44 can be fabricated of an integral extrusion, wherein the tubes are joined together by portions of the extrusion.
The tubing set 36 runs from the individual off-carriage cartridges 31-34 to the carriage mounted cartridges 18 in a run length of approximately 25 to 30 inches for a small printer, with about 26-28 inches in the exemplary embodiment. The inner tube diameter is in the range of 0.030 to 0.150 inches, depending on the required ink flow rates, with 0.054 to 0.094 inches the preferred range, and about 0.064 inches an exemplary preferred diameter of the tubing for the printer 10. The tubing outer wall thickness is preferably in the range of 0.010 inch to 0.020 inch, with a preferred value of 0.015 inches. The tubing bend stress versus air diffusion requirements tends to define this value.
The tubing set 36 runs in a channel guide 48 which is open along a side facing the print zone 14. A clamp (not shown) located at the off-carriage supply end of the channel guide secures the position of the tubing set 36 relative to this end of the guide. The channel guide 48 constrains the tubing set 36 such that it cannot move further away from the print zone 14 than the upright wall 48A of the member 48, yet permits the tubing set 36 to move out of the channel guide-as needed to follow the movement of the carriage 16.
The tubing set 36 is clamped upright to the carriage 16 by a stress relief clamp 50, and so the tubing set 36 includes an off-carriage portion and an on-carriage portion divided by the clamp 50. The tube carrier 46 terminates at the stress relief clamp. The tubing set 36 is bent upwardly in this exemplary embodiment from the level of the carriage 16 to the level of the channel member 48. This upward curve is accomplished by bending the tubes 38-44 to make the transition from a horizontal plane at carriage level to an upper horizontal plane at the channel guide 48. Downstream of the clamp 50, the ends of the tubes 38-44 are respectfully connected to input ports of a plastic manifold 60, which routes the ink through corresponding channels to manifold output ports (not shown). The manifold output ports are in turn then fluidically coupled to the corresponding print cartridges 18 via ink couplers 66 and needle/septum arrangements. Further details are more particularly described in the co-pending applications, "Ink-jet Printing System with Off-Axis Ink Supply and High Performance Tubing," Ser. No. 08/706,061, now abandoned; "Compliant Ink Interconnect Between Print Cartridge and Carriage," Ser. No. 08/706,045 filed on Jun. 30, 1996, and "Fluidic Delivery System with Tubing and Manifolding for an Off-Axis Printing System," Ser. No. 08/706,060 filed on Jun. 30, 1996, which are herein incorporated by reference.
It is understood that the above-described embodiments are merely illustrative of the possible specific embodiments which may represent principles of the present invention. Other arrangements may readily be devised in accordance with these principles by those skilled in the art without departing from the scope and spirit of the invention.
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An off-carriage printing system with high performance tubing. The printing system includes a media transporting system for transporting a print medium along a medium path to a print area, a scanning carriage for holding a printing structure including a printhead, and a scanning apparatus for scanning the carriage along a scanning axis transverse to the media path at the print area. The system further includes fixed ink supply station including an ink reservoir. A fluid conduit for the flow of ink, interconnects between the ink reservoir of the fixed ink supply station and the printing structure, the fluid conduit including a length of hollow flexible multiple layer tubing routed such that a flexible loop is formed therein. The multiple layer tubing comprises at least one inner barrier layer to water vapor transmission from the ink, at least one barrier layer to oxygen permeability, and at least one outer barrier layer to water vapor transmission from the atmosphere.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to holding and tensioning devices for leather and leather-like pieces of material and specifically for clamping and tensioning devices used to locate and hold leather pieces while stitching decorative thread patterns in the leather with an automatic stitching machine. The invention has particular utility in connection with stitching leather boot uppers and will be described in connection with such utility, although other utilities are contemplated.
2. Description of the Prior Art
Western style "cowboy" boots are manufactured by sewing together upper portions of leather known as "quarters" or "panels". A boot quarter is typically a flat piece of single or multi-ply leather or leather-like material with at least two straight opposing edges and two roughly straight, curved, or, most typically, chevron shaped opposing edges at 90° to the straight edges. The quarter, which can be either leather, leather-like material, or a synthetic substitute, is clamped into a frame or fixture known as a "pallet". The pallet locates or orients the boot quarter and holds the same in place so that decorative thread patterns can be stitched in the boot quarter with an automatic stitching machine. The automatic stitching machines may be hand operated or numerically controlled. Often, pallets are "ganged" so that several boot quarters can be stitched with the same or similar pattern in succession, thus increasing manufacturing speeds.
Prior pallet designs clamped the outer opposing edges of the boot quarter onto the side of the frame. For example, U.S. Pat. No. 4,422,310 issued to Eggenberger on Dec. 27, 1983 teaches a pallet comprising pivoting bars mounted on base strips by toggle mechanisms and having a plurality of pins on the underside which engage and pierce the edges of the boot quarter. These pins are received in corresponding holes located on base strips attached to the pallet. While the leather is drawn taut such that close rows of decorative stitches can be made without stitch overlap, this tensioning device necessitates the creation of a plurality of holes on the edges of the leather boot quarter. Furthermore, the Eggenberger patent does not define means for determining the positional coordinates of the boot quarter surface to facilitate the use of numerically controlled stitching machines.
A need exists, therefore, for a device which will not only properly locate the boot quarter in the pallet and support the same for stitching, but which will also tension the quarter without the need for piercing and subsequent damaging or marring of the edges of the boot quarter.
OBJECTS AND SUMMARY OF THE INVENTION
A primary object of the present invention is to provide a new and useful tensioning device for clamping and positioning leather or leather-like quarters which provides for stretching the boot quarter in preparation for stitching without the need for piercing the edges or otherwise damaging the material.
A further object of the present invention is to provide a boot quarter tensioning device that provides for the determination of positional coordinates on the surface of the leather or leather-like boot quarter so that numerically controlled stitching machines may be used to embroider and/or stitch decorative patterns onto the surface of the boot quarter.
A tensioning device for leather and leather-like materials according to this invention comprises a pallet having two pairs of opposing frame members and a pair of adjustable positioning clamps respectively slidably mounted on one of the two pairs of the frame members. The positioning clamps include a positioning bar, two positioning pegs that are mounted on and extend from a surface of the bar and are spaced from one another so as to contact two respective sides of the leather-like material, and fastening means, such as a screw or pin, for engaging the positioning bar to prevent it from moving relative to the pallet.
In use, the positioning bar is slidably adjusted so that the positioning pegs are seated adjacent the two respective opposing sides of the material. The positioning bar is then fastened to the position clamp, by tightening a screw or the like, so as to positively fix the material in position on the pallet. In this way, the material is held on the pallet between the adjustable positioning clamps ready for tensioning. Once the material has been positioned between the positioning clamps, two dove tail rails (which may either be fixed to the pallet or removable therefrom) are positioned so as to impinge upon the material in preparation for clamping. Preferably, the dove tail rails are shorter in length than the material piece. The piece may then either be manually or automatically tensioned prior to clamping. The dove tail rails include means for clamping onto and holding taut the thus tensioned piece. Advantageously, the clamping means are slidably mounted on the dove tail rails. Thus, the piece is held taut on the pallet between the dove tail rails and the positioning pegs.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects, advantages, and novel features of the present invention will become apparent from the following Detailed Description of the invention when considered in conjunction with the accompanying drawings, wherein:
FIG. 1 is a perspective view of the preferred embodiment of a device according to the present invention; and
FIG. 2 is a perspective view of the embodiment shown in FIG. 1, but including a webbing system for locating the position of the boot quarter relative to the pallet.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
A preferred embodiment of a device 1A according to the present invention has a metallic or wooden pallet 1 made up of two pairs 12, 13 of opposing frame members and a pair of adjustable positioning clamps 2A, 2B slidably mounted in, preferably, tracks 25A, 25B on one pair 12 of members of the pallet 1, as illustrated in FIG. 1. The adjustable positioning clamps 2A, 2B are made up of a positioning bar 3 having two positioning pegs 4A, 4B mounted on and extending from a surface of the bar 3, and suitable fastening means 5, such as a screw or pin, for engaging the positioning bar 3 to hold it in a desired position relative to the pallet 1. As stated previously, a boot quarter 6 is most typically a flat piece of single or multi-ply leather or leather-like material with two straight opposing edges 7A, 7B and two roughly straight, curved, or chevron shaped opposing edges 8A, 8B at about 90° to the straight edges 7.
In such a typical boot quarter construction, the device 1A of the present invention places adjacent the apices 9A, 9B of the chevron shaped edges 8A, 8B of the boot quarter 6 the two pegs 4A, 4B, respectively. The positioning bar 3 is slidably adjusted so that the positioning peg 4A may be seated in the apex 9A of the chevron shaped edge 8A. The other peg 4B may then be placed in position on the bar 3 adjacent the other side 8B in the apex 9B. Of course, the order of peg seating may be reversed. The positioning bar 3 is then fastened to the position clamp 2, by tightening a screw 5 or the like, whereby the boot quarter 6 is positively affixed in position on the pallet 1. In this way, the boot quarter 6 is held on the pallet 1 ready for tensioning.
Once the boot quarter 6 has been positioned between the pegs 4A, 4B, two dove tail rails 10A, B (which may either be fixed to the pallet 1 or removable therefrom via, for example, screw locks 32, are placed adjacent the edges 7 of the quarter 6). The dove tail rails 10A, B preferably are shorter in length than the boot quarter 6. The quarter 6 may be either manually or automatically tensioned prior to clamping. Once the dove tail rails 10A, B are placed adjacent the edges 7 of a boot quarter 6 (either tensioned or untensioned), the rails 10A, B are preferably clamped in place and held there immovably by toggle clamps, representatively referred to by numeral 11. Toggles 11 preferably comprise conventional toggle clamping mechanisms, as will be known to those skilled in the art. Swinging spring clamp mechanisms 30 (comprised within the toggle clamp mechanisms 11) of conventional construction are then used to hold the sides 7A, 7B of the boot quarter in place on the pallet, without damaging the quarter 6. Thus, the boot quarter 6 is held taut on the pallet 1 between the dove tail rails 10A, 10B and the positioning pegs 4A, 4B. In this preferred embodiment, the spring clamps 30A, 30B run substantially the entire length of the sides 7A, 7B, so as to provide uniform tension along the entire quarter 6. Further, according to the instant invention, the rails 11 are slidably mounted in, preferably, track means 28A, 28B, as shown in FIG. 2.
In the embodiment of the present invention shown in FIG. 2, a numerically controlled automatic stitching machine may use positions of the material 6 determined using the web 26 (in this embodiment, of grid-like construction, although other constructions are possible) as references to facilitate automatically stitching decorative patterns onto the boot quarter 6.
While the above disclosure provides a full and complete disclosure of the preferred embodiments of the instant invention, various modifications, alternatives and equivalents may be employed without departing from the spirit and scope thereof. For example, two or more pallets may be fashioned according to the instant invention and "ganged" together so that several boot quarters may be stitched at the same time to reduce manufacturing time. Additionally, if the dimensions of the material piece 6 are known or predetermined, the locks 32 may be eliminated, the rails fixed to the frame, and the positioning bar may also be fixed to the frame. Also, the bar may comprise a plurality of peg holes adapted to permit the pegs to be placed therein, so as to allow the distance between the pegs to be adjustable thereby. Therefore, the above description and illustrations should not be construed as limiting the scope of the invention, which is defined only by the hereinafter appended claims.
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A holding and tensioning device for leather and leather-like pieces of material having a pallet and a pair of adjustable positioning clamps mounted on the pallet is provided. Advantageously, the device of the instant invention is capable of holding the piece in place without damaging it, as was the case in the prior art.
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[0001] This application claims the benefit of U.S. Provisional Application No. 60/777,180, filed Feb. 27, 2006.
TECHNICAL FIELD
[0002] The present invention relates to equipment calibration and, more particularly, to a method embodied in a computer program for calibration of a valve, more particularly to calibration of a proportional solenoid valve, and even more particularly to calibration of a proportional solenoid valve used in the propulsion system of an agricultural windrower.
BACKGROUND OF THE INVENTION
[0003] U.S. Pat. No. 6,901,729, is incorporated herein by reference in its entirety. This patent describes a windrower. While other embodiments are possible, it is this general type of windrower that provides the best example of the type of system with which the apparatus and method of the instant invention can/should be used. U.S. Provisional Application No. 60/777,180, filed Feb. 27, 2006, is also incorporated herein by reference in its entirety.
[0004] In any modern windrower, and much other similar equipment, proportional solenoid controlled valves, activated by electrical currents, are used to control hydraulic devices such as cylinders in the actuation of various systems including the propulsion system. Associated with these valves is a range of current values that causes movement of a movable element of the valve such as a spool or barrel, without creating a path for hydraulic fluid flow between ports. The current value required to move the valve sufficiently to allow fluid communication between ports is referred to as an offset value. An offset of particular interest is the input current required to move the valve to a point in which hydraulic fluid first begins to flow.
[0005] It is important to efficient and effective operation of the system to calibrate the valve based on the offset values required to directly activate a proportional valve using electrical current. These offset values can determine the “crack” points between various ports. The “crack” points are the electrical signal levels at which two ports of interest are just beginning to open to one another from a closed position. Of particular interest are the crack points from the supply pressure port to each of the work ports and from the tank port to each of the work ports.
[0006] Therefore, it would be desirable to have a method which enables calibration of a valve based on the electrical current offset required to determine the crack points, for instance, those from the supply port to each of the working ports and from the tank port to each of the working ports.
SUMMARY OF THE DISCLOSURE
[0007] What is disclosed is an apparatus and method which enables calibration of a proportional solenoid valve activated by electrical current, by determining the crack points from the supply port to the working ports and from the tank port to each of the working ports by automatically deriving the electrical current offsets associated with these crack points.
[0008] According to a preferred aspect of the invention, the method utilizes a programmable control module in connection with at least one proportional solenoid valve and a sensor for detection of hydraulic cylinder displacement. The displacement of the moveable element of the hydraulic cylinder is variably controllable as a function of the electrical current signals. The electrical current signals are varied based on an actual displacement of the moveable element of the hydraulic cylinder as compared to a predetermined displacement corresponding to the initial electrical current signal. The current value associated with the offsets can be found by applying levels of input current to the valve and monitoring the hydraulic cylinder for initiation of movement as an indication of fluid flow.
[0009] A control module is programmed as part of an automatic calibration routine for directing control signals to the signal controlled device and receiving sensor inputs representative of an actual displacement of the hydraulic cylinders. The solenoid controlling the valve receives test control signals having values which will vary based the actual displacement of the hydraulic cylinder as compared to a predetermined displacement.
[0010] According to a preferred aspect of the invention, the signals comprise electrical current values within a range anticipated to encompass the current values required for the displacement of the hydraulic cylinder through its range of displacements. Additionally the sensor provides information representative of displacement of the hydraulic cylinder.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] The advantages of this invention will be apparent upon consideration of the following detailed disclosure of the invention, especially when taken in conjunction with the accompanying drawings wherein:
[0012] FIG. 1 is a side elevational view of a crop harvesting machine of the type with which the invention may be used;
[0013] FIG. 2 includes a diagram, schematic and a representative relationship between flow rate and input current for a valve of the type with which the invention may be used;
[0014] FIG. 3 is a top level block diagram including the interconnections of the invention;
[0015] FIG. 4 is a high level flow diagram of steps of a preferred embodiment of a computer program of the invention;
[0016] FIG. 5 is another high-level flow diagram of steps of a preferred embodiment of a computer program of the invention;
[0017] FIG. 6 is another high-level flow diagram of steps of a preferred embodiment of a computer program of the invention;
[0018] FIG. 7 is another high-level flow diagram of steps of a preferred embodiment of a computer program of the invention;
[0019] FIG. 8 is a written listing of steps of the preferred program of the invention;
[0020] FIG. 9 is a written listing of still further steps of the preferred program of the invention; and
[0021] FIG. 10 is a written listing of still further steps of the preferred program of the invention;
[0022] FIG. 11 is a written listing of still further steps of the preferred program of the invention;
[0023] FIG. 12 is a written listing of still further steps of the preferred program of the invention;
[0024] FIG. 13 is a written listing of still further steps of the preferred program of the invention;
[0025] FIG. 14 is a written listing of still further steps of the preferred program of the invention;
[0026] FIG. 15 is a written listing of still further steps of the preferred program of the invention;
[0027] FIG. 16 is a written listing of still further steps of the preferred program of the invention;
[0028] FIG. 17 is a written listing of still further steps of the preferred program of the invention;
[0029] FIG. 18 is a written listing of still further steps of the preferred program of the invention;
[0030] FIG. 19 is a written listing of still further steps of the preferred program of the invention;
[0031] FIG. 20 is a written listing of still further steps of the preferred program of the invention;
[0032] FIG. 21 is a written listing of still further steps of the preferred program of the invention;
[0033] FIG. 22 is a written listing of still further steps of the preferred program of the invention;
[0034] FIG. 23 is a written listing of still further steps of the preferred program of the invention;
[0035] FIG. 24 is a written listing of still further steps of the preferred program of the invention;
[0036] FIG. 25 is a written listing of still further steps of the preferred program of the invention;
[0037] FIG. 26 is a written listing of still further steps of the preferred program of the invention;
[0038] FIG. 27 is a written listing of still further steps of the preferred program of the invention;
[0039] FIG. 28 is a written listing of still further steps of the preferred program of the invention;
[0040] FIG. 29 is a written listing of still further steps of the preferred program of the invention;
[0041] FIG. 30 is a written listing of still further steps of the preferred program of the invention;
[0042] FIG. 31 is a written listing of still further steps of the preferred program of the invention;
[0043] FIG. 32 is a written listing of still further steps of the preferred program of the invention;
[0044] FIG. 33 is a written listing of still further steps of the preferred program of the invention;
[0045] FIG. 34 is a written listing of still further steps of the preferred program of the invention;
[0046] FIG. 35 is a written listing of still further steps of the preferred program of the invention;
[0047] FIG. 36 is a written listing of still further steps of the preferred program of the invention;
[0048] FIG. 37 is a written listing of still further steps of the preferred program of the invention;
[0049] FIG. 38 is a written listing of still further steps of the preferred program of the invention; and
[0050] FIG. 39 is a written listing of still further steps of the preferred program of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0051] Many of the fastening, connection, processes and other means and components utilized in this invention are widely known and used in the field of the invention described, and their exact nature or type is not necessary for an understanding and use of the invention by a person skilled in the art, and they will not therefore be discussed in significant detail. Also, any reference herein to the terms “left” or “right” is used as a matter of mere convenience, and is determined by standing at the rear of the machine facing in its normal direction of travel. Furthermore, the various components shown or described herein for any specific application of this invention can be varied or altered as anticipated by this invention and the practice of a specific application of any element may already by widely known or used in the art by persons skilled in the art and each will likewise not therefore be discussed in significant detail.
[0052] FIG. 1 shows the present invention utilized in connection with a self-propelled windrower 10 ; however, it will be appreciated that the principles of the present invention are not limited to a self-propelled windrower, or to any specific type of harvesting machine.
[0053] In the illustrated embodiment, the self-propelled windrower 10 comprises a tractor 12 and a header 14 attached to the front end of a frame 18 or chassis of the tractor 12 . FIG. 3 shows a top level block diagram 30 of the interconnections of exemplary valve apparatus that can be calibrated using the method embodied in the invention. The method of the present invention describes a routine programmed in a control module 32 that calibrates the input current offsets of a proportional solenoid valve controlled hydraulic actuator as represented by hydraulic actuator 20 which is a common hydraulic cylinder. Application of the input current offsets to a solenoid 24 , 26 causes movement in the valve to the point at which two ports are just beginning to open to one another. This offset current can be identified by monitoring a motion or displacement of a moveable element 42 of the actuator 20 , which can be, for instance, a piston and rod assembly. A sensor 22 is used to sense cylinder 42 motion and/or position, embodied by motion or displacement of element 42 . The offset values to be sensed can be, but are not necessarily limited to:
1. The ‘cracking’ of a supply pressure port (P) 34 to each of the work ports 36, 38. 2. The ‘cracking’ of a tank port (T) 40 to each of the work ports 36 , 38 .
[0056] The ‘crack’ points are defined as the electrical signal levels at which two ports 34 , 36 , 38 , 40 of interest are just beginning to open to one another from a closed position. The profile 43 of the ‘crack’ points in relation to hydraulic fluid flow and current applied to solenoid 24 , 26 is shown in FIG. 2 . Points iAp, iAt, iBp, and iBt can be defined as crack points. A crack point is detected via motion of actuator 20 which is directly correlated to flow. To calibrate a ‘cracking’ point, a binary divide algorithm is used.
[0057] The binary divide routine uses a set of predetermined parameters. These parameters must be defined before execution of the algorithm. These parameters are:
1. Upper limit of electrical signal value (i_ul). 2. Lower limit of electrical signal value (i_ll). 3. Nominal value of electrical signal (i_nom). 4. Dwell time 1 (dt 1 ). 5. Dwell time 2 (dt 2 ). 6. A predetermined distance of cylinder motion (dp). 7. Tolerance on predetermined distance of cylinder motion (dp_tol). 8. Value of electrical signal to be held between stages of calibration (i_null). 9. Number of loops through calibration (n_loops). Other variables used in the algorithm are: 10. High signal history value (i_hh). 11. Low signal history value (i_hl). 12. Electrical test signal value (i_test). 13. initial cylinder position (p_i). 14. Final cylinder position (p_f). 15. Cylinder position difference (dp_diff). 16. Loop counter (count). 17. Number of time cylinder moved (num_mv). 18. Number of times cylinder didn't move (num_nomv).
[0076] Noted below is the step by step procedure involved in running a calibration for a single crack point:
Initialization of Binary Divide Algorithm:
[0000]
Step 1: Set Electrical test signal to nominal value, i_test=i_nom.
Step 2: Set high history value to upper limit of electrical signal value, i_hh=i_ul.
Step 3: Set low history value to lower limit of electrical value, i_hl=i_ll.
Step 4: Set counters to zero, Count=num_mv=num_nomv=0.
Binary Divide Algorithm:
[0000]
Step 1: Check position of cylinder by averaging sensor value over dt 1 . Set p_i to this value.
Step 2: Set hardware to the test value, i_test, and hold for dt 2 .
Step 3: While maintaining electrical signal at i_test, check cylinder position by averaging sensor value over dt 1 . Set p_f to this value. Set i_test to i_null.
Step 4: Check distance of cylinder motion d by comparing p_i and p_f.
Step 5: Did cylinder move?
If cylinder moved greater than dp, increment num_mv counter. num_mv=num_v+1. If cylinder moved less than dp, increment num_nomv counter. num_nomv=num_nomv+1. Increment loop counter, count=count+1. If loop counter (count) is greater than limit (n_loops), prepare to exit algorithm. If either num_mv or num_nomv is equal to zero (cylinder either always moved or never moved),
[0091] Calibration Failed.
Otherwise record and/or return value of i_test and exit algorithm.
[0093] Calibration Complete.
Step 6: Determine new value of i_test.
If distance of cylinder motion greater than dp, set next electrical test signal value to: i_test=i_test+(i_hh−i_test)/2. If distance of cylinder motion greater than dp, set next electrical test signal value to: i_test=i_test−(i_test−i_hl)/2.
Step 7: Check to see if new i_test values are out of bounds.
If i_test>i_ul or i_test<i_ll, then set warning flag and exit calibration.
[0099] Calibration Failed.
Step 8: Return to Step 2.
[0101] This algorithm is run for each of the defined calibration points. For example the crack points iAp, iAt, iBp, and iBt shown in FIG. 3 , the binary divide routine would be run a total of four times. Each of the values 1-8 noted above would have to be redefined for each of the four runs. For the crack to tank calibrations, an external force would have to be applied to the cylinder to force oil flow from the hydraulic cylinder through the valve. One way of doing this is to use a spring centered cylinder and set the cylinder to a position away from the spring centered position at the beginning of the test.
[0102] Referring also to FIGS. 4-7 , a flow diagram 80 illustrating steps of a method of the instant invention for determining the offset values for control of a proportional solenoid valve operable for controlling movement of element 42 of hydraulic cylinder 20 is shown. The steps of flow diagram 80 are preferably programmed in, and executable by, control module 32 at appropriate times, such as, but not limited to, when changes in the hydraulic system are effected. The calibration routine will be initiated and automatically run in such situations. As shown in FIG. 4 , block 82 initiates an offset calibration routine. The variables referenced above are initialized at block 82 . At block 84 a current input i_test is applied for a specified duration dt 2 . The actual responsive movement d of hydraulic cylinder element 42 is computed at block 86 as the final position p_f of cylinder 42 minus the initial position p_i of cylinder 42 .
[0103] Following bubble A to FIG. 5 module 32 checks for cylinder 42 movement at block 88 . Actual displacement d is compared to a predetermined displacement expected dp in response to the initial input i_test in the step shown in decision blocks 100 , 102 . If actual displacement d of cylinder 42 exceeds predetermined displacement expected dp in response to the initial input i_test, a counter indicating cylinder element 42 movement, num_mv is incremented at block 104 . If actual displacement d of cylinder 42 is less than predetermined displacement expected dp in response to the initial input i_test, a counter indicating a lack of cylinder element 42 movement, num_nomv is incremented at block 106 .
[0104] Following bubble B, a loop counter count is incremented at block 108 as shown in FIG. 6 . Count is compared to a predetermined number of times n_loops as shown at block 110 . If count has reached n_loops, module 32 compares counters num_mv and num_nomv to zero at decision block 112 . If either num_mv or num_nomv are zero, cylinder 42 either moved for every value of i_test or for no value of i_test. Module 32 reports a calibration failure. If num_mv and num_nomv are nonzero, calibration is complete and the value of i_test is noted or stored by module 32 . If count has not reached n_loops, a new value of i_test is calculated by following bubble C to FIG. 7 which represents additional steps of module 32 .
[0105] In FIG. 7 a new value of i_test is calculated as shown at block 114 . Decision block 116 compares actual displacement d to predetermined displacement dp. If actual displacement d is less than predetermined displacement dp, i_test is calculated to be a value half way between a previously set high history i_hh value of i_test according to a binary divide algorithm as indicated in block 118 . If actual displacement d is not less than predetermined displacement dp, i_test is calculated to be a value half way between a previously set low history i_hl value of i_test according to the binary divide algorithm as indicated in block 120 . The high history i_hh is initialized to the current upper limit, and updated with the value i_test when actual displacement d is greater than dp. The low history i_hl is initialized to the current lower limit, and updated with the value i_test when actual displacement d is less than dp. Once the new i_test is calculated, its value is checked against the input current upper limit and lower limit. If the new i_test is outside these limits, the calibration fails. If the new i_test is within these limits, module 32 follows bubble D to repeat application of i_test at block 84 of FIG. 4 with the new i_test.
[0106] As a result of execution of the calibration routine of the instant invention, registers of control module 32 will contain information representative of input electrical current values required to be directed to solenoid 24 , 26 to determine current values corresponding to crack points such as iAp, iBp, iAt, and iBt.
[0107] Referring also to FIGS. 8-39 , lines of code of an actual computer program embodying the above described steps of the method of the invention is disclosed. The notes accompanying the lines of code describe many features of the method of the invention.
[0108] It will be understood that changes in the details, materials, steps and arrangements of parts which have been described and illustrated to explain the nature of the invention will occur to and may be made by those skilled in the art upon a reading of this disclosure within the principles and scope of the invention. The foregoing description illustrates the preferred embodiment of the invention; however, concepts, as based upon the description, may be employed in other embodiments without departing from the scope of the inventions. Accordingly, the following claims are intended to protect the invention broadly as well as in the specific form shown.
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A method for calibrating a proportional solenoid valve used in the propulsion system of a windrower, wherein a programmable control module in connection with a valve and a sensor is programmed as part of an automatic calibration routine for directing test control signals to the valve for causing a predetermined displacement of the hydraulic cylinder, the test control signals having values which vary based on the actual displacement of the hydraulic cylinder as compared with a predetermined value of displacement, and operating the hydraulic cylinder using the test control signal that causes the predetermined displacement of the element. The predetermined displacements correspond to the crack points, or the electrical signal levels at which two ports of interest are just beginning to open to one another from a closed position. Of particular interest are the crack points from the supply pressure port to each of the work ports and from the tank port to each of the work ports.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a divisional of application Ser. No. 10/953,991 filed Sep. 29, 2004, now U.S. Pat. No. 7,459,112, which is a divisional of application Ser. No. 09/965,489, filed Sep. 27, 2001, now U.S. Pat. No. 6,821,625, the contents of which are incorporated by reference herein in their entirety.
BACKGROUND
In nearly every sector of the electronics industry, electronic circuitry involves the interconnection of an integrated chip (hereinafter “chip”) and a surface or device upon which the chip is supported. During operation of the circuitry, heat is generated and a heat flux is established between the chip and its environment. In order to remove heat more effectively to ensure the proper functioning of the circuitry, the heat flux is disseminated across a surface area larger than the surface area of the chip and transferred to an attached heat sink device. Once the heat is transferred to the heat sink device, it can be removed by a forced convection of air or other cooling means.
In some applications, multiple processors and their associated control and support circuitry are arranged on a single chip. Such arrangements may result not only in a further increase in the heat flux, but also in a non-uniform distribution of the heat flux across the surface of the chip. The non-uniformity of the distribution of the heat flux is generally such that a higher heat flux is realized in the processor core region and a significantly lower heat flux is realized in the region of the chip at which the control and support circuitry is disposed. The high heat flux in the processor core region may cause devices in this region to exceed their allowable operating temperatures. The resulting disparity in temperature between the two regions, which may be significant, may contribute to the stressing and fatigue of the chip.
A thermally conductive heat spreading device is oftentimes disposed between the chip and the heat sink device to facilitate the dissemination of heat from the chip. Such heat spreading devices are generally plate-like in structure and homogenous in composition and fabricated from materials such as copper, aluminum nitride, or silicon carbide. Newer carbon fiber composites exhibit even higher thermal conductivities than these traditional thermal spreader materials; however, they tend to be anisotropic in nature, exhibiting wide variations in thermal conductivity between a major axis normal to the face of the structure (in the Z direction) and the axes orthogonal to the major axis (in the X and Y directions). Moreover, the lower thermal conductivity in the direction along the major axis tends to have the effect of increasing the thermal resistance of the heat spreading device, thereby inhibiting the dissemination of heat from the device.
SUMMARY
A thermal spreading device disposable between electronic circuitry and a heat sink is disclosed. The device includes a substrate having a first face and a second face and a plurality of conduits extending through the substrate from the first face to the second face. The two faces of the substrate are disposed in a parallel relationship. The material of which the substrate is fabricated has a first thermal conductivity value in a direction parallel to the faces and a second thermal conductivity value in a direction normal to the faces, with the second thermal conductivity value being less than the first thermal conductivity value. The material of which each conduit is fabricated has a thermal conductivity value associated with it, with the thermal conductivity value of each conduit being greater than the second thermal conductivity value of the substrate.
One method of fabricating the thermal spreading device includes arranging a plurality of thermally conductive rods such that the rods extend longitudinally in a common direction, disposing a molding material radially about the longitudinally extending rods, hardening the molding material around the plurality of thermally conductive rods, and cutting the hardened molding material into slices in a direction perpendicular to the direction in which the rods longitudinally extend. Other methods of fabrication include press fitting or shrink fitting the thermally conductive rods into holes in the substrate.
BRIEF DESCRIPTION OF THE DRAWINGS
The present disclosure will be better understood by those skilled in the pertinent art by referencing the accompanying drawings, where like elements are numbered alike in the several FIGURES, in which:
FIG. 1 is a perspective cutaway view of a thermal spreading device;
FIGS. 2A through 2C are perspective views of a batch process of the fabrication of a thermal spreading device;
FIGS. 3A and 3B are perspective views of a batch process of the fabrication of a thermal spreading device in which conduits are press fitted into the substrate;
FIG. 4 is a sectional view of a step in a batch process of the fabrication of a thermal spreading device in which conduits are shrink fitted into the substrate;
FIG. 5 is a sectional view of the engagement of a thermal spreading device with a chip and a heat sink;
FIGS. 6 and 7 are plan and cross sectional views of an alternate exemplary embodiment of a thermal spreading device; and
FIG. 8 is an exploded perspective view of the engagement of the thermal spreading device of FIGS. 6 and 7 with a chip.
DETAILED DESCRIPTION
Referring now to FIG. 1 , an exemplary embodiment of a thermal spreading device is shown generally at 10 and is hereinafter referred to as “thermal spreader 10 .” Thermal spreader 10 is a conduction medium that provides for thermal communication between electronic circuitry (e.g., a chip) and an environment to which thermal spreader 10 is exposed. The thermal communication is effectuated by the conduction of heat across a substrate 12 to a heat sink (shown with reference to FIG. 5 ). Because the materials from which substrate 12 are fabricated are generally of an anisotropic nature, substrate 12 is oftentimes characterized by a marked disparity in thermal conductivities in orthogonal directions. In particular, the thermal conductivity of substrate 12 in a direction shown by an arrow 16 (Z direction), which is normal to the interface of thermal spreader 10 and the circuitry (not shown), may be substantially less than thermal conductivities in the directions shown by an arrow 18 (X direction) and an arrow 19 (Y direction) along the same interface of thermal spreader 10 and the circuitry. Due to such disparities, the thermal resistance across substrate 12 (in the direction of arrow 16 ) is increased, and the rate of heat transfer (flux) across thermal spreader 10 varies dramatically from the flux in the direction (as shown by arrows 18 and 19 ) that the interface extends.
In order to enhance the thermal communication across thermal spreader 10 , substrate 12 is configured to include thermal conduits 14 . The materials from which thermal conduits 14 are fabricated generally have thermal conductivity values that are substantially higher than the thermal conductivity values in the Z direction of the material from which substrate 12 is fabricated. Because the flux through conduits 14 is greater than the flux in the same direction across the surrounding substrate 12 , heat conduction is enhanced across substrate 12 in the direction shown by arrow 16 (Z direction), viz., in the direction in which conduits 14 extend. Heat transfer is thereby optimized through substrate 12 via conduits 14 .
Conduits 14 are defined by rods or wires having substantially circular cross sectional geometries, as is shown. Rods or wires having substantially circular cross sectional geometries enable a substantially uniform transfer of heat to be maintained in the directions radial to the circular cross section. Other cross sectional geometries that may be used include, but are not limited to, elliptical, square, flat, multi-faced, and configurations incorporating combinations of the foregoing geometries. Regardless of the cross sectional geometry, conduits 14 are formed from materials having high thermal conductivities. Such materials include, but are not limited to, copper, aluminum, carbon, carbon composites, and similar materials that exhibit a high thermal conductivity along the conduit axis. The carbon materials may be fibrous or particulate in structure.
Substrate 12 provides an anchor into which conduits 14 are disposed while further providing a medium for the transfer of heat in directions along and parallel to the interface defined by the positioning of thermal spreader 10 on the chip. Exemplary materials from which substrate 12 can be fabricated include, but are not limited to, carbon and carbon composites. As noted above with respect to conduits 14 , the carbon materials may be fibrous or particulate in structure.
The configuration of thermal spreader 10 is generally such that conduits 14 are arranged to be parallel to each other, as is shown in FIG. 1 . Furthermore, conduits 14 generally extend linearly between opposing surfaces of substrate 12 . As shown, the architecture of thermal spreader 10 is further defined by a substantially uniform spatial positioning of conduits 14 over any randomly selected section of substrate 12 . The even distribution of conduits 14 facilitates and improves the conduction of heat from a first face 20 disposed adjacent the chip and an opposingly-positioned second face 24 disposed adjacent the heat sink. Such a distribution provides for the effective transfer of heat longitudinally through conduits 14 while maintaining the substantially uniform transfer of the heat in the directions radial to the surfaces of conduits 14 .
When thermal spreader 10 is mounted between a chip (shown with reference to FIG. 5 ) and a heat sink (also shown with reference to FIG. 5 ), conduits 14 enable heat generated during the operation of the chip to be communicated from first face 20 of thermal spreader 10 through conduits 14 across substrate 12 to second face 24 of thermal spreader 10 . Although the material of which substrate 12 is fabricated allows for some degree of thermal conduction between faces 20 , 24 , the anisotropic nature of the material causes heat generated by the chip and transferred to thermal spreader 10 to be more substantially dissipated through substrate 12 in the directions shown by arrows 18 and 19 . Dissipation of heat in the directions shown by arrows 18 and 19 allows for the heat to be conducted to a larger number of conduits 14 , which further allows for the more effective transfer of heat from the chip to the heat sink.
Referring now to FIGS. 2A through 2C , an exemplary batch process illustrating the fabrication of the thermal spreader is illustrated. The process comprises arranging the rods or wires by which conduits 14 are defined into an array, which is shown generally at 30 in FIG. 2A . The rods are arranged such that the longitudinal axes of the rods are parallel to each other and held fast by a jig (not shown) or other device configured to maintain the rods in their proper alignment. Molding material of which the substrate is formed is then disposed around the rods, hardened, and cured, as is shown in FIG. 2B . The hardened and cured molding material forms a block, shown generally at 32 , having thermal conduits 14 extending between first face 20 and opposing second face 24 thereof. Block 32 is then sawed or otherwise made into sheets 34 , as is illustrated in FIG. 2C . Each sheet 34 is of a thickness t s , which is slightly in excess of the desired thickness of the finished thermal dissipating device. Sheets 34 are then polished on at least one face thereof to bring thicknesses t s within the allowable tolerances of final product. Polishing of the sheets on both sides further provides sheets 34 with surface textures conducive to a more effective transfer of heat between the chip and the heat sink. Finally, sheets 34 are cut into individual thermal spreaders 10 of the desired length and width.
In another exemplary process of the fabrication of the thermal spreader, thermal conduits 14 may be press-fitted into substrate 12 , as is shown in FIGS. 3A and 3B . Referring to FIG. 3A , holes 28 are drilled, punched, or otherwise formed in block 32 . The cross sectional geometries of holes 28 correspond with the cross sectional geometries of conduits 14 insertable into holes 28 . Referring now to FIG. 3B , conduits 14 are inserted into holes 28 under a compressive force C f effectuated by a press (not shown) or a similar apparatus. The mechanical tolerances of conduits 14 are such that when conduits 14 are received in holes 28 , a tight fit is maintained between the inner surfaces of holes 28 and the outer surfaces of each conduit 14 , thereby allowing effective thermal communication to be maintained between the material of block 32 and conduits 14 . Block 32 may then be sawed or otherwise formed into sheets and polished and cut to the desired lengths and widths.
In yet another exemplary process of the fabrication of the thermal spreader, thermal conduits 14 may be shrink-fitted into substrate 12 , as is shown in FIG. 4 . In the shrink-fitting process, holes 28 are again drilled, punched, or otherwise formed in block 32 , as was described above. Block 32 is heated to a temperature that causes block 32 (and subsequently holes 28 ) to expand. Upon expansion, conduits 14 are inserted into holes 28 with little effort such that space is defined by inner surfaces 34 of holes and outer surfaces 36 of conduits 14 . Block 32 is then cooled to cause the material of fabrication of block 32 to contract, thereby constricting holes 28 and eliminating the spaces defined between the inner surfaces of holes 28 and the outer surfaces of conduits 14 . Once constricted, conduits 14 are securely retained within block 28 . Block 32 may then be sawed or otherwise formed into sheets and polished and cut to the desired dimensions in manners similar to those described above to form the final product.
Referring now to FIG. 5 , a thermal conduction package is shown generally at 38 . In thermal conduction package 38 , thermal spreader 10 is shown as it would be disposed between the chip 40 disposed in electronic communication with its associated circuitry through substrate 42 and the heat sink 44 . Thermal spreader 10 is adhered to chip 40 with an adhesive 48 , which may be a solder or an epoxy material applied to chip 40 as a thin layer upon which thermal spreader 10 is placed. A layer of thermal paste 50 , which is typically a natural or synthetic oil-based compound with thermally conductive particle filler, is applied to the exposed surface of thermal spreader 10 upon which heat sink 44 is mounted. Both adhesive 48 and thermal paste 50 facilitate the transfer of heat between chip 40 and thermal spreader 10 and thermal spreader 10 and heat sink 44 respectively, thereby enhancing the conduction of heat across thermal spreader 10 .
As is shown with reference to FIGS. 6 and 7 , another exemplary embodiment of a thermal dissipating device is shown generally at 110 . Thermal spreader 110 is substantially similar to thermal spreader 10 as illustrated above with reference to FIGS. 1 through 5 . Thermal spreader 110 , however, includes an arrangement of variably spaced conduits 114 disposed within a dissipating substrate 112 . The arrangement of variably spaced conduits 114 is configured to define regions 150 in which the density of conduits 114 is greater than the density of conduits 114 in adjacently positioned regions 152 of the same substrate 112 . The high-density regions 150 are positioned on substrate 112 to register with areas of high heat flux on a chip upon assembly of the thermal conduction package.
Referring now to FIG. 8 , the engagement of the thermal spreader with the chip is illustrated generally at 138 . When thermal spreader 110 is placed in communication with chip 140 , the high-density regions 150 register with the areas of high flux 160 on chip 140 . Such a placement allows for the increased transfer of heat from the areas of high flux 160 on chip 140 to high-density regions 150 of thermal spreader 110 while simultaneously providing a thermally adequate transfer of heat from the areas of chip 140 from which lower heat flux is realized. The disparities in the densities of the conduits in each region 150 , 152 are engineered to provide for the removal of heat from each portion of chip 140 and the transfer of heat to the heat sink to minimize disparity in heat build up at the interface of chip 140 and thermal spreader 110 . Minimization of such disparity may provide improved operability of chip 140 and increase the useful life thereof. Fabrication of thermal spreader 110 is effectuated in a batch process substantially similar to that illustrated in FIGS. 2A through 4 for thermal spreader 10 .
While the disclosure has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the disclosure. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the disclosure without departing from the essential scope thereof. Therefore, it is intended that the disclosure not be limited to the particular embodiment disclosed as the best mode contemplated for carrying out this disclosure, but that the disclosure will include all embodiments falling within the scope of the appended claims.
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A thermal spreading device disposable between electronic circuitry and a heat sink includes a substrate having parallel first and second faces and conduits extending through the substrate between the faces. The substrate material has a first thermal conductivity value in a direction parallel to the faces and a second thermal conductivity value in a direction normal to the faces, with the second thermal conductivity value being less than the first thermal conductivity value. The conduit material has a thermal conductivity value associated with it, with the thermal conductivity value being greater than the second thermal conductivity value of the substrate. One method of fabricating the thermal spreading device includes disposing a molding material radially about the rods and hardening the material. Other methods include press fitting and shrink fitting the rods into a substrate material.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation-in-part of the following applications, which are hereby incorporated by reference: U.S. patent application Ser. No. 11/134,786 filed May 20, 2005; U.S. patent application Ser. No. 11/204,920 filed Aug. 15, 2005; U.S. patent application Ser. No. 11/344,883 filed Feb. 1, 2006; U.S. patent application Ser. No. 11/348,745 filed Feb. 7, 2006; U.S. patent application Ser. No. 11/279,360 filed Apr. 11, 2006; U.S. patent application Ser. No. 11/413,829 filed Apr. 28, 2006; U.S. patent application Ser. No. 11/537,602 filed Sep. 29, 2006; U.S. patent application Ser. No. 11/537,590 filed Sep. 29, 2006; U.S. patent application Ser. No. 11/537,599 filed Sep. 29, 2006; U.S. patent application Ser. No. 11/537,595 filed Sep. 29, 2006; U.S. patent application Ser. No. 11/685,548 filed Mar. 13, 2007; U.S. patent application Ser. No. 11/685,551 filed Mar. 13, 2007; and U.S. patent application Ser. No. 11/744,591 filed May 4, 2007.
BACKGROUND OF THE INVENTION
1. The Field of the Invention
The present invention relates to systems and methods for out-of-band communication across optical transceiver modules of a network fabric.
2. The Relevant Technology
In modern networks, network devices such as switches, routers, host bus adapters (HBA), servers, and the like, are coupled to one another by means of fiber optic transceivers. Many transceivers are “active,” meaning that they have memory and processing capabilities. U.S. patent application Ser. No. 11/070,757, filed Mar. 2, 2005, which is hereby incorporated by reference, discloses systems and methods by which transceiver modules communicate with one another independently of the network device from which they receive data. The '757 application discloses a system wherein an optical transceiver module modulates the peak or average power of a transmitted signal at a low frequency in order to transmit module specific data out of the frequency band carrying the network data transmitted by the module. A receiving module demodulates the out-of-band data by tracking modulation of the peak or average power of the received signal.
In a typical network, components are not all updated or replaced simultaneously. Both new and old components must therefore be able to communicate with one another even though older components may not be updated. Some transceivers have firmware that may be reprogrammed to facilitate communication with newer modules. However, it is not convenient to update each transceiver in a network each time a newer module is installed. Furthermore, older transceivers have physical limitations, such as a smaller memory, lower processing speed, and less sophisticated optics that cannot be readily updated.
In view of the foregoing, it would be an advancement in the art to provide systems and methods for enabling out-of-band communication across a heterogeneous fiber optic network including transceiver modules of differing capabilities.
BRIEF SUMMARY OF THE INVENTION
In one aspect of the invention, communication between transceiver modules having a memory defining a number of tables each having a size and offset address includes determining a table and offset address for requested data according to a table size of an originating module. A system address corresponding to the table and offset address is generated and a read command having a command type indicating a system address size, the system address, a length of the requested data, and a contingency field storing the table size of the originating module is transmitted to a receiving module. The receiving module regenerates the table and offset address from the system address and the table size stored in the contingency field. If the table size stored in the contingency field is the same as a table size of the receiving module, then data having the length of the requested data stored at an address corresponding to the table and offset address is transmitting to the receiving module. If the table size stored in the contingency field is not the same as the table size of the receiving module, data having a length different from the requested length from a table of the receiving module having a table number corresponding to the regenerated table and offset address is transmitted.
In another aspect of the invention, the receiving module evaluates whether it has sufficient memory to return data having the length of requested data beginning at the regenerated table and offset address, and, if not, evaluating an extended contingency field. If the extended contingency field does not contain an instruction not to truncate, the receiving module transmits to the originating module data beginning at the regenerated table and offset address having a length less than the length of requested data.
In another aspect of the invention, communication between the originating and receiving modules occurs in an out-of-band optical channel.
In another aspect of the invention a method for discovering a network fabric includes transmitting a first knock knock command from the transmit port of a first transceiver module of a plurality of transceiver modules having receive ports and transmit ports. If a response to the first knock knock command is received at the receive port of the first transceiver module, then the first transceiver records an indicator that it is in a point-to-point network. If a response to the first knock knock command is not received at the receive port of the first transceiver module, then it sends a second knock knock command containing an instruction to forward the second knock knock command N times, where N is greater than 1. If a response to the second knock knock command is received at the receive port of the first transceiver module, then the first transceiver module an indicator that it is in a ring network having N layers.
if a response to the second knock knock command is not received at the receive port of the first transceiver module, then it sends a plurality of subsequent knock knock commands each containing an instruction to forward, wherein each subsequent knock knock command instructs a receiving transceiver module to forward the subsequent knock knock command M times, where M is the number of times the previous knock knock command of the subsequent knock knock commands instructs the receiving transceiver module to forward the subsequent knock knock command plus an increment value. If a response to one of the subsequent knock knock commands is received, then the first transceiver module records an indicator that the first transceiver module is in a ring network having M layers. If a response to one of the subsequent knock knock commands having a value of M greater than a maximum value is not received, then the first transceiver module records an indicator that the first transceiver module is not in a ring or point-to-point network.
These and other objects and features of the present invention will become more fully apparent from the following description and appended claims, or may be learned by the practice of the invention as set forth hereinafter.
BRIEF DESCRIPTION OF THE DRAWINGS
To further clarify the above and other advantages and features of the present invention, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. It is appreciated that these drawings depict only typical embodiments of the invention and are therefore not to be considered limiting of its scope. The invention will be described and explained with additional specificity and detail through the use of the accompanying drawings in which:
FIG. 1 illustrates a schematic block diagram of in-band and out-of-band links transceiver modules hosted by network devices in accordance with an embodiment of the present;
FIG. 2 is a schematic block diagram of a ring network;
FIG. 3 is a schematic block diagram of a star network;
FIG. 4 is a schematic block diagram of a network fabric;
FIG. 5 is a process flow diagram of a method for discovering module connections in accordance with an embodiment of the present invention;
FIG. 6 is a process flow diagram of a method for reading and writing data between dissimilar transceivers in accordance with an embodiment of the present invention;
FIG. 7 is a process flow diagram of a method for suppressing error message traffic in accordance with an embodiment of the present invention;
FIG. 8 is a process flow diagram of a method for discovering a network configuration in accordance with an embodiment of the present invention; and
FIG. 9 is a process flow diagram of a method for detecting network intrusions in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1 , a network 10 includes a number of network devices 12 a , 12 b . The network devices may be embodied as workstations, servers, switches, routers, host bus adapters, or the like. Transceiver modules 14 a , 14 b are coupled to each network device 12 a , 12 b and received network data 16 by means of a data channel 18 . In the illustrated embodiment, the transceiver modules 14 a , 14 b are optical transceivers including a transmitter optical subassembly (TOSA) and a receiver optical subassembly (ROSA). The transceiver modules 14 a , 14 b may conform to any industry standard form factor such as SFP, XFP, X2, XPAK, or XENPAK.
The transceiver modules 14 a , 14 b store module data 20 that includes diagnostic and operational data that is used by the modules 14 a , 14 b to control parameters governing the transmission of data over an optical fiber, such as output power, carrier frequency, bit period, duty cycle, rise time, fall time and the like. Module data 20 may include data relating to receiving of data over an optical fiber such as eye profile, eye mask parameters, threshold, sensitivity, and the like. The module data 20 may include diagnostic data regarding itself and another module 14 a , 14 b to which it is connected. Such data may include the received power, recovered clock frequency, bit error rate, or the like, of a received signal. The diagnostic data may include self diagnostic data such as the results of self-tests of a module component such as a laser.
The modules 14 a , 14 b are coupled to one another by a data channel 22 and an out-of-band (OOB) channel 24 . In a preferred embodiment, the data channel 22 and OOB channel 24 include the same physical medium, such as an optical fiber. For example, the data channel 22 may include high frequency modulation of an optical signal transmitted over an optical fiber whereas the OOB channel 24 includes low frequency modulation of the power envelope of the same optical signal, such as is disclosed in U.S. patent application Ser. No. 11/070,757, which is incorporated herein by reference. In other embodiments, the data channel 22 includes optical signals transmitted over an optical fiber or wire whereas the OOB channel 24 includes a radio frequency (RF) channel.
The network data 16 is transmitted over the data channel 22 by the transceiver modules 14 a , 14 b . Diagnostic and configuration data included in the module data 20 are communicated to other transceiver modules 14 a , 14 b in the OOB channel 24 . However, in some embodiments, both diagnostic and configuration and network data are transmitted over the same data channel 22 . For purposes of this disclosure all communication over an OOB channel 24 may also take place over the in-band data channel 22 . OOB channel 24 may also carry instructions from a transceiver 14 a to a transceiver 14 b . For example, U.S. application Ser. No. 11/966,646 discloses a test transceiver that communicates with a corrective transceiver to generate network errors for diagnostic purposes. Communication between the test transceiver and corrective transceiver in the abovereferenced application may occur in the OOB channel 24 . For example, the test transceiver may instruct the corrective transceiver not to correct for errors that the test transceiver introduces into the data channel 22 . In other applications a transceiver 14 a may instruct a transceiver 14 b by means of the OOB channel 24 to encrypt data in the data channel 22 .
Examples of systems that may use an OOB channel 24 to transmit diagnostic and configuration information include those disclosed in U.S. patent application Ser. No. 11/134,786 filed May 20, 2005; U.S. patent application Ser. No. 11/204,920 filed Aug. 15, 2005; U.S. patent application Ser. No. 11/344,883 filed Feb. 3, 2006; U.S. patent application Ser. No. 11/348,745 filed Feb. 7, 2006; U.S. patent application Ser. No. 11/279,360 filed Apr. 11, 2006; U.S. patent application Ser. No. 11/413,829 filed Apr. 28, 2006; U.S. patent application Ser. No. 11/537,602 filed Sep. 29, 2006; U.S. patent application Ser. No. 11/537,590 filed Sep. 29, 2006; U.S. patent application Ser. No. 11/537,599 filed Sep. 29, 2006; U.S. patent application Ser. No. 11/537,595 filed Sep. 29, 2006; U.S. patent application Ser. No. 11/685,548 filed Mar. 13, 2007; U.S. patent application Ser. No. 11/685,551 filed Mar. 13, 2007; and U.S. patent application Ser. No. 11/744,591 filed May 4, 2007.
Referring to FIG. 2 , the network 10 may have a “ring” configuration, in which the transmit port 26 of a transceiver module 14 a , for example, is coupled to the receive port 28 of a transceiver module 14 d and the receive port 28 of the transceiver module 14 a is coupled to the transmit port 26 of a transceiver module 14 b . In this manner, data must be circulated through a number of intervening transceiver modules 14 a - 14 d before reaching a destination module 14 a - 14 d . For example, in order to transmit data from transceiver module 14 a to transceiver module 14 b , the data must be transmitted through modules 14 d and 14 c.
Referring to FIG. 3 , in some embodiments, the network 10 may have a “star” configuration, in which both the transmit port 26 and receive port 28 of each transceiver 14 a - 14 d is coupled to a corresponding transmit port 26 and receive port 28 of a hub 30 . The hub 30 routes signals to the receive port 26 of the destination network device 14 a - 14 d . In this manner, data needs to travel through at most one other device before reaching a destination device 14 a - 14 d.
Referring to FIG. 4 , in some embodiments, a network 10 is arranged in layers in which a network device 12 a of layer 0 includes a plurality of modules 14 a - 14 c each coupled to modules 14 a - 14 c of network devices 12 b - 12 c in layer 1 . The network devices 12 b - 12 c further include modules 14 a - 14 c that are part of layer 2 coupled to modules 14 a - 14 c of network devices 12 d - 12 f defining a layer 3 , and so on. It is readily apparent that some network devices include modules 14 a - 14 c belonging to two different layers. The network devices 12 a - 12 c may control routing of data through the network. For example, the network devices 12 a - 12 h may be embodied as routers or switches for directing network traffic.
In some embodiments, modules 14 a - 14 c in a first layer are able to communicate with modules 14 a - 14 c of a second layer that are coupled to the same network device 12 a - 12 f by means of a host bridge 32 . The host bridge transfers module data 20 from one module 14 a - 14 c to another, in the same or a different layer, that are coupled to the same network device 12 a - 12 f . In some embodiments, a module 14 a - 14 c may set a bit in data output to the network device 12 a - 12 f to which it is coupled indicating that it has module data 20 to transmit to another module 14 a - 14 c . The network 12 a - 12 f may then read the module data 20 and transfer it to another module 14 a - 14 c coupled thereto. The network device 12 a - 12 f may transfer the data by setting a bit in data provided to the destination module 14 a - 14 c indicating that module data 24 is available to be input to the destination module 14 a - 14 c . The destination module 14 a - 14 c may then store data received as module data 20 , rather than transmitting it over the data channel 18 .
Communications between modules 14 a - 14 c included in any of the foregoing, and other, network configurations may follow a protocol accommodating different capacities of modules 14 a - 14 c . Communications may include packets of data having fields described in Table 1, below.
TABLE 1
Data Packet Field Definitions
Field
Bits
Description
Preamble
8
To inform other device that something will be sent
Lock
3
To allow other device to lock on start of sequence
Communication Type
8
0x01 = Knock Knock
(CT)
0x02 = Acknowledge
0x03 = Command/system address = 16 bits
0x04 = Response 16 bits
0x05 = Communication Corrupted
0x06 = Communications stopped
0x07 = Command/system address = 32 bits
[0x08-0x0F = cross fabric communications for ring
or star networks]
0x051 = Mass Error Alert (See FIG. 7)
Communication
8
Originator creates this starting as a random number.
ID (C-ID
Respondent returns this same number. Originator
increments number for each next communication it
originates
Sync
8
Alternate bits (01010101) to verify that no bits have
been dropped such that data is now in the wrong
place
Command ID
8
See Table 2
(CMD)
System Address
Depends
CT = 0x03 -- 16bits
on CT
CT = 0x07 -- 32 bites
Length
Depends
CT = 0x00 -- 0x10
on CT
CT = 0x0A through 0x FF -- Not yet defined
Data Bytes
Depends
on
Length
Sync
8
Alternate bits to verify that no bits have been
dropped such that data is now in the wrong place
(01010101)
Status/
16
Status of response 0x0000 - OK
Contingency
Other Values - error type
Extended Status/
16
Extended status of response.
Contingency
Meaning of value depends on Status (error
messages, version information, contingency
instructions,)
Wrapper Count
16
Wrapper = Number of Communication IDs
(WC)/Layer
included in wrapper when communicating across a
network fabric
Layers = a layer count incremented for each layer
across which the data packet is transmitted. May be
negative depending on the location of module
originating a data packet in relation to the module
that initiated communication.
Wrappers/Layers
(depends
Wrappers = Communication IDs are placed in this
on WC)
field as a data packet is passed along the fabric,
creating a trail describing the network.
Layer = depends on layer of originating module.
The layer field does not change as the data packet is
forward along the fabric. Layer may be negative
where the module originating the message has a
lower layer number than the module that initiated
communication.
Communication
3
Signals communication is over
Complete
The Preamble field contains a sequence of bits that communicate to a receiving transceiver that a data packet is being sent. The Preamble field may be any sequence of bits that serves this function. The Lock field includes a sequence of bits enabling a receiving transceiver to lock onto the start of the sequence. The Lock field may enable the receiving transceiver to recognize the starting bit of the data packet. The Lock field may also enable a clock data recovery (CDR) circuit to generate a clock signal synchronous with bit transitions within data packet.
Sync Fields are provided at one, two, or more positions within the packet. The Sync Fields may include alternating bits, i.e., 10101010, to enable the receiving transceiver to evaluate whether received bits are properly positioned. For example, if the receiver had shifted one bit position out of synchronization, then evaluation of the Sync Fields would enable detection and correction of the error. The final field of the data packet may be a Communication Complete Field, which contains a data code indicating to the transceiver that the complete data packet has been received.
The Communication Type field defines how subsequent fields of the data packet will be interpreted. In particular, the number of fields in the packet may be different depending on the Communication Type field.
In a first example, the Communication Type field defines the number of bits that are used to define the address field in a read or write command. As noted in Table 1, where the Communication Type field is equal to 0x03, a following Command/System Address field has a length of 16 bits. When the Communication Type field is equal to 0x07, a following Command/System Address field has a length of 32 bits. Other values for the Communication Type field may define other lengths for the Command/System Address field.
In some embodiments, the Communication Type field also communicates information to set up and provide feedback regarding a connection between transceivers. For example, a value of 0x01 may indicate that a data packet is a Knock Knock command instructing the receiving transceiver to respond with a packet having a Communication Type field equal to 0x02, which corresponds to an Acknowledge message.
In some embodiments a value of 0x05 indicates that communication between the transceivers has become corrupted and a value of 0x06 indicates that communication has stopped. The definitions for values of the Communication Type field are exemplary and may be assigned arbitrarily.
The Communication ID field identifies the data packet. Upon generating a data packet, the sending transceiver will insert a random string of bits in the Communication ID field. The receiving transceiver will use the same Communication ID in its response. The sending transceiver may then increment the Communication ID and use the incremented value in the next communication. In some embodiments, the value for the initial Communication ID is taken from the transceivers “live data” which refers to measured parameters regarding optical data transmitted from and received by the transceiver, such as output power, received power, temperature, and the like.
The communication identifier used by the requestor can also be used as an encryption seed for a command or response to a communication in addition to public and private keys known to the transmitting and receiving module. For a subsequent command or response the encryption seed may be based on the next random Communication identifier. The random number may be seeded by a byte of the live data, which tends to be random.
Exemplary values for the Command Identifier field are summarized in Table 2. As is apparent in Table 2, the function associated with values of the Command Identifier field is dependent on the value of the Command Type field. The function and number of subsequent fields in the data packet may be dependent on the Command Type and Command Identifier fields.
TABLE 2
Command Descriptions
Communication
Type
Command
Description
Fields
0x01
0x00
Knock knock
C-ID/Sync/CMD/status/extended
status/checksum/communication
complete
0x01
0x01
Knock knock
C-ID/Sync/CMD/status/extended
status/layer
count/layer/checksum/communication
complete
0x02
0x00
Acknowledge
C-ID/Sync/CMD/status/extended
status/checksum/communication
complete
0x02
0x01
Acknowledge
C-ID/Sync/CMD/status/extended
status/layer count/layer/
checksum/communication complete
0x03
0x01
Read request
C-ID/sync/CMD/system address 16
bits/length/sync/
contingency/extended
contingency/checksum/
communication complete
0x03
0x02
Write request
C-ID/synclCMD/system address 16
bits/length/data
bytes/sync/contingency/extended
contingency/checksum/
communication complete
0x04
0x01
Read response
C-ID/sync/CMD/system address 16
bits/length/data bytes/sync/status/
extended status/checksum/
communication complete
0x04
0x02
Write response
C-ID/sync/CMD/system address 16
bits/length/sync/status/extended
status/checksum/communication
complete
0x05
0x00
Sync byte out of
C-ID/sync/CMD/status/extended
place
status/checksum/communication
complete
0x05
0x01
Checksum
C-ID/sync/CMD/status/extended
problem
status/checksum/communication
complete
0x06
0x00
Not receiving
C-ID/sync/CMD/status/extended
out-of-band
status/checksum/communication
complete
0x06
0x01
Not receiving
C-ID/sync/CMD/status/extended
data
status/checksum/communication
complete
0x07
0x01
Read request
C-ID/sync/CMD/system address 32
bits/length/sync
contingency/extended
contingency/checksum/communication
complete
0x07
0x02
Write request
C-ID/sync/CMD/system address 32
bits/length/sync/contingency/extended
contingency/checksum/communication
complete
0x08
0x01
Read Response
C-ID/sync/CMD/system address 32
bits/length/data
bytes/sync/status/extended
status/checksum/communication
complete
0x08
0x02
Write Response
C-ID/sync/CMD/system address 32
bits/length/sync/status/extended
status/checksum/communication
complete
Referring to FIG. 5 , a method 40 may be used for initiating communication between a transmitting module and a receiving module. The method 40 may include evaluating whether a Knock Knock message has been received recently at step 42 . If so, in order to prevent a storm of Knock Knock messages, the transmitting module may suppress sending of a Knock Knock command for a waiting period at step 44 . Step 42 may then be repeated. If at step 42 no Knock Knock message has been received, step 46 may be executed by transmitting a Knock Knock message to the receiving module. Step 46 may include transmitting a Knock Knock message directly to the receiving module without any instruction to pass it on to another module. For the example commands of Table 2, this may be accomplished by transmitting a data packet having CT=0x01 and CMD=0x00.
At step 48 , the method 40 includes evaluating at the transmitting module whether a response has been received at the receiving module. A response may include an Acknowledge message including data packet having CT=0x02 and CMD=0x00 as illustrated in Table 2. If a response is received at step 48 , then the network type is point-to-point wherein the transmitter and receiver of the transmitting module are coupled to the receiver and transmitter, respectively of the receiving module. Step 50 may therefore include recording this fact within the transmitting module, such as by setting a Network Type variable or setting to a value corresponding to a point-to-point network, such as a value for a layer count of the network equal to 1 or 0 indicating a point to point connection.
If no response is received at step 48 , then step 52 is performed, which includes sending a Knock Knock message that instructs the receiving module to retransmit the message. The Knock Knock message may further instruct N subsequent receiving modules to retransmit the message. For example, the transmitting module may transmit a message having CT=0x01 and CMD=0x01. As noted in Table 2, this command includes Layer Count and Layer fields. The Layer field may indicate the number of times that the message is to be re-transmitted. The Layer count may indicate to a receiving module how many times the message has already been retransmitted. The receiving module, and any subsequent receiving module, may then compare the Layer Count to the Layer field, if the layer count is less than the layer field, then the module will increment the layer count and retransmit the message. Step 52 may include setting the Layer field to an initial value N, such as 10, or some other value.
In some embodiments, the Layer Count and Layer field relate to Wrappers, rather than layers. For some communications, a receiving module will generate a data packet, or wrapper, having a received data packet embedded therein, such as in the Data field. In such embodiments, the Layer Count field indicates the number of wrappers in the data packet. In such instances the Layer field indicates the number of wrappers at which the original data packet has reached its destination. In some embodiments, the wrappers may be used to conduct fabric discovery as each intervening module that receives a discovery request adds a wrapper that may include a unique Communication ID, and perhaps other data such as the live data of the intervening module. The final wrapper will therefore contain data from each of the intervening modules. Alternatively, wrappers may consist only in addition of a module identifier or communication ID into the wrapper field. A module forwarding a data packet with a wrapper may also increment the wrapper count field.
Step 54 may include evaluating at the original transmitting module whether a response has been received. The response may include one of the Acknowledge messages outlined in Table 2. A response may be received from a transceiver having its transmit port coupled to the receiver port of the original transmitting module.
If a response is received at step 54 , then the network is a ring network wherein the transmitter and receiver of the transmitting module are coupled to the receiver and transmitter of different modules, such as is illustrated in FIG. 2 . Step 56 may therefore include recording this fact within the transmitting module, such as by setting a Network Type variable or setting to a value corresponding to a ring network. Step 56 may also include noting that the number of layers in the ring network is equal to the value of the Layer field in the Knock Knock message sent in the last iteration of step 52 .
If no response has been received at step 54 , then step 58 may be performed which includes comparing the value of the layer field from step 52 (or previous iteration of step 64 described below) to determine whether it exceeds an L MAX value. If it does, then step 60 includes recording within the original transmitting module that the network is a star type.
If the value of the layer field from step 52 (or a previous iteration of step 64 described below) does not equal or exceed the L MAX value, then the layer field is incremented by an increment amount D, such as 1, 5, 10, or some other value at step 62 . Inasmuch as a ring networks typically do not have more than twenty layers, L MAX may be equal to 20 in some embodiments. At step 64 , another Knock Knock message is transmitted having the Layer field equal to the incremented value calculated at step 62 . Step 54 may then be repeated.
In many networks, transceiver modules are replaced one at a time as they begin to fail. Accordingly, newer transceivers will often be required to communicate with older transceivers with less functionality. Accordingly, the method 70 of FIG. 6 may be used to accommodate such differences.
In typical transceiver modules, data is accessed with reference to a table number and a position or “offset” within the table corresponding to the table number. The size of each table may vary depending on the amount of memory in the module and the standard or “multi-source agreement” (MSA) with which it complies. As standards develop, the type of data stored in each table may be augmented, but previously defined table locations are maintained the same. Accordingly, as table sizes increase, the initial storage locations in each table may conform to previous standards, whereas subsequent table locations contain other types of data defined by newer standards. Methods in accordance with embodiments of the present invention accommodate such table/offset standards, but are capable of use in the absence of such standards.
In one embodiment, the method 70 includes determining at 72 by a transmitting module the table/offset address of data that the transmitting module intends to write to or request from a receiving module as defined by a standard with which the transmitting programmed has been programmed to comply.
At step 74 , the transmitting module translates the table/offset address into a system address. The division of transceiver memory into tables is typically logical and the data is actually stored in random access memory embodied as an undifferentiated array of memory locations 0-N. Accordingly, the table/offset address may be mapped to a specific memory location referred to as a system address. For example, where a transceiver has tables of 256 bytes, table 0/offset 124 , may be mapped to system address 124 , whereas table 1/offset 124 may be mapped to system address 380 .
At step 76 , a Read or Write request is transmitted to a receiving module. The request may include data packet having CT=0x03 and CMD=0x01 (16 bit read request), CT=0x03 and CMD=0x02 (16 bit write request), CT=0x07 and CMD=0x01 (32 bit read request), CT=0x07 and CMD=0x02 (32 bit write request) as defined by Table 2. The request may also include some other Read or Write request that define layer and layer count fields in order to address a transceiver other than to which the transmitting receiver is immediately coupled.
A read request preferably includes a Command Type (CT) field that defines the system address length (e.g. 16 or 32 bits). The read request may also indicate the system address calculated at step 74 in the System Address field and the length of requested data in the Length field. In some embodiments of the invention, the read request also stores the table size of the transmitting module in the Status/Contingency field. A write request may additionally include data stored in the Data field to be written in the memory of the receiving module. In a write request, the Length field may refer to the number of bytes included in the Data field, or the number of address locations occupied by the data included in the Data field
At step 78 , the read or write request is received. At step 80 , the receiving module evaluates whether it recognizes the Command Type field. Where the receiving module is older than the transmitting module, the Command Type field may not be recognized. If the command type is not recognized, then step 82 may be executed, which include sending an error message, which may be embodied as a data packet having the Extended Status field storing an identifier of the protocol version of the receiving module. On receiving the error message the original transmitting module may transmit subsequent Read and Write requests that conform to the protocol indicated in the error message.
If the command type is recognized, then step 84 may be executed, which includes determining whether the table size stored in the Status/Contingency field of the read or write request is the same as that of the receiving module. If they are the same, then the method 70 may include sending the data stored at the system address of the receiving module indicated in a read request or writing data to the system address indicated in a write request at step 86 .
If the table sizes are not the same, then at step 88 the system address of the read or write request may be translated into a table and offset of the transmitting module using the table size stored in the Contingency field of the read or write request. At step 90 , the receiving module evaluates whether it has sufficient memory to read or write the amount of data specified in the Length field beginning at the table/offset determined at step 88 . If it does, then the requested data may be transmitted to the transmitting module or written to the memory of the receiving module at step 86 .
If the receiving module is found not to have sufficient memory, then the Extended Contingency field of the read or write request may be examined at step 92 . If the Extended Contingency field contains a value instructing the receiving module not to truncate its response, then an error message is sent at step 94 with an Extended Status field storing the table size of the receiving module. If the Extended Contingency field does not instruct the receiving module not to truncate its response, then the value of the Length field of the read or write request is truncated at step 96 and the truncated amount of data is either transmitted to the original transmitting module or written to the receiving module at step 98 according to the table/offset calculated at step 88 . Step 98 may include transmitting a Write Response or Read Response (see Table 2) having an Extended Status field storing the table size of the receiving module. In some embodiments, where the receiving module has a larger memory or at least a larger table size, the receiving module will analyze the table size in a received read or write request and transmit only data in tables up to the table size of the transmitting module to the receiving module. For example, if the transmitting module has a table size of 128 and the receiving module has a table size of 256, then the receiving module may respond to a request for data in table 1, for example, by sending only 128 bytes of data therefrom.
Referring to FIG. 7 , in some embodiments a network device 12 a - 12 b may cooperate with a plurality of transceiver modules 14 a - 14 b coupled thereto to control the amount of out-of-band data transmitted across the network fabric according to a method 100 . At step 102 a first transceiver module receives an error message from another transceiver module in the fabric. At step 104 , the first transceiver module examines the Command Type field of the error message. If the Command Type is a value corresponding to a high priority error, designated here as RED ALERT, then the first transceiver module suppresses any error messages for a wait period at step 106 .
If the error message is found not to be a RED ALERT, then the first transceiver module notifies the host network device to which it is immediately coupled that it has an error message to transmit at step 108 . At step 110 , the host network device evaluates whether other transceiver modules to which it is immediately coupled have provided notice of pending error messages. If so, then the host network device instructs the first transceiver module to suppress the error message at step 112 for a wait period. If not, then the host network device instructs the first transceiver module to transmit the error message at step 114 . The first transceiver module then transmits the error message at step 116 .
Referring to FIG. 8 , while referring again to FIG. 4 , the host network devices 12 a - 12 f may facilitate discovery of the fabric layout according to a method 118 in order to facilitate out-of-band communication between transceiver modules 14 a - 14 c of different layers. In some embodiments, one of the network devices, such as network device 12 a may be designated a listening portal to which fabric layout information will be transmitted.
The method 118 may include evaluating at step 120 at an individual transceiver module whether a discovery request has been received from another transceiver module. If so, then the individual transceiver module may suppress discovery requests indefinitely, or for a wait period, at step 122 in order to avoid generating undue chatter. If a discovery request has not been received, then at step 124 , the individual transceiver module will discover modules to which it is connected. Step 124 may include sending Knock Knock messages according to the method of FIG. 5 . The individual transceiver module may then evaluate responses to determine which transceiver modules it is connected to. Step 124 may include sending a message instructing other modules to add a wrapper and/or other data to the message and retransmit, such that when a response circulates back to the individual transceiver module over a ring network, for example, it will contain data regarding all intervening modules. Step 124 may include discovery conducted without involvement of any network devices hosting the modules.
At step 126 , the individual transceiver module transmits a discovery request to the network device to which it is immediately coupled. At step 128 , the individual transceiver module also transmits connection information determined at step 124 to its host network device. At step 130 , the host network device transmits a fabric discovery request to other network devices. The request may be transmitted in-band rather than out-of-band. Upon receiving the discovery requests, the other network devices may transmit discovery requests to transceiver modules that they host at step 132 . In response to step 132 , the transceiver modules will discover out-of-band module connections at step 134 , such as by sending Knock Knock messages according to the method of FIG. 5 or as described with respect to step 124 and evaluating responses to determine which transceiver modules it is connected to.
At step 136 , the transceiver modules of steps 132 and 134 will transmit the connection information from step 134 to the host network device to which they are immediately coupled. At step 138 , the network devices transmit the connection information collected at step 136 to the listening portal. At step 140 , the listening portal assembles the information transmitted from the network devices during step 138 into a description of the network fabric. At step 142 , the listening portal broadcasts the fabric description to the network devices. Step 142 may include transmitting the data in-band rather than out-of-band. At step 144 , each network device may transfer all or part of the fabric description to transceiver modules that it hosts.
Referring to FIG. 9 , while also referring to FIG. 4 , in some embodiments, communication in an OOB channel 24 may be used to detect unauthorized intrusion in a network. For example, a tap may be placed on an optical link 150 between transceiver module 14 c of layer 2 hosted by network device 12 c and the transceiver module 14 b of layer 3 hosted by network device 12 g . Alternatively, one of the modules 14 c and 14 b coupled to link 150 may be replaced by an unauthorized transceiver.
Accordingly, the method 152 of FIG. 9 may be used to detect the intrusion and reroute data, such as over link 154 between module 14 a of layer 2 hosted by network device 12 c and module 14 b of layer 3 hosted by network device 12 e.
At step 156 , the method 152 includes evaluating whether a break in communication in the OOB channel has occurred. If so, then one or both of the modules 14 c and 14 b coupled to link 150 will notify the listening portal 12 a of the breach at step 158 . Notification may include providing notice to one or both of the network devices 12 c and 12 g of the breach, which may then provide notice to the listening portal 12 a either through the data channel 22 or the OOB channel through one of the other modules hosted by the network devices 12 c and 12 g.
At step 160 , the method includes evaluating whether a transient interruption in the optical connection between a transmitting module and a receiving module has occurred. If not, communication of data continues at step 162 . If so, then step 164 includes evaluating whether an input to the transmitting module was interrupted. If so, then transmission continues at step 166 . If not, then step 168 includes evaluating whether a drop in received optical power followed the transient interruption. If not, then transmission continues at step 166 . If so, then step 170 includes evaluating whether the transmitting module has reduced its transmit power, such as by inquiring over the OOB channel 24 whether a drop has occurred. If so, then transmission of data continues at step 162 . If not, then step 172 includes the transmitting module raising its output power by X decibels. At step 174 , the receiving module evaluates whether more than Y % of the X decibel increase has been detected. The transmitting module may communicate the value of X to the receiving module by means of the OOB channel 24 . The value of Y may be 90, 80, or some other value. If more than Y % of the X decibel increase is detected, than at step 162 , data transmission continues. If not, then at step 176 , the receiving module notifies its host network device that a security breach has occurred. At step 178 , the network device hosting the receiving module takes steps necessary to route data through an alternate link. For example, if link 150 is found to be compromised, data may be routed through link 154 instead. At step 180 , the transmitting and receiving module may begin to either encrypt data communicated therebetween or send random data. At step 182 a listening portal may be notified of the security breach by one or both of the network devices hosting the transmitting and receiving modules.
The present invention may be embodied in other specific forms without departing from its spirit or essential characteristics. The described embodiments are to be considered in all respects only as illustrative and not restrictive. The scope of the invention is, therefore, indicated by the appended claims rather than by the foregoing description. All changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
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Methods for managing an optical network through out-of-band communication between optical transceiver modules in a heterogeneous network fabric are disclosed. The disclosed methods include methods for performing fabric discovery, communicating error messages, detecting intrusion. Methods are also disclosed for communicating between transceivers of differing protocol versions and memory capacity.
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FEDERALLY SPONSORED RESEARCH AND DEVELOPMENT STATEMENT
This invention was not developed in conjunction with any Federally sponsored contract.
CROSS-REFERENCE TO RELATED APPLICATIONS (CLAIMING BENEFIT UNDER 35 U.S.C. 120)
This application is related to U.S. patent application, Ser. No. 10,715,258, filed on Nov. 17, 2003, by John Parker Burg.
MICROFICHE APPENDIX
Not applicable.
INCORPORATION BY REFERENCE
This application is incorporated by reference related patent application, Ser. No. 10,715,258 in its entirety.
BACKGROUND OF THE INVENTION
The fitting-out of occupiable space is continuously becoming more important and ever more challenging for those utilizing modem office buildings, business and conference centers, hotels, classrooms, medical facilities, and the like. In the competitive business environment, cost concerns alone often dictate the efficient use of interior space. Thus, the finishing or fitting-out of building spaces for offices and other areas where work is conducted has become a very important aspect of effective space planning and layout.
Business organizations, their work patterns and the technology utilized therein are constantly evolving and changing. Building space users require products that provide for change at minimal cost. At the same time, their need for functional interior accommodations remains steadfast. Issues of privacy, functionality, aesthetics, acoustics, etc., are unwavering. For architects and designers, space planning for both the short and long term is a dynamic and increasingly challenging problem. Changing work processes and the technology required demand that designs and installation be able to support and anticipate change.
Space allocation and planning challenges are largely driven by the fact that modern office spaces are becoming increasingly more complicated due to changing and increasing needs of users for more and improved utilities support at each workstation or work setting. These utilities encompass all types of resources that may be used to support or service a worker, such as communications and data used with computers and other types of data processors, telecommunications, electronic displays, etc., electrical power, conditioned water, and physical accommodations, such as lighting, HVAC, sprinklers, security, sound masking, and the like. For example, modern offices for highly skilled “knowledge workers” such as engineers, accountants, stock brokers, computer programmers, etc., are typically provided with multiple pieces of very specialized computer and communications equipment that are capable of processing information from numerous local and remote data resources to assist in solving complex problems. Such equipment has very stringent power and signal requirements, and must quickly and efficiently interface with related equipment at both adjacent and remote locations. Work areas with readily controllable lighting, HVAC, sound masking, and other physical support systems, are also highly desirable to maximize worker creativity and productivity. Many other types of high technology equipment and facilities are also presently being developed which will need to be accommodated in the work places of the future. Moreover, the office space layout of these “knowledge workers” changes frequently to accommodate new technology, or to accommodate changing work teams resulting from changing business objectives, changing corporate cultures, or a combination thereof.
Office workers today need flexible alternative products that provide for the obtainment of numerous, often seemingly conflicting objectives. For example, the cultural aims of an organization may require the creation of both individual and collaborative spaces, while providing a “sense of place” for the users, and providing a competitive edge for the developer. Their needs include a range of privacy options, from fully enclosed offices which support individual creative work to open spaces for collaborative team work. At the same time, their products must be able to accommodate diverse organizations, unique layout designs, and dynamic work processes.
Further compounding the challenge are the overall objectives to promote productivity, minimize the expenses of absenteeism and workforce health insurance, and reduce potential liability. Meeting these objectives often requires improved lighting, better air quality, life safety, and ergonomic task support.
As previously mentioned, the cost efficient use of building floor space is also an ever-growing concern, particularly as building costs continue to escalate. Open office plans that reduce overall office costs are commonplace, and generally incorporate large, open floor spaces. These spaces are often equipped with modular furniture systems that are readily reconfigurable to accommodate the ever-changing needs of specific users, as well as the divergent requirements of different tenants. However, for privacy, productivity, or other reasons, interior walls and/or partitions are still required although the functionality requirements of interior walls is changing.
Historically, office walls or partitions are made by erecting a wood frame comprising vertical studs spaced on a regular interval, lining each side with gypsum board (sheet rock) panels, then finishing the wall surfaces with a variety of textures and paint. When additional thermal and/or acoustic insulation is needed, insulation medium such as fiberglass, rock wool or mineral wool will commonly be placed to fill the interior space between vertical studs and gypsum board panels.
These conventional walls have proven sturdy, provide adequate privacy and sound proofing, and provide a surface that easily accepts wall hangings such as pictures, paintings, plaques and the like. Furthermore, as is commonly known, conventional walls can easily be repainted, retextured, and readily patched and repaired when damaged. Conventional gypsum board partitions are typically custom built floor-to-ceiling installations that, due primarily to the vertical studs, are time-consuming to erect and build. The increased need for utility wiring, such as power and communication cables, have made conventional vertical stud-based walls more cumbersome and inconvenient as horizontal paths for the utility wiring must be routed either through numerous vertical studs or up and into a ceiling passage or plenum, then back down and to the end location.
As stated, interior walls in offices, hotels and the like are typically made by erecting a frame that includes vertical studs, either wood or steel, on a 16″ or 24″ spacing, lining each side with gypsum board (sheet rock) panels, then finishing the wall surfaces with a variety of textures and paint. FIGS. 1 a - 1 d illustrate a cross-sectional top-down view of such constructions.
FIG. 1 a shows a wall construction 100 comprised of vertical 2×4 studs 102 lined on each side by ⅝″ gypsum board 101 with empty space 103 therebetween. FIG. 1 b shows a wall construction 200 comprised of vertical 2×4 studs 202 lined on each side by ⅝″ gypsum board 201 with insulation 203 filling the interior space.
FIG. 1 c shows a wall construction 300 comprised of 3½″ vertical steel studs 302 lined on each side by ⅝″ gypsum board 301 . FIG. 1 d shows a wall construction 400 comprised of 3½″ vertical steel studs 402 lined on each side by ⅝″ gypsum board 401 with insulation 403 filling the interior space.
For the primary objective of increasing the sound attenuating properties of walls, numerous alternative practices have been used. FIGS. 1 e - 1 g provide top-down cross-sectional views of alternative constructions.
FIG. 1 e shows a wall construction 500 wherein vertical 2×4 studs 502 are placed in a staggered configuration such that no direct rigid connection is made between gypsum board panels 501 lining each wall face. Insulation 503 is used to fill interior spaces.
FIG. 1 f shows a wall construction 600 wherein vertical 2×4 studs 602 are placed in a two-wide configuration effectively doubling the overall wall thickness. Gypsum board 601 lines each face and insulation 603 fills interior spaces.
FIG. 1 g is similar to FIG. 1 f except the two-wide 2×4 studs are replaced by 7″ steel studs 702 and two layers of gypsum board 701 are used on one side. Insulation 703 is used to fill interior spaces. The wall construction of FIG. 1 g , by way of the double layer of gypsum board on one face provides a one hour fire rating as required by many commercial applications such as hotel constructions.
Based upon the state of the art as described in FIGS. 1 a - 1 g , a wall construction is needed that effectively utilizes the favorable structural and acoustic properties of superior construction materials, namely compressed straw panels discussed infra, and preferably construction materials made primarily from recovered or otherwise discarded materials. Further, what is needed in the art is a wall construction method that is quicker and more cost effective to install than conventional wall constructions while providing easy routing and re-routing of increasing amounts of utility wiring and communication cables. Still further, what is needed in the art is a wall construction method that provides the flexibility and reconfigurability of currently available partial or full height partition systems while providing the sturdiness, sound attenuation and ease of resurfacing provided by conventional gypsum board walls. Finally, what is needed in the art is a wall construction that contains no exterior connectors such as nails, screws, and the like that require additional surface treatment to finish.
The current applicant's invention disclosed in pending U.S. patent application Ser. No. 10/715,258 provides a wall construction system that meets these stated needs of the art, while providing a system made primarily of recycled materials.
There further exists a need in the art, however, for a wall construction system and method that provides easy lateral movement of vertically oriented hat-channel studs while maintaining alignment along a wall line and which eliminates the need for a rigid attachment between the top and bottom of each hat-channel stud and the ceiling and floor respectively.
SUMMARY OF THE INVENTION
The present invention relates to the construction of interior and exterior walls and especially to the finishing or fitting-out of building space such as offices, hotels, conference centers, business centers, meeting rooms, medical facilities, classrooms, etc. Particularly, the present invention provides for the finishing out of open space using a system comprising a series of rails attached along a wall line to a ceiling and floor. Floor and ceiling rails are designed to hold a plurality of vertically oriented hat-channel shaped studs therebetween such that the studs are able to slide laterally along the wall line while being held between said floor and ceiling rails. Studs are laterally spaced at intervals approximately equal to the width of compressed straw building panels to be assembled thereon, but remain laterally moveable to provide for lateral adjustment as wall assembly proceeds. Compressed straw panels are attached to the studs in a specific systematic manner resulting a wall or partition that includes no exterior penetrations or connectors.
The result is a relatively seamless exterior surface that can be finished in a plurality of ways, but one that, if desired, can be utilized with minimal surface treatment. The finished wall is structurally strong, but substantially hollow, thus enabling very easy routing and re-routing of utility wiring there through. Said studs are provided with a plurality of horizontal opening through which utility wiring and communication cabling can easily be routed. Assembly is simple, fast and inexpensive relative to the construction of conventional interior walls primarily due to significant potential savings in labor costs. The features and advantages of the present invention will be further understood and appreciated by those skilled in the art by reference to the following written specification, claims, and appended drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention should be more fully understood when the written description is considered in conjunction with the drawings contained herein, wherein:
FIGS. 1 a - 1 g , provide illustrations of known wall construction methods.
FIG. 2 shows an isometric view of our sliding flanged stud and the associated floor and ceiling rails;
FIG. 3 a shows an isometric detailed view of our sliding flanged stud;
FIG. 3 b shows an isometric detailed view of our floor and ceiling rail;
FIG. 4 a shows an isometric view of our assembly comprising first and second sliding flanged studs properly positioned and held between a floor and ceiling rail;
FIG. 4 b shows a side view of our assembly comprising first and second sliding flanged studs properly positioned and held between a floor and ceiling rail;
FIG. 5 a shows an isometric sectional view of the assembly shown in FIG. 4 ;
FIG. 5 b shows the assembly of FIG. 5 a with a first strawboard panel attached;
FIG. 5 c shows the assembly of FIG. 5 b with a second strawboard panel attached;
FIG. 5 d shows the assembly of FIG. 5 c with a third strawboard panel positioned and illustrates the lateral adjustment of second sliding flanged stud;
FIG. 5 e shows the assembly of FIG. 5 d with a third strawboard panel attached;
FIG. 5 f shows the assembly of FIG. 5 e with a fourth strawboard panel attached;
FIG. 6 provides a top-down sectional detail of the connection between strawboard panels and flanged stud;
FIG. 7 provides an isometric view of two alternative embodiments of floor rail, ceiling rail and flanged stud;
FIGS. 8 a and 8 b provide isometric views of a third alternative embodiment of flanged stud; and
FIGS. 9 a and 9 b provide a side view and installation details of a third alternative embodiment of flanged stud.
DETAILED DESCRIPTION OF THE INVENTION
Though most of the background discussion, supra, implies an interior application, said construction is well suited for exterior wall constructions as well. In exterior applications, the hollow interior space may be used to contain supplemental thermal and/or acoustic insulation. Further, said compressed straw panels are well suited for accepting a variety of weather proof panels, coatings, or the like attached thereto.
The present invention preferably utilizes solid core compressed straw or strawboard panels comprised of a matrix of highly compressed straw, usually wheat, rice or other recovered agricultural straw, lined on all sides by paper or paperboard. Typically, the strawboard panels are made through a dry extrusion process wherein straw is compressed into a substantially flat continuous web, normally between 1½″ and 3½″ thick and between 40″ and 60″ wide. The continuous web is then cut into rectangular panels of various lengths. Panel length is easily varied. The compressed straw is arranged in layers with the straw fibers substantially parallel in orientation extending transversely across the strawboard panel from side to side when the strawboard panel is in a normal in-use orientation. Said strawboard panels are typically rectangular in shape, and for the purposes of this disclosure, will be oriented such that the longer edges are substantially vertical and the shorter edges are substantially horizontal. In this orientation, said straw fibers will assume a generally horizontal orientation. Said strawboard panels have a tackable surface, i.e., are suitable for securely accepting nails, tacks, screws and other connecting means for attaching and/or hanging items from the strawboard panel surfaces.
Further, surfaces of the strawboard panels are suitable for accepting surface texture, paint, wall paper, and other conventional wall coverings. Strawboard panels can be factory finished with surface texture, paint, wall paper and the like, or said surface treatments can easily be applied to a finished wall. Compressed strawboard panels are typically much thicker and stronger than gypsum board and possess higher nail pull values, thus providing nails, screws, or the like driven therein to support more weight than if driven into gypsum board. Additionally, said strawboard panels possess sound insulating properties superior to both conventional gypsum board walls and many currently available commercial interior partition systems.
Solid core strawboard panels further provide fire resistant properties superior to materials used in many presently available interior wall construction and partition systems. To enhance flexibility, these strawboard panels can be cut and formed in the field using conventional tools such as circular, saber or band saws, routers, drywall hand saws, utility knives and the like. Ideally, however, the wall will be designed so that field alteration of said strawboard panels is minimized, thus minimizing installation time and costs. In the preferred embodiment, strawboard panels manufactured by Affordable Building Systems of Texas are used.
Referring first to FIG. 3 a , a detailed isometric view of our flanged stud 5 is provided and is shown to comprise a large flange 10 and a small flange 11 in a substantially co-planar position and disposed about a spine channel 12 , said spine channel 12 comprising the entire portion of flanged stud 5 except large flange 10 and small flange 11 . As illustrated, each spine channel 12 is provided with a pair of laterally disposed rail guides 15 at each end. Both large flange 10 and small flange 11 are provided with a plurality of lag screw receivers 13 for accepting the shaft of a properly sized lag screw therein.
The relative dimensions of large flange 10 , small flange 11 and spine channel 12 are variable and can be changed to meet specific criteria such as wall depth. It should be noted that throughout this disclosure flanged stud 5 is shown as having a large flange 10 and a small flange 11 . This size differentiation is done largely for descriptive purposes, and said flanges can alternatively be the same size.
Flanged stud 5 is preferably made from 16 gauge steel, but alternately can be made from any material, metal or non-metal, that provides comparable strength and stiffness and preferably a comparable or higher melting temperature (˜2500° F.).
FIG. 3 b provides a detailed isometric view of ceiling rail 7 and floor rail 8 , each comprised of a first flange 16 , and second flange 17 , and a raised channel 18 disposed between said flanges. Said first flange 16 and second flange 17 are each preferably provided with a plurality of lag screw receivers 13 for accepting the shaft of a properly sized lag screw therein. It can be seen that ceiling rail 7 and floor rail 8 are identical pieces in opposite orientation and can be used interchangeably in a preferred embodiment. Both floor rail 8 and ceiling rail 7 are preferably made from 16 gauge steel, but can be made from any material, metal or non-metal, that provides comparable strength and stiffness and a comparable or higher melting temperature (˜2500° F.). The actual gauge needed will depend upon the specific application and may be heavier or lighter than 16 gauge.
FIG. 2 provides an isometric view of an assembly of a flanged stud 5 positioned between a floor rail 8 and a ceiling rail 7 . Flanged stud 5 is preferably provided with a utility opening 14 that allows for the routing of utilities such as power wiring and communication cables through the interior of a finished wall. Typically, each flanged stud 5 is provided with a plurality of utility openings 14 . FIG. 2 specifically illustrates the interaction between said rail guides 15 and raised channels 18 . Each rail guide 15 and raised channel 18 is designed and sized to provide component interaction that allows flanged stud 5 to slide laterally in a plane defined by the lateral center lines of opposed floor rail 8 and ceiling rail 7 , while preventing flanged stud 5 from moving out of said plane. Said plane then defines the centerline of the finished wall.
FIG. 2 further illustrates that the first flange 16 and second flange 17 of both the floor rail 8 and ceiling rail 7 are preferably sized so as to make a flush fit along the end of flanged stud 5 when each components are assembled. Each rail guide 15 is preferably sized to provide a horizontal clearance of approximately ¼″ between said rail guide 15 and each raised channel 18 properly positioned there through.
FIGS. 4 a and 4 b , respectively, provide isometric and side views of our new wall frame assembly comprising floor rail 8 , ceiling rail 7 and a first flanged stud 5 and second flanged stud 6 properly disposed therebetween.
FIG. 4 a further provides a view of first flanged stud 5 and second flanged stud 6 each provided with a plurality of utility openings 14 .
FIG. 4 b illustrates the contact and implied connection between floor rail 8 and floor 24 and between ceiling rail 7 and ceiling 23 . The respective connections between floor rail 8 and floor 24 and between ceiling rail 7 and ceiling 23 can be made by an number of suitable means such as screws, nails, bolts, anchor bolts, adhesive, etc., When an installation requires ceiling rail 7 to be attached to runner of a suspended ceiling or the like, a clip connection or the like may be used in place of screws or adhesive.
The step by step assembly of a wall according to the present invention is illustrated in FIGS. 5 a - 5 f which provide isometric sectional views of our wall assembly as it is being assembled. Note that the views provided in FIGS. 5 a - 5 f are sectional views, and the ceiling rail 7 as well as top of first and second flanged stud 5 , 6 and the top of each strawboard panel 1 , 2 , 3 , 4 are not shown.
In FIG. 5 a , floor rail 8 , first flanged stud 5 , and second flanged stud 6 are shown in assembled form. It can be seen that both first and second flanged studs 5 , 6 are preferably provided with a plurality of utility openings 14 and lag screw receivers 13 . The designed fit of raised channel 18 and rail guide 15 can also be seen. As previously stated, in the assembled form, i.e., a flanged stud is positioned between ceiling rail and a floor rail with raised channels residing in rail guides at both ends, said stud will be moveable laterally along a plane defined by the opposed ceiling and floor rails.
In FIG. 5 b a first strawboard panel 1 is shown positioned in substantially co-planar relation to the wall centerline and adjacent to the large flange 10 on first flanged stud 5 . Though not shown, first strawboard panel 1 is rigidly attached to said large flange 10 by means of screws, nails, or other penetrating connectors. In the preferred embodiment, said rigid attachment is made by means of 1½″ lag screws.
Referring to FIG. 6 which provides a top-down cutaway view of preferred strawboard panel-stud connections, the connection between first strawboard panel 1 and large flange 10 is shown. Attachment is made be means of a plurality of 1½″ lag screws 9 inserted through lag screw receivers 13 (not shown) and penetrating first strawboard panel 1 . Further, it is important that first strawboard panel 1 does not completely cover the outer face of large flange 10 so as to provide room for third strawboard panel 3 to contact a portion of large flange 10 when in abutted edge-to-edge relation to first strawboard panel 1 . Throughout this disclosure, lag screws are used for illustration and are the connector of choice, but nails or other suitable penetrating connectors may be used. Lag screws provide for easy disassembly of a wall with minimal damage to strawboard panels.
FIG. 5 c shows second strawboard panel 2 positioned in co-planar relation to first strawboard panel 1 and positioned adjacent to the outer face of spine channel 12 . A plurality of disc connectors 19 can be seen protruding from the edge of second strawboard panel 2 . Said disc connectors, disclosed in U.S. Pat. No. 6,634,077 and pending U.S. application Ser. No. 10/387,994 are preferably inserted in fitted receivers (not shown). FIG. 6 provides illustration of the arrangement between second strawboard panel 2 and spine channel 12 including rigid connection by means of a plurality of lag screws 9 inserted through lag screw receivers 13 (not shown) and penetrating second strawboard panel 2 to provide a rigid attachment thereto. It is important to point out here that second strawboard panel 2 preferably does not completely cover the outer face of spine channel 12 so as to leave room for a portion of fourth strawboard panel 4 . FIG. 6 also illustrates the connection between second strawboard panel 2 and fourth strawboard panel 4 by means of a plurality of disc connectors 19 .
FIG. 5 d shows third strawboard panel 3 properly positioned in co-planar and abutted edge to edge relation with first strawboard panel 1 and secured to small flange 11 of first flanged stud 5 by means of lag screws 9 . A primary feature of this invention is illustrated by the large inward-facing arrow adjacent to second flanged stud 6 , said arrow indicating that second flanged stud 6 can be laterally moved along floor rail 8 and ceiling rail 9 (not shown) into proper position for accepting connection to third strawboard panel 3 . FIG. 5 e then shows second flanged stud 6 in the desired lateral position for connection to third strawboard panel 3 . As with the other strawboard panels, the connection between third strawboard panel 3 and second flanged stud 6 is preferably achieved by means of a plurality of 1½″ lag screws inserted through lag screw receivers and secured within said third strawboard panel 3 .
FIG. 5 f shows fourth strawboard panel 4 properly placed in co-planar and abutted edge to edge relation to second strawboard panel 2 . A connection between fourth strawboard panel 4 and second flanged stud 6 is made by via a plurality of lag screws 9 positioned through lag screw receivers 13 located on the outer face of spine channel 12 of second flanged stud 6 . Connection between fourth strawboard panel 4 and second flanged stud 6 as well as the connection between second strawboard panel 2 and fourth strawboard panel 4 are illustrated in FIG. 6 . The connection between second strawboard panel 2 and fourth strawboard panel 4 is preferably achieved by means of a plurality of disc connectors 19 positioned within connector receivers located in the facing edges of second strawboard panel 2 and fourth strawboard panel 4 .
FIGS. 7 a and 7 b illustrate alternative embodiments of the ceiling rail 7 , floor rail 8 (not shown), and flanged stud 5 . FIG. 7 a illustrates an alternative ceiling rail 7 a which contains two raised flanges 18 a in lieu of raised channel 18 (not shown). Further, rail guides 15 (not shown) are replaced by two receiving slits ( 18 a ) positioned on the end of alternate flanged stud 5 a such that raised flanges 18 a can be slidably received therein. Also on flanges stud 5 a , utility opening 14 has been replaced by a non-rectangular alternate utility opening 14 a.
FIG. 7 b illustrates a second alternative ceiling rail 7 b comprising a raised channel 18 b with a substantially triangular cross section in lieu of the substantially rectangular shape in the preferred embodiment. Alternative rail guides 15 b located on the end of flanged stud 5 b are comparably shaped to slidably receive raised channel 18 b therein. Alternative utility openings 14 b are provided as small group of circular openings.
FIGS. 7 a and 7 b illustrate only the top portions of alternative flanged stud 5 a and 5 b , as well as only associated ceiling rails 7 a and 7 b , but it should be noted that for both alternative embodiments, as with the preferred embodiment, the ceiling and floor rails can be identical components and the rail guides provided on each end of flanges studs can be identical. Thus, FIGS. 7 a and 7 b effectively illustrate both the ceiling and floor rails as well as the rail guides located at both ends of each flanged stud.
FIGS. 8 a and 8 b illustrate additional alternative embodiments of flanged stud 5 . In both FIG. 8 a and FIG. 8 b anchor tab 25 is illustrated. Said anchor tab 25 is included to provide a convenient means for providing a secure attachment between the top of flanged stud 5 and ceiling rail 7 and between the bottom of flanged stud 5 and floor rail 8 . This feature allows for the flexibility of placing a flanged stud 5 in a predetermined position between ceiling rail 7 and floor rail 8 , then securing the stud in place by means of self-tapping screw 26 or comparable attachment means placed through said anchor tab 25 and secured to raised channel 18 portion of each ceiling rail 7 and floor rail 8 . Also illustrated in FIG. 8 a and FIG. 8 b , the ends of large flange 10 and small flange 11 each have been tapered 27 with said taper 27 increasing from center to edge. As illustrated in FIGS. 9 a and 9 b , said taper 27 provides for the placement of a flanged stud 5 in between a floor rail 8 and ceiling rail 7 by means of in-place lateral rotation after said stud has been properly positioned.
As noted supra, each rail guide 15 is preferably sized to provide a horizontal clearance between said rail guide 15 and horizontal edge of raised channel 18 portion of each floor rail 8 and ceiling rail 7 . Said horizontal clearance and flange taper 27 provide for an unencumbered in-place lateral rotation of flanged stud 5 .
The embodiments which have been shown and described are exemplary. Even though numerous characteristics and advantages of the present invention have been described in the drawings and accompanying text, the description is illustrative only, and changes may be made in the detail, especially in matters of shape, size, and arrangement of the parts without departing from the scope of the present invention.
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An improved wall and partition construction method that features use of no exterior panel attachment means, and which provides a finished wall with a substantially seemless outer surface. The improved wall is comprised of ceiling and floor rails attached along a top and bottom wall line, and a plurality of vertical studs, slidably disposed between the floor and ceiling rails. Vertical slidable studs each have a hat-shaped cross section and include a plurality of openings that provide a pathway for cables and wiring along the interior of a finished wall. Wall panels such as compressed straw panels are attached to the vertical studs in a slightly offset alternating manner such that each strawboard panel can be rigidly connected to a stud by a plurality of lag screws with each penetrating the strawboard panel from the inside so that the finished wall has no exterior penetrations.
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This application is a continuation of application Ser. No. 07/700,878, filed on May 10, 1991, now abandoned, which is a continuation of Ser. No. 405,325, filed on Sep. 11, 1989, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the use of tires after blowout or in case of significant loss of pressure. It proposes a safety support that is mounted on the rim, inside the tire, to take up the load in case of failure of said tire.
2. Background of the Related Art
Among the very many supports of this type, there can be cited French patent publication FR 2 297 738, which shows a support in two parts that can be mounted on a rim in a single piece, of the type having a mounting groove. There can also be cited United Stated patent publication U.S. Pat. No. 4,197,892 which shows a support to be used on a rim with a removable edge. The success of these supports remains extremely limited because when they fulfill their role of load relief support of the tire when it is failing, their intervention causes instabilities in the behavior of the vehicles and therefore a degradation of the road stability performance.
To eliminate this drawback, United States patent publication U.S. Pat. No. 4,461,333 proposes a support, one part of which is extended to hold the tread axially. This support provides good road stability performances but it is complex and therefore costly to produce, which limits its use.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a safety support for supporting the tread of a vehicle tire in case of loss of inflation pressure of the tire, whose cost is low.
It is a further object of the invention to provide such a safety support having a gradual intervention.
It is yet a further object of the present invention to provide such a safety support which imparts an excellent level of road stability.
It is yet another object of the present invention to provide a method for mounting such a safety support on a wheel.
According to the present invention, the above and other objects are achieved by a safety support for supporting the tread of a vehicle tire in case of loss of inflation pressure of the vehicle tire, comprising a base fixed to a rim of a wheel having means for mounting the wheel to a vehicle such that an inside axial side of the wheel faces toward the vehicle and an outside axial side of the wheel faces away from the vehicle. A substantially cylindrical top is normally positioned radially outside of the base in substantial axial alignment with the base and with an axis substantially coaxial with the wheel axis. The top is normally radially spaced from the base such that when the support is positioned within a tire mounted to the vehicle rim, a radial clearance exists between the top and the tire tread. A connection between the base and the top comprises means for permitting a relative movement between the base and the top. The connection joins the base at an outside axial side thereof and joins the top at an inside axial side thereof, relative to a plane perpendicular to the wheel axis and passing through an axial middle of the top. As a result, a resultant of forces acting on the top moves axially toward the inside side of the wheel during the relative movement of the top toward the base.
According to another feature of the invention, a method for mounting a safety support having a substantially Z shape to a vehicle wheel comprises the steps of fitting a top of the support in a tire, fixing a base of the support to the wheel rim, and mounting the wheel to a vehicle such that the joint between the support base and the connector between the base and a support top faces away from the vehicle.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a partial meridian sectional view of a tire assembly equipped with the safety support according to the invention;
FIG. 2 is an orthogonal detail of the safety support;
FIG. 3 shows performance differences as a function of the material used to make the support;
FIG. 4 illustrates the operation of a tire assembly equipped with the safety support, and
FIG. 5 schematically illustrates the deflection of the support in response to a radially inward force thereon.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIG. 1, there is seen a completely ordinary vehicle tire 1, comprising a tread 10, two sides 11 and two beads 12 for providing the mechanical connection of tire 1 to wheel 2 having lug holes 2a for attachment to a vehicle. The latter comprises a rim 20, one part 201 of which is removable by bolts (not shown) and another part 202 of which forms a single piece with disk 23 of wheel 2. Rim 20 comprises two seats 21 which taper radially outward.
Safety support 3, in this example, has the general shape of a "Z," seen in meridian section. It comprises three parts: a base 30, a substantially cylindrical top 31 which is normally coaxial with the wheel rotational axis O-I and in axial alignment with the base, and a connection 32 joined between base 30 and top 31. The angle between the base 30 and the connection 32 is a least 30°. The support is preferably unitarily formed of elastic material.
When this support 3 is pushed radially inward by a radial force thereon, the movement of top 31 (in relation to base 30) is in both the radial direction and the axial direction (with respect to the wheel axis of rotation), due to the "Z" shape of the support. That is, the top 31, as seen in meridian section, can be thought of (i.e., simulates) as pivoting around an instantaneous center of rotation C relative to base 30 and rim 20 in response to radial inward forces. Action-reaction forces, due to flexure of the support necessarily result in the top 31 remaining parallel to the axis of rotation (O-I) of wheel 2 due to road-tire contact.
Of course, neither the connection 32 nor the top 31 actually pivot about the center C. Instead, this flexure approximates a pivoting about an instantaneous center of rotation C. That is, as shown in FIG. 5 the resultant reaction force R causes flexure of the connection 32, much like a leaf spring flexes along its length. This flexure provides a movement equivalent to, or simulating, pivoting about a single point. Moreover, since the resultant reaction force R is axially spaced from the instantaneous center of rotation C by the distance d, a moment force acting around center C will cause the top 31, and so the resultant R, to move axially inward (in the direction I; see dash lines in figure). Of course, as the top 31 moves axially inwardly, the distance d becomes larger (d'), and so the value of this moment will increase for a given reaction force R, thereby causing an increase of the bending of the support 3 at a constant load.
Support 3 is not symmetrical, as seen in meridian section. Its operation is therefore different depending on the direction of its mounting on rim 20. In the remainder of the description, "axially inside" designates a side oriented toward the inside I of the vehicle (with reference to the mounting position of the wheel) and "axially outside" a side oriented toward the outside O of the vehicle.
It has been found that the performance with reference to the quality of the handling of the vehicle is very different (and more favorable) in one mounting direction versus the other, and that in the illustrated favorable mounting direction this performance is much better than what is obtained with known supports. For this reason, by use of the contact between tread 10 and top 31, it is proposed to design the support 30 so that the resultant R of the forces exerted on said top 31, which in the absence of disturbances extends approximately radially and is centered in the middle of top 31, passes axially inside the instantaneous center of rotation C of top 31 in relation to rim 20, so as to produce an axial reaction in the desired direction.
When taking up the load in case of failure of tire 1, said top 31 necessarily rests on rim 20 of wheel 2. Consequently, the base 30 assures the bonding with rim 20 and connection 32 therefore joins said base 30 axially toward the outer side O of the vehicle, to provide the desired offset for the instantaneous center of rotation C of top 31 in the desired direction. By "bonding" on the rim is meant a connection such that there is no relative movement between base 30 and rim 20. If necessary, base 30 is reinforced with circumferentially extending rings 300.
The Z shape is very advantageous because it makes it possible to offset as much as possible the meeting point between connection 32 and base 30. It also makes it possible to offset in the opposite direction, i.e., toward the inside of the vehicle, the meeting point between connection 32 and top 31. This arrangement has a tendency to move toward the inside of the vehicle, and so to the inside of C, the point of application of the resultant of the forces R acting on top 31, and therefore to increase the bending of support 3 at a constant load. This has a favorable effect on the handling of the vehicle during the intervention of support 3. The "Z" shape also results in a base 30 whose width in the axial direction corresponds to the available space between beads 12 of tire 1, which makes it possible for support 3 to fulfill also the "locking of beads 12" function, necessary when driving at reduced or zero pressure.
The material of the support should be elastic. The material chosen influences the flexibility of such a support 3 and therefore the gradualness of its intervention. Preferably, a polyurethane will be selected whose modulus of elasticity varies between 55 MegaPascal (curve I, FIG. 3) and 40 MegaPascal (curve II, FIG. 3), as measured on a test specimen with 2% extension and at 20° C.
EXAMPLE
Support 3 was made of polyester TDI 4,4'-methylene bis ortho chloroaniline. The combination of the shape described and of the selection of this material produced a deflection curve for a tire 1-support 3 combination as a function of the inflation pressure of tire 1, as shown in FIG. 4. Tire 1 was of the Michelin 165/65 SR 13 MXL type.
At nominal pressure (2 bar), the deflection of tire 1 resulting from a static load of 380 decaNewton, was 19 mm. At that time there was a clearance of 10 mm between top 31 and tread 10. This clearance disappeared when the tire pressure fell to a pressure of 1.1 bar, which provided the threshold of intervention of support 3. The very good flexibility of support 3 gave a very gradual variation in the slope of the deflection curve for pressure values less than 1.1 bar. At zero pressure, there was observed a deflection of the tire 1 plus support 3 unit that was equivalent to 37/75 mm. This corresponded to a radial inward movement of 8 mm for the top 31 of support 3, at which time it took up the entire load, and to an increase in compression of the rubber of tread 10.
FIG. 2 shows an optional feature wherein the radially outside face of top 31 comprises ribs 35 oriented approximately parallel to the axis of rotation of tire 1. In this example, the tread is reinforced, as is well known, by a belt having a length in the circumferential direction which is much greater than the circumferential length of top 31. The role of ribs 35 is to absorb the difference in circumference of top 31 and tread 10 by facilitating a relative sliding between the tread 10 and the top 31.
If ribs 35 are absent, the sliding friction produced between tread 10 and a smooth top 31 can also be tolerable, or else may be reduced by other palliatives known to a person skilled in the art.
Of course, it is necessary to perforate base 30 to make it possible for the inflation air to flow from valve 13 to tire cavity 14, or to provide any appropriate arrangement for this purpose. Apart from this perforation 36 and ribs 35, support 3 is a rotational solid produced by the rotation of the section appearing clearly in FIG. 1. However, this geometric feature is, of course, not limiting. Connection 32 could be provided by an assembly of individual arms. Base 30 could be only an extension of connection 32, the holding of beads 12 on their seats 21 being provided in another way. Base 30 could be designed to be mounted in a single piece rim via a mounting groove. Support 3 could be made in two or more pieces assembled inside the tire during mounting.
The details of implementation given in this description make it possible to produce a support 3 in a single piece, easy to release from the mold since there is no undercut, and which nevertheless is mounted very easily as follows: Support 3 is first made oval by extending it with a motor vehicle jack, or a specifically adapted extension cylinder, inside of it; support 3 is then introduced in the center of tire 1 by presenting it so that the major axis of the oval is approximately perpendicular to the median plane of said tire; the ovalization is freed; then an ovalization is caused whose major axis is parallel to the median plane of the tire, and is located inside of it; then, by a relative rotation of support 3 and tire 1, said support 3 is brought completely inside beads 12 and it is allowed to resume its natural circular shape; then the tire containing support 3 is attached on rim 20.
To illustrate the performance reached in road stability, a car was driven whose rear wheel on the outside of the turn was equipped with an assembly comprising support 3 as described above and a 165/65 SR 13 Michelin MXL tire at zero pressure. The test, consisting of making a turn with a radius equivalent to 40 m on a dry tarred pavement, gave the following results:
Speeds up to 60 km/hr were possible in the favorable direction of mounting and speeds only up to 50 km/hr were achieved with a support mounted on the wrong side, these speeds being reached at the limit of the side slip of the vehicle. During these tests, the tire 1 deflected according to curves I and II of FIG. 3 in response to loads applied thereto.
Obviously, numerous modifications and variations of the present invention are possible in light of the above teachings. It is therefore to be understood that within the scope of the appended claims, the invention may be practiced otherwise than as specifically described herein.
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A safety support for supporting the tread of a vehicle tire in case of theoss of inflation pressure of the tire has the shape of a Z. The base of the support is fixed to a wheel rim while the connector between the support base and the support top is oriented so as to join the base on a side thereof opposite that facing the vehicle to which the tire is mounted. The asymmetric shape of the support and its orientation produces improved stability upon intervention of the support.
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This is a continuation, of application Ser. No. 08/665,122, filed Jun. 14, 1996, U.S. Pat. No. 5,849,168.
BACKGROUND OF THE INVENTION
1. Field of The Invention
The present invention relates to golf balls having a cover and a core and to a method of coating the cover during or immediately following the molding of the cover material onto the core. The invention additionally relates to golf balls having a coated cover wherein the cover has external dimensions which correspond to the internal dimensions of the mold which adds dimples to the cover material.
1. Description Of The Prior Art
Conventional golf balls can be classified as one-piece, two-piece, and three-piece balls. One-piece balls are molded from a homogeneous mass of material with a dimple pattern molded therein. Two-piece balls are made by molding a cover about a solid core. Three-piece are typically, but not always wound balls which are made by molding a cover about a wound core. The core of a two-piece ball is typically formed of rubber and can be solid, semi-solid or have a liquid center. A wound core is prepared by winding a lengthy thread of elastic material about the rubber core described above. The wound core is then surrounded with a cover material. The more recent trend in the golf ball art is towards the development of multi-component golf balls such as balls having two or more cover layers, two or more core layers or both multiple core and multiple cover layers.
Golf ball covers are presently formed from a variety of materials, such as balata, SURLYN®, IOTEK® and polyurethane, depending upon the performance characteristics desired for the golf ball. One of the softest materials conventionally used to form golf ball covers is balata, which is the trans form of the 1,4-chain polymer of isoprene. For many years, balata was the standard cover stock material used in forming most golf balls. Balata covered balls are favored among professionals and more advanced amateur players because the softness of the cover allows the player to achieve spin rates sufficient to precisely control ball direction and distance, particularly on shorter approach shots.
However, because of its softness, balata is susceptible to cuts or other damage to the cover resulting from a "mis-hit" shot. Accordingly, harder, more durable cover materials, e.g., ionomer resins such as SURLYN®, have been developed which provide higher durability, but less spin and feel, than the balata balls. Resins such as SURLYN® are generally ionic copolymers of an olefin such as ethylene and a metal salt of an unsaturated carboxylic acid such as acrylic acid, methacrylic acid or maleic acid. Metal ions, such as lithium, zinc or sodium are used to neutralize some portion of the acidic groups in the copolymer resulting in a thermoplastic elastomer for use as a golf ball cover. Additionally, various softening comonomers such as n-butyl acrylate may be added during the ionomer manufacturing process to improve golf ball performance characteristics such as spin and feel. In the early 1980s, low modulus SURLYN® ionomers were introduced and subsequently utilized to impart more spin and an improved, balata-like feel to golf balls.
All golf balls, regardless of type, have an outer surface which contains a dimple pattern. As used herein, "dimples" refer the topical relief of the outer surface of the ball, typically depressions or indentations formed into to provide desired aerodynamic effects. However, the dimple pattern may comprise of any form of topical relief on the outer surface of the golf ball formed to provide a desired aerodynamic effect to the ball, including formations such as protrusions from the outer surface.
Further to the above, golf balls are provided in a variety of colors. Conventionally they are white, but they may be manufactured in essentially any desired color, including yellow, orange and pink. The color is imparted to the ball either by applying layers of paint to the outer surface of the cover or by incorporating a pigment directly into the cover composition. Typically, in a painted ball, a first primer layer is applied, followed by a second, finishing coat layer. After a ball has been provided with a color, identifying indicia such as a trademark, logo, identification number, model name or number and the like are hot stamped or pad printed onto the ball.
Golf balls must be capable of withstanding a variety of weather conditions such as strong sunlight, extreme temperature ranges, and immersion in water, preferably for an extended period. Further, the surface of a golf ball is flexed due to the impact every time it is struck with a club and consequently these surfaces must be able to withstand such repeated stresses. Moreover, especially with the recreational player, golf balls are susceptible to striking any of a number of hard, abrasive surfaces such as concrete, asphalt, brick, stone, etc. as a result of errant shots. It is therefore desirable for golf ball manufacturers that their golf balls be resistant to delamination or chipping of the paint layers, as such defects impact negatively upon the public perception of the quality of the golf ball. Likewise, golf ball manufacturers also seek to prevent obliteration of all or part of their trademarks, logos or other identifying indicia which identifies the brand of the ball to the playing public. Protective coatings are therefore applied to the surface of the golf ball cover. A clear primer coat and top coat layer are commonly applied to the cover to provide a high gloss and an overall enhanced appearance to the ball. In such coated balls, the various identifying indicia may be applied either to the cover, the primer coat or the topcoat.
Protective and decorative coating materials, as well as methods of applying such materials to the surface of a golf ball cover are well known in the golf ball art. Generally, such coating materials comprise urethanes, urethane hybrids, polyesters and acrylics. If desired, more than one coating layer can be used. Typical two pack polyurethane coatings include separate packages of polyol and diisocyanate. Conventionally, a primer layer such as a solvent-based or a water-based polymer may be applied to promote adhesion or to smooth surface roughness before the finish coat(s) are deposited on the golf ball. In general, a cured polyurethane top coat is most widely used as a protective coating material.
In-mold coating of substrates is known, but has never before been used to coat golf balls. For example, U.S. Pat. No. 4,515,710 describes an in-mold coating composition that is free radically cured to create a thermoset coating having good adhesion to a substrate, good surface smoothness, and good paintability. U.S. Pat. No. 4,242,415 describes another in-mold coating composition containing amine-terminated reactive liquid polymers, a vinyl monomer, and crosslinkable ester urethane resins. Neither of these references, however, nor any other references presently known describe the use of these or similar materials for the in-mold coating of golf balls.
One problem encountered during golf ball coating is that each coat typically needs to be applied to the golf ball surface in a separate operation after the final molding of the golf ball cover about the core. Each of these steps is time consuming as once each coating is applied to the ball surface, there is a need to allow that coat to cure for a period of time before the next coat is applied. Also, as each of the often successive coats are applied to the golf ball the definition of the curves on the molded golf ball are smoothed and lose their sharpness due to build-up of the coating composition on the ball's outer surface, which also increases the outer diameter of the ball.
Accordingly there exists a need in the golf ball art for a process of coating a golf ball using a method that reduces the amount of necessary steps. Further, there exists a need for a method of making an in-mold coated golf ball having a dimple pattern wherein the external dimensions of the coated ball are substantially the same as those of the internal dimensions of the golf ball mold cavity.
SUMMARY OF THE INVENTION
The present invention is directed to a process for in-mold coating of golf balls. The phrase "in-mold coating", as used herein, refers to the application of a coating material to a golf ball while the ball is in a mold. The process of the present invention offers a number of significant advantages over prior art processes used to coat golf balls. For example, the invention permits a significant reduction, if not a complete elimination, of the amount of solvents used in formulating and applying the coating upon the balls. This has a twofold beneficial effect, i.e., less solvent means less drying time, thus significantly reducing the duration of the coating process (e.g., 30 minutes vs. 20 hours for the prior art). The reduction in the amount of solvent also means a concurrent reduction in the amount of volatile organic compounds ("VOC") materials encountered in the spraying process, thus offering significant safety and environmental benefits.
Further, for elastomer cover materials such as urethanes there is a substantial increase in the bond strength or adhesion between the coating material and the underlying substrate (the ball cover) since the temperature and present conditions under which the coating is applied results in the occurrence of a chemical reaction between the coating material and the ball surface, thus leading to the creation of chemical, and not just a mechanical, bond between the coating and the ball.
However, for thermoplastic cover materials such as Surlyn, upon heating of the cover materials, the molecular motion of the polymer chains therein allows for entanglements with the coating material, thereby enhancing the interfacial bonding between the thermoplastic cover materials and the coating composition.
Still further, with the use of the claimed process it is possible to produce a coated golf ball having a crisp and sharp dimple pattern that is not obscured by numerous coating layers, and which is readily releasable from the molding apparatus. Another advantage to the use of the in-mold coating process of the invention is that it permits the production of golf balls with more intricate dimple patterns in comparison to those obtained in the prior art where the golf balls are coated after molding.
One aspect of the invention is thus directed to a method of applying an in-mold coating upon the outer surface of a golf ball. The coating may be applied by a variety of methods in accordance with the invention including, in a first embodiment, forming a mold cavity between upper and lower mold dies, at least partially filling the cavity with a golf ball cover-forming composition and applying a desired pressure to the upper and lower mold dies to form, in the case of a one-piece ball, a golf ball, or alternately, in the case of a two or three-piece ball, a golf ball cover around a central core. Thereafter, a golf ball coating material, such as a fluidized plastic material, e.g., a polyester or urethane, is introduced, e.g., by spraying, injection or any other method known in the art, into the mold cavity between the golf ball outer surface and the inner surface of the mold cavity where the material coats the outer surface of the golf ball cover and is then cured, e.g., by thermosetting, to form a coating layer upon the ball. When the coating material is directed into the mold cavity, the mold cavity pressure may optionally be reduced to facilitate the flow of the coating material over the ball surface.
In a further embodiment, particularly useful for applying a polyurethane coating to the outer golf ball surface, the method of the invention comprises the steps of:
(1) forming a polyurethane coating composition by combining
(a) a first component including at least one polyol; and
(b) a second component comprising a substantially solvent-free isocyanate prepolymer; (2) forming an uncoated golf ball between at least two separable mold dies which form a mold cavity therebetween by molding the uncoated golf ball within the cavity until the golf ball reaches a condition where its surface has cured to the point that it is receptive to the application of the coating, i.e., wherein the coating material will not substantially penetrate the outer surface but will bond therewith; (3) injecting the coating composition into the mold cavity at a pressure substantially in excess of what the positive mold cavity pressure was immediately prior to injection while maintaining the dies in a pressurized, closed position whereby the coating composition is forced over the surface of the uncoated golf ball; and (4) curing the coated, formed golf ball.
A further aspect of the invention relates to in-mold coated golf balls produced according to the method of the invention. Such balls may be any type conventionally known in the art including one-piece, two-piece or wound. Once coated, the outer dimensions of these balls are substantially the same as the inner dimensions of the mold cavity in which they are coated.
DETAILED DESCRIPTION OF THE INVENTION
As used herein, the term "coating" means a material applied to the outer surface of a golf ball cover which may be opaque or transparent (i.e., known as a "clear coat"), which may impart a glossy or shiny appearance to the ball and which may provide some measure of protection and/or durability to the cover of the ball. Clear coats are generally free of pigmentation and are water white. However, any in-mold coating material, including those which contain one or more of a dye, pigment, optical brightener and/or other additives, is considered as falling within the scope of the invention.
The coating compositions useful in the present invention are those which are particularly useful in coating golf balls made by conventional molding techniques such as compression molding, injection molding and reactive material casting processes, all of which are well known in the art as evidenced, e.g. by the disclosure of U.S. Pat. Nos. 4,798,586 to Berard and 5,334,673 to Wu and Japanese Patent Publication No. 60-210272.
The in-mold coating materials appropriate for use in the present invention include any thermoplastic or thermosetting resin suitable for use with one or more of the conventional golf ball cover materials such as balata, ionomers, including acrylic and methacrylic acid based ionomers, urethanes, styrenes and olefinic polymers, to name but a few. Useful coating materials include, but are not limited to thermoplastic and thermosetting epoxies, acrylics, urethanes, polyesters, amino resins, phenolic resins, silicone resins, organo silane resins and fluoro resins. The in-mold coatings produced according to the present invention preferably have a suitable viscosity to enable them to flow out in an even layer over molded parts within relatively short periods of time. It is also desirable that the in-mold coating materials used in the invention have storage stability such that they do not prematurely cure or phase separate during storage or equipment shutdowns. It is also preferable that such in-mold coatings exhibit resistance to abrasion, solvents, and external deformations while retaining good adhesion to the cover material and sufficient flexibility to prevent cracking due to flexural strains.
The preferred in-mold coating compositions for use in the method of the invention include two component urethanes composed of a polyol or polyamine (e.g., a diamine) first component and a isocyanate prepolymer second component such as those disclosed, for example in U.S. Pat. No. 5,387,750, expressly incorporated herein by reference. Polyester resins, such as those disclosed in U.S. Pat. No. 5,304,332, may also be used as the in-mold coatings according to the present invention. Other useful in-mold coating materials include hydroxyterminated telechelic rubber polymers and block copolymers of flexible polymers of unsaturated polyester resins as described in U.S. Pat. No. 5,389,443, or polyesterurethane together with a multifunctional epoxy compound as disclosed in U.S. Pat. No. 5,143,788. Additional in-mold coating components for use in the invention are known in the coating art and are described in U.S. Pat. Nos. 4,076,788; 4,081,578; 4,515,710; 4,189,517; 4,242,415; 4,245,006; 4,414,173; 4,477,405; 5,132,052 and 4,668,460.
Other weatherable and durable coating compositions can be used to coat golf balls according to the present invention. For example, a coating of thermoset fluorinated polymers is suitable for use in the present invention. In particular, fluorinated polymers available from Zeneca, Inc. under the tradenames LUMIFLON 4-200F, LF-601, LF-710F, LFX-910 LM, LF-916 and LF-9200 are suitable coating compositions. A blend of an urethane resin and a fluoropolymer may also be used.
Typical solvents known in the art can be used in the present invention to dilute the coating composition or to reduce viscosity include: xylene, toluene, methyl ethyl ketone, methyl amyl ketone, methyl isobutyl ketone, propylene carbonate, N-methyl pyrrolidone and the like. For each 100 parts by weight of resin in the coating formulation, from 0 to about 100 parts by weight, or more preferably from 0 to 50 parts by weight, each of pigments, fillers, opacifiers, antioxidants, ultraviolet absorbers, or other additives may be added to the coating composition.
Some of the pigments contemplated for use in the invention are: carbon black, titanium oxide, chrome oxide (green), zinc oxide, ferrite yellow oxide, ferric oxides, raw sienna, burnt sienna, copper phthalocyanine blue, phthalocyanine green, ultramarine blue, toluidine red, parachlor red, cadmium reds and yellows, iron blues, and organic maroons. Silica, glass frit or flour, calcium carbonate, mica, antimony trioxide, fumed alumina, kaolin, talc, lithophone, zinc sulfide, zirconium oxide, calcium sulfate dihydrate, barium sulfate, china clay, diatomaceous earth, aluminum trihydrate, onyx four, metallic oxides, such as titanium dioxide, zinc oxide, iron oxide and the like, metal hydroxide, metal flakes such as aluminum flake, chromates, such as lead chromate, sulfides, sulfates, carbonates, carbon black, silica, talc, phthalycyanine blues and greens, organo reds, organo maroons and other organic pigments and dyes and calcium silicate are examples of additives, pigments, fillers and opacifiers contemplated. The fillers, pigments, and opacifiers may be suspended in the coating composition by the use of dispersing agents such as those taught in U.S. Pat. No. 4,016,115, which is incorporated herein by reference.
The pigments are formulated into a mill base by mixing with a dispersing resin which may be the same as the binder of the composition or may be another compatible dispersing resin or agent. The pigment dispersion is formed by conventional means such as sand grinding, ball milling, high speed dispersing or three roll milling. The mill base can then be blended with the binder of the composition to form the coating composition.
To improve weatherability of the coating composition, in particular with regard to clear coat compositions, about 0.01-5.0% by weight, based on the weight of the binder, of an ultraviolet light stabilizer or ultraviolet absorber, or a combination of ultraviolet light stabilizers and ultraviolet absorber, can be added to the clear coating composition. Typically useful ultraviolet light stabilizers and ultraviolet absorber are as follows:
Benzophenones such as hydroxy dodecyloxy benzophenone, 2,4-dihydroxybenzophenone, hydroxybenzophenones containing sulfonic groups and the like. Triazoles such as 2-phenyl-4-(2',2'dihydryoxylbenzoyl) -triazoles, substituted benzotriazoles such as hydroxy-phenyltriazoles and the like.
Triazines such as 3,5-dialkyl-4-hydroxyphenyl derivatives of triazine, sulfur containing derivatives of dialyl-4-hydroxy phenyl triazines, hydroxy phenyl-1,3,5-triazine and the like.
Benzoates such as dibenzoate of diphenylol propane, tertiary butyl benzoate of diphenylol propane and the like.
Other ultraviolet light stabilizers that can be used include lower alkyl thiomethylene containing phenols, substituted benzenes such as 1,3-bis-(2'-hydroxybenzoyl)benzene, metal derivatives of 3,5-di-t-butyl-4-hydroxy phenyl propionic acid, asymmetrical oxalic acid, diarylamides, alkylhydroxy-phenyl-thioalkanoic acid ester and the like.
Particularly useful ultraviolet light stabilizers that can be used are hindered amines of bipiperidyl derivatives such as those disclosed in Murayama, et al., U.S. Pat. No. 4,061,616, issued Dec. 6, 1977.
When used as a clear coat, the coating composition can also contain transparent pigments to improve durability and weatherability. These transparent pigments should have the same or a similar refractive index as the binder of the clear coat and have a small particle size of about 0.015-50microns. Typical pigments that can be used in the clear coat in a pigment to binder weight ratio of about 1:100 to 10:100 are inorganic siliceous pigments, such as silica pigments and have a refractive index of about 1.4-1.6.
If the coating composition is used as a conventional pigmented monocoat coating composition or as the basecoat of a clear coat/basecoat composition, the composition preferably contains pigments in a pigment to binder weight ratio of about 1:100-50:100. It may additionally be advantageous to use the aforementioned ultraviolet stabilizers and/or ultraviolet absorbers in the pigmented composition.
Mixing of the ingredients of the in-mold coating composition should be thorough. Injection molding, compression molding, transfer molding, or other molding apparatus or machines can be used for the in-mold coating. Molding apparatus and methods may be found in U.S. Pat. Nos. 4,076,780;; 4,076,788; 4,081,578; 4,082,486; 4,189,517; 4,222,929; 4,245,006; 4,239,796; 4,239,808 and 4,331,735.
See also, "Proceedings of the Thirty-Second Annual Conference Reinforced Plastics/Composites Institute," SPI Washington, February, 1977, Griffith et al., Section 2-C, pages 1-3 and "33rd Annual Technical Conference, 1978, Reinforced Plastics/Composites Institute, The Society of the Plastics Industry, Inc.," SPI Ongena Section 14-B, pages 107.
According to the invention the in-mold coating method comprises forming a mold cavity between upper and lower mold dies, at least partially filling the cavity with a golf ball cover-forming composition and applying a desired pressure to the upper and lower mold dies to form, in the case of a two or three-piece ball, a golf ball cover around a central core. In another embodiment involving the formation of a one-piece ball, the cavity is filled with a golf-ball cover forming composition and a desired pressure is applied to the mold cavity to form a golf ball suitable for coating according to the invention. Thereafter, a golf ball coating material, such as a fluidized plastic material, e.g., a polyester or urethane, is introduced, e.g., by spraying, injection or any other method known in the art, into the mold cavity between the golf ball outer surface and the inner surface of the mold cavity where the material coats the outer surface of the golf ball cover and is then cured, e.g., by thermosetting, to form a coating layer upon the ball. When the coating material is directed into the mold cavity, the desired pressure may optionally be reduced to facilitate the flow of the coating material over the ball surface. Such an in-mold coating method is described, for instance, in U.S. Pat. No. 4,668,460, entitled "METHOD OF MOLDING AND COATING A SUBSTRATE IN A MOLD," issued May 26, 1987.
Alternatively, if desired, the uncoated ball may be removed from the first, "ball-forming mold" and coated in a separate, second mold in the manner indicated above while the first mold is operated to produce additional balls to be coated.
A preferred method for in-mold coating an uncoated golf ball with a polyurethane coating includes the steps of
(1) forming a polyurethane coating composition by combining
(a) a first component including at least one polyol; and
(b) a second component comprising a substantially solvent-free isocyanate prepolymer; (2) forming an uncoated golf ball between at least two separable mold dies which form a mold cavity there between by molding the uncoated golf ball within the cavity until the golf ball reaches a condition where its surface has cured to the point that it is receptive to the application of the coating, i.e., wherein the coating material will not substantially penetrate the outer surface but will bond therewith; (3) introducing the coating composition into the mold cavity at a pressure in excess of what the positive mold cavity pressure was immediately prior to introduction while maintaining the dies in a pressurized, closed position whereby the coating composition is forced over the surface of the uncoated golf ball; and (4) curing the coated, formed golf ball.
To form urethane coating composition for use in the present invention, predetermined volumes of each component are mixed in an impingement or static mixer prior to injection into the mold. Preferably, to ensure the proper mixing, either the polyol component, the isocyanate component or both components are heated so that the viscosity of these components are approximately the same. The coating composition can either be injected into the mold after the uncoated golf ball has completely cured, or, more preferably, when the substrate has sufficiently cured so that the coating will not penetrate the substrate. The coating composition is introduced into the mold cavity between the surface of the uncoated golf ball and the mold surface. Thereafter, the mold is retained in a closed position for a sufficient period to allow the molded golf ball to complete further curing and to allow the coating composition to be cured as an adherent coating over the outer surface of the molded golf ball.
The cure time required for the coatings of the invention should be slow enough to allow the coating to flow over the substrate in the mold prior to excessive gelation, but short enough to allow substantial curing within the molding cycle. The cure time of the coating depends on a number of factors, including the thickness of the coating, the temperature of the mold, the amount of catalyst and the reactivity of the polyol and the isocyanate prepolymer. The cure time of the coating is typically about 0.01-30.0 minutes at a mold temperature of about 250-350° C.
Typical coating compositions according to the present invention have a thickness of from about 0.05-100.0 mils or more preferably from about 0.05-20.0 mils.
While it is preferred that the above described materials be used for in-mold coating of golf balls according to the invention, other materials may be used for this purpose, including those described in any of the following patents U.S. Pat. Nos. 3,216,877; 4,205,028; 4,228,113; 4,287,310; 4,315,884; 4,499,235; 4,873,274.
Generally speaking, the in-mold coating compositions contemplated for use in the invention can be applied to the substrate and cured at a temperature of from about 25° to 350° C. and at a pressure of from about 1 psi to about 1,000 psi for from about 0.01 to 30.0 minutes. This creates a promising coating for use in preserving and protecting golf ball covers.
All aforementioned patents and other publications are herein specifically incorporated by reference in their entirety.
The scope of the following claims is intended to encompass all obvious changes in the details, materials, and arrangement of parts that will occur to one of ordinary skill in the art.
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A method of applying a coating material, such as a urethane, to an outer dimpled surface of a golf ball by forming a first mold cavity between upper and lower mold dies configured and adapted for molding a golf ball, molding a golf ball having an outer dimpled surface within the first mold cavity under a first pressure greater than ambient pressure until the golf ball is sufficiently cured to receive a coating that will not substantially penetrate the outer dimpled surface of the ball, opening the first mold cavity and transferring the molded but uncoated golf ball to a second mold cavity, preparing an in-mold golf ball coating composition, introducing a sufficient amount of the coating composition into the second mold cavity between the outer dimpled surface of the golf ball and an inner surface of said second mold cavity to substantially surround and coat the outer surface of said golf ball, curing said coating composition to form a coated golf ball having at least one layer of said coating composition, and removing said coated ball from the second mold cavity so as to produce a coated golf ball having a dimple pattern thereon.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a centrifugal wastewater separation, and more particularly to a wastewater separator.
[0003] 2. Description of the Prior Art
[0004] A conventional wastewater separator such as a sullage concentrator disclosed in Taiwan Pat. No. 092221042 generally utilizes an inner pressure tank to discharge the sullage into a centrifugal type separator, and then enables the sullage to swirl in the centrifugal type separator. Therefore, the sullage is subjected to a centrifugal force, so that the sediment subjected to gravity greater than the centrifugal force will drop down, and the water subjected to gravity smaller than the centrifugal force will be kept in the centrifugal type separator and then guided out of the separator, thus separating the water from the sediment.
[0005] However, the above technology only utilizes the high pressure supplied from the pressure tank to produce the centrifugal force required for separation, so that when the ratio of the sediment and the water in the sullage changes, it is necessary to readjust the pressure supplied from the pressure tank to the sullage, thus increasing the operational complexity. In addition, the pressure supplied from the pressure tank can only separate the water from the sediment roughly, so that the above wastewater separator must be additionally equipped with a sieving machine to separate the water from the sediment completely, thus causing the increase of the operation procedure.
[0006] The present invention has arisen to mitigate and/or obviate the afore-described disadvantages.
SUMMARY OF THE INVENTION
[0007] The primary objective of the present invention is to provide a wastewater separator, which can achieve the objective of separating the water from the impurities in the wastewater by utilizing an inner pivoting assembly and an outer pivoting assembly to produce a centrifugal force to enable the impurity which is relatively heavy in the wastewater to fall down along the helical blade and the water which is relatively light in the wastewater to flow upwards along the outer pivoting assembly.
[0008] In order to achieve the above objective, the wastewater separator comprises a housing, an outer pivoting assembly and an inner pivoting assembly. The housing is provided with a power source. The outer pivoting assembly is pivoted to the housing and connected to the power source. The outer pivoting assembly includes a cover cylinder. The inner pivoting assembly is pivoted in the outer pivoting assembly and connected to the power source. The inner pivoting assembly includes a helical blade which extends in an axial direction of the inner pivoting assembly and arranged opposite to the cover cylinder.
[0009] The outer pivoting assembly and the inner pivoting assembly are driven to pivot by the power source, so that when the wastewater is guided onto the blade of the inner pivoting assembly, since the blade is helical, the impurity which is relatively heavy in the wastewater will fall down along the blade, and the water which is relatively light in the wastewater will flow outwards under the action of the centrifugal force. When contacting the cover cylinder, the water flowing outwards from the blade will flow upwards along the cover cylinder, thus separating the water from the impurities in the wastewater.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 is a schematic view illustrating that a wastewater separator in accordance with the present invention is disposed on a machine;
[0011] FIG. 2 is a schematic view illustrating that a power source for a wastewater separator in accordance with the present invention consists of two motors;
[0012] FIG. 3 is a schematic view illustrating that the power source for a wastewater separator in accordance with the present invention consists of a motor; and
[0013] FIG. 4 is a schematic view illustrating that the power source for a wastewater separator in accordance with the present invention includes a gear box;
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0014] The present invention will be clearer from the following description when viewed together with the accompanying drawings, which show, for purpose of illustrations only, the preferred embodiment in accordance with the present invention.
[0015] Referring to FIGS. 1-2 , a wastewater separator in accordance with the present invention comprises a housing 10 , an outer pivoting assembly 20 , an inner pivoting assembly 30 , and a water supplier 40 .
[0016] The housing 10 , as shown in FIG. 1 , is disposed on a machine F and provided with a power source 11 consisting of a first motor 12 and a second motor 13 . The shaft 121 of the first motor 12 is fixed with a first active member 122 , and the shaft 131 of the second motor 13 is fixed with a second active member 132 .
[0017] The outer pivoting assembly 20 is exteriorly provided with plural outer bearings A and interiorly provided with plural inner bearings B. The outer bearings A are further disposed in the housing 10 to pivot the outer pivoting assembly 20 in the housing 10 and make the outer pivoting assembly 20 pivot in a direction vertical to the ground. The outer pivoting assembly 20 includes a sleeve 21 , a connection case 22 and a cover cylinder 23 . The sleeve 21 , the connecting case 22 are successively integrally connected with one another in such a manner both axial ends of the outer pivoting assembly 20 communicate outwards. A first passive member 211 is disposed outside the sleeve 21 and connected to the second active member 132 of the second motor 13 of the power source 11 through a first drive member C. The connecting case 22 is formed with an axial through hole 221 . The cover cylinder 23 is vertically tapered downwards.
[0018] The inner pivoting assembly 30 is disposed in the inner bearings B of the outer pivoting assembly 20 in such a manner that the inner pivoting assembly 30 is pivoted in the outer pivoting assembly 20 and pivots in a direction vertical to the ground. The inner pivoting assembly 30 includes a duct 31 , a blade socket 32 and a blade 33 . The duct 31 includes a guiding hole 311 and is exteriorly provided with a second passive member 312 , which is connected to the first active member 122 of the first motor 12 of the power source 11 through a second drive member D. The blade socket 32 is radially formed with plural flow passages 321 communicating with one another at an upper end thereof. The upper end of the blade socket 32 is integrally connected with the duct 31 , and the flow passages 321 of the blade socket 32 communicate with the guiding hole 311 of the duct 31 . The blade socket 32 further includes a water passage 322 and plural water outlet passages 323 . The water passage 322 is axially formed under the blade socket 32 . One end of the respective water outlet passages 323 communicates with the water passage 322 , and the other end of the respective water outlet passages 323 communicates outwards from the side surface of the blade socket 32 . The blade 33 is disposed on the side surface of the blade socket 32 . The blade 33 helically extends in an axial direction of the inner pivoting assembly 30 and is arranged opposite to the cover cylinder 23 of the outer pivoting assembly 20 . Between blade 33 and the cover cylinder 23 is provided a clearance.
[0019] The water supplier 40 is exteriorly provided with plural bearings E at one end thereof. The bearings E are further disposed in the water passage 322 of the blade socket 32 of the inner pivoting assembly 30 in such a manner that the end of the supplier 40 is pivoted in the water passage 322 of the blade socket 32 from the lower end of the blade socket 32 . The water supplier 40 further includes a through hole 41 communicating with the water passage 322 .
[0020] The shaft 121 of the first motor 12 of the power source 11 utilizes the first active member 122 , the second drive member D and the second passive member 312 of the duct 31 of the inner pivoting assembly 30 to drive the inner pivoting assembly 30 to pivot. The shaft 131 of the second motor 13 of the power source 11 utilizes the second active member 132 , the first drive member C and the first passive member 211 of the sleeve 21 of the outer pivoting assembly 20 to drive the outer pivoting assembly 20 to pivot.
[0021] When being guided in from the guiding hole 311 of the duct 31 of the inner pivoting assembly 30 , under the action of the centrifugal force produced by the pivoting of the inner pivoting assembly 30 , the wastewater will flow out to the blade 33 from the flow passage 321 of the blade socket 32 . As the inner pivoting assembly 30 pivots and the wastewater is continuously guided in, the relatively heavy impurities in the wastewater will continuously increase and be pressed to drop down along the blade 33 , and the relatively light water will flow outwards under the action of the centrifugal force produced by the pivoting of the inner pivoting assembly 30 . When contacting the cover cylinder 13 , the water flowing from the blade 33 will be guided by the tapered cover cylinder 23 in the clearance between the blade 33 and the cover cylinder 23 to flow upwards along the cover cylinder 23 and then spew upwards from the through hole 221 of the connecting case 22 of the outer pivoting assembly 20 . By such arrangements, the water can be separated from the impurities.
[0022] If the power source 11 drives the outer pivoting assembly 20 and the inner pivoting assembly 30 to pivot in the same direction, the separation effect of the impurities and water in the wastewater can be improved. In addition, increasing the pivoting speed higher than the outer pivoting assembly 20 can further improve the separation effect and make the purity of separated water reach 90% and the dryness of the separated impurities reach 60%.
[0023] When the clean water is guided in through the through hole 41 of the water supplier 40 , the clean water will flow in the water passage 322 of the blade socket 32 of the inner pivoting assembly 30 and then flow out of the water outlet passages 323 onto the blade 33 , so that the blade 33 of the inner pivoting assembly 30 and the cover cylinder 22 of the outer pivoting assembly 20 . In addition, the clean water which is guided in through the through hole 41 of the water supplier 40 during the separation of wastewater can wash the impurities separated from the wastewater.
[0024] Additionally, besides consisting of a first motor 12 and a second motor 13 to drive the inner pivoting assembly 30 and the outer pivoting assembly 20 , the power source 11 can consist of a motor 14 whose shaft 141 is fixed with a third active member 142 and a fourth active member 143 to drive the inner pivoting assembly 30 and the outer pivoting assembly 20 .The third active member 142 is connected to the second passive member 312 of the duct 31 of the inner pivoting assembly 30 through the second drive member D, and the fourth active member 143 is connected to the first passive member 211 of the sleeve 21 of the outer pivoting assembly 20 through the first drive member C.
[0025] In the above embodiments, the active members 122 , 132 , 142 , 143 and the passive members 211 , 312 can be in the form of a pulley, gear, dentate disc or other pivoting actuating elements. The drive members C and D can be in the form of a belt, chain or other linkage elements. The cover cylinder 23 of the outer pivoting assembly 20 can also be a straight cylinder, which has the function of separating the impurities from water in the wastewater.
[0026] Further referring to FIG. 4 , the power source 11 can also consist of a motor 14 and a gear box 50 . The motor 14 is connected to the gear cluster in the gear box 50 , and a first gear 51 and a second gear 52 are exposed out of the gear box 50 . The first passive member 211 and the second passive member 312 are both in the form of a gear. The first passive member 211 is engaged with the second gear 52 , and the second passive member 312 is engaged with the first gear 51 . By such arrangements, the motor 14 of the power source 11 can utilize the first gear 51 and the second gear 52 to drive the second passive member 312 and the first passive member 211 to enable the outer pivoting assembly 20 and the inner pivoting assembly 30 to pivot, so as to separate the water from the impurities in the wastewater.
[0027] While we have shown and described various embodiments in accordance with the present invention, it is clear to those skilled in the art that further embodiments may be made without departing from the scope of the present invention.
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A wastewater separator comprises an inner pivoting assembly and an outer pivoting assembly. The wastewater is guided onto a blade which helically extends in the axial direction of the inner pivoting assembly. The inner pivoting assembly and the outer pivoting assembly are driven to pivot for enabling the impurity in the wastewater to fall off along the blade and the water in the wastewater to flow upwards along the outer pivoting assembly, so as to achieve the objective of separating the water from impurity in the wastewater.
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RELATED APPLICATION DATA
[0001] This application is based on and claims the benefit of U.S. Provisional Patent Application No. 60/449,167 filed on Feb. 20, 2003.
INTRODUCTION
[0002] Financial assistance for this invention was provided by the United States Government, Division of Cancer Treatment and Diagnosis, National Cancer Institute, Department of Health and Human Services Outstanding Investigator Grant Numbers R01-CA9044-01 and CA44344-05-1-12; the Arizona Disease Control Research Cornmission; and private contributions. Thus, the United States Government has certain rights in this invention.
FIELD OF THE INVENTION
[0003] This invention relates to the isolation from natural sources, and elucidation of the structure of, a compound having antineoplastic, antibacterial and antifungal properties.
BACKGROUND OF THE INVENTION
[0004] Marine porifera have continued to be an increasingly important source of new nitrogen heterocyclic compounds with significant biological activities. Recent examples include the cytotoxic constituents pateomine ( Mycale sp. ), a pyridine betaine ( Microcosnus vulgaris ), topsentin B2 ( Rhaphisia lacazei ), asmarine A ( Raspailia sp. ), cyclic guanidines ( Monanchiora sp. ), the antiviral dragmacidin F ( Halicortex sp. ) and the isolation and structure determination of cribrostatins 4 (1) and 5 (2) from the Republic of Maldives blue-colored sponge Cribroclhalina sp. (West, L.; et al., J. Org. Chem. 2000, 65, 445-449; Aiello, A., et al., J. Nat. Prod. 2000, 63, 517-519; Casapullo, A., et al., J. Nat. Prod. 2000, 63, 447-451; Yosief, T., et al., J. Nat. Prod. 2000, 63, 299-304; Braekman, J., et al., J. Nat. Prod. 2000, 63, 193-196; Cutignano, A., et al., Tetrahedron 2000, 56, 3743-3748, Pettit, G., et al., J. Nat. Prod. 2000, 6, 793-798.)
SUMMARY OF THE INVENTION
[0005] The present invention relates to the elucidation of the molecular structure for a novel compound denominated Cribrostatin 6, as well as to a method for isolating the compound Cribrostatin 6 from the Marine organism Cribrochalina sp. Cribrostratin 6 exhibits antineoplastic, antibacterial and antiflngal properties. Accordingly, the invention also relates to the use of Cribrostatin 6 as a pharmaceutical agent for the treatment of neoplastic disease, as well as for the treatment of bacterial and fungal infections.
DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 illustrates the solid-state structure of Cribrostatin 6.
[0007] FIG. 2 illustrates the chemical structures of Cribrostatins 1, 2, 3, 4, 5 and 6.
DETAILED DESCRIPTION OF THE INVENTION
[0008] Earlier we had observed a number of biologically active blue to black colored fractions arising during P388 lymphocytic leukemia guided separations of a 195 g dichloromethane-soluble portion of the extract obtained from 350 kg (wet wt.) of Cribrochalina sp. The cancer cell growth (P-388) inhibitory dark-colored fractions were finally separated by a successive series of gel permeation and partition chromatographic techniques on Sephadex LH-20. That sequence was followed by high-speed countetcurrent distribution using an Ito Coil-Planet centrifuge to afford 88 mg of a dark-blue constituent (P388 ED 50 0.3 μg/ml), designated cribrostatin 6 (3). Owing to difficulties in unequivocally deducing the structure of this interesting substance based on spectral evidence, attempts were made at various times over a ten year period to reach a correct solution and/or to produce crystals suitable for X-ray structure determination. We were eventually pleased to find that cribrostatin 6 (3) would crystallize from acetone following long cold storage of the solution. To follow is a summary of the spectral and X-ray crystallographic interpretation that completed a correct structural assignment for cribrostatin 6 (3).
[0000] Results and Discussion
[0009] The molecular formula of cribrostatin 6 (3) was established as C 15 H 14 N 2 O 3 by HRMS, using an APCI inlet system. Inspection of the 1 H and APT NMR spectra indicated the presence of three methyls, one methylene, three methines and eight quaternary carbons. Protonated carbons were assigned using a HMQC experiment. The APT spectrum indicated that four of the carbons were oxygenated and suggested the presence of the quinone. An HMBC experiment allowed placement of the C-9 ethoxy (H-13 to C-9) and C-8 methyl (H-12 to C-7, 8, and 9) groups and established the positions of the quaternary carbons at C-8 and 9 as well as the carbonyl carbons at C-7 and 10, which were assigned by analogy with known isoquinolinequinones such as the Saframycins. (Cooper, R., et al., Antibiotics 1985, 38, 24-30). This accounted for five of the ten degrees of unsaturation determined from the molecular formula. The nature of the B ring was established by 1H-1H COSY, which indicated the presence of a double bond. The HMBC spectrum showed connectivities from the proton at H-6 to C-6a, 7 and 10a as well as establishing the position of the double bond at Δ, which was confirmed by HMBC correlations from H-5 to C-6 and 6a. (Braekman, J., et al., J. Nat. Prod. 2000, 63, 193-196; Cutignano, A., et al., Tetrahedron 2000, 56, 3743-3748.) The remaining three degrees of unsaturation and the fragment C 3 H 4 N 2 suggested an imidazo-partial structure for a C ring. The overall structure was determined by X-Ray diffraction on a small needle-shaped crystal. Although the overall connectivity could be readily established, the low observed data-to-parameter ratio did not permit a clear distinction between structures 3 and 4. Analogy to previous cribrostatin-related compounds (cf. 1, 2) gave the location of one of the N atoms at position 4 with reasonable certainty (Pettit, G., et al., J. Nat. Prod. 2000, 6, 793-798; Pettit, G., et al., Can. J. Chem. 1992, 70, 1170-1175), but conclusive structural assignment as 9-ethoxy-3,8-dimethyl-imidazo[5,1-a]isoquinoline-7, 10-dione (3) required further, more detailed analysis of earlier and new NMR data.
[0010] Examination of the HMBC spectrum showed correlations from H5 to C-3 and C10b and implied placement of a nitrogen at position 4. A strong correlation from the remaining methine proton to C-3 suggested position 1 with the remaining nitrogen at position 2. An additional correlation from H-11 to C-3 located the remaining methyl group (δ 2.75p) at C-3. A DPFGSENOE (GOESY) experiment demonstrated NOE enhancement between H-5 and H-11 that would be consistent with either structure 3 or 4, but gave no indication of an enhancement between H-2 and H-11, that would be expected to exist in structure 4 (Stonehouse, J., et al., J. Amer. Chem. Soc. 1994, 116, 6037-6038). Measurement of 15 N- 1 H HMBC showed two strong 3-bond correlations from the methyl protons H11 to both nitrogens N2 and N4. HMBC correlations were observed H5 and H6 to N4, but not N2. H1 showed weak correlations to both N2 and N4. Only structure 3 is consistent with these results.
[0011] In addition to cancer cell growth inhibition of murine P388 lymphocytic leukemia and human cancer cell lines (see Table II), cribrostatin 6 exhibited antimicrobial activity against numerous antibiotic-resistant Gram-positive bacteria and patlhogenic fungi (see Table III). The only Gram-negative bacterium of those tested which was inhibited by cribrostatin 6 was Neisseria gonorrhoeae. Cribrostatin 2 has an antimicrobial profile similar to cribrostatin 6, while cribrostatins 1, 3, 4 and 5 have antibacterial but not antifungal activities. (Pettit, G., et al., J. Nat. Prod. 2000, 6, 793-798). Thus, the inventors believe that the cribrostatins, particularly cribrostatin 6, warrant further investigation as antibacterial and/or antifungal agents.
[0012] Recently, two phosphorylated sterol sulfates were isolated from a Cribrochalina sp. and found to be membrane-type metalloproteinase (MT1-MMP) inhibitors. (Fujita, M., et al., Tetrahedron 2001, 57, 3885-3890.) That advance extends the structural variety of Cribrochalina genus cell growth regulatory constituents that so far range from acetylenic alcohols to quinones (cf. 3) and peptides. (Hallock, Y., et al., J. Nat. Prod. 1995, 58, 1801-1807; Garcia, J., et al. Tetrahedron: Asymmetry 1999, 10, 2617-2626; Sharma, A.; et al., S. Tetrahedron: Asymmetry 1998, 9, 2635-2639; Pettit, G., et al., J. Nat. Prod. 2000, 6, 793-798; Pettit, G., et al., Can. J Chem. 1992, 70, 1170-1175; Yeung, B., et al., J. Org. Chem. 1996, 61, 7168-7173.)
[0000] Experimental Section
[0013] General Experimental Methods. Except as noted, the general experimental procedures employed in our original investigations of the Cribrochalina sp. were continued here. For discussion of these original investigations, see Pettit, G., et al., J. Nat. Prod. 2000, 6, 793-798; and Pettit, G., et al., Can. J Chem. 1992, 70, 1170-1175, which are incorporated herein by reference. NMR spectra were recorded using a Varian Inova system equipped with a 5 mm triple resonance triaxial PFG probe at 500 MHz for 1 H and 125 MHz for 13 C, and 50.65 MHz for 15 N. 15 N- 1 H gradient HMBC experiments were performed on 2.2 mg of sample dissolved in 100 μl CDCl 3 using a Shigemi 3 mm NMR tube susceptibility matched to CDCl 3 , a Nalorac 3 mm 1 H{ 15 N- 31 P} indirect-detection probe and delays optimized for coupling constants of 90 Hz (1-bond) and 5 Hz (multiple-bond). The 15 N spectra were referenced to formamide (112 pm downfield of liquid ammonia). (Martin, G. et al., J. Nat. Prod. 2000, 63, 543-585.) The 1 H NMR and 13 C NMR spectra were referenced to residual solvent signals at 7.25 and 77.0 ppm for CDCl 3 . HRMS data was obtained using a JEOL LCMate magnetic sector instrument in the APCI mode, calibrated using a polythylene glycol reference mixture. The X-Ray data collection was accomplished using a Bruker AXS 6000 diffractometer.
[0014] Isolation of Cribrostatin 6 (1). The blue marine sponge Cribrochalina sp. was collected and extracted as known to one of skill in the art, as described in Pettit, G., et al., J. Nat. Prod. 2000, 6, 793-798 and Pettit, G., et al., Can. J. Chem. 1992, 70, 1170-1175, which is incorporated herein by reference. Fractionation of the extract, guided by the blue color, and the screening results obtained using the murine P-388 lymphocytic leukemia cell line, was carried out on columns of Sephadex LH-20, eluted successively with a.) CH 3 OH; b.) CH 2 Cl 2 -CH 3 OH (3:2); c.) hexane-toluene-CH 3 OH (3:1:1); and d.) hexane/i-PrOH-CH 3 OH (8:1:1). In preparation for a separation using high-speed countercurrent distribution on an Ito Coil-Planet centrifuge, the blue fraction from the previous column was triturated with the upper (less polar) phase of the system hexane-EtOAc-CH 3 OH-water (700:300:150:60), and the solution was filtered. The sparingly-soluble material thus obtained (35.7 mg) proved to be the same as the solid isolated from the principal blue fraction from the countercurrent run (53 mg). The two were combined and recrystallized from acetone to afford dark-blue needles: mp 169-171° C.; P-388 ED 50 0.3 μg/ML; λ max 203 (26,758), 266 (24,432), 323 (5597), 552 (1479); IR v max 2920, 1660, 1620, 1605, 1522, 1170 cm −1 ; 1 H and 13 C-NMR, see Table I; LREIMS (m/z) 270, 242, 214, 185, 172, 157, 145, 116; HRMS (APCI + ) 271.10968 (calcd for (M+H) + ion C 15 H 15 N 2 O 3 , 271.10828 error 5.2 ppm).
[0015] Crystal Structure of Cribrostatin 6 (3). All data including atomic coordinates, thermal parameters, bond distances, angles, and observed and calculated structure factors have been deposited in the Cambridge Crystallographic Data Centre and can be obtained, free of charge, on application to the Director, CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax: +44-(0)1223-336003 or e-mail: deposit@ccdc.cam.ac.uk). A very small, dark-blue needle obtained via slow evaporation of an acetone solution, with approximate dimensions of (0.05×0.05×0.20 mm), was mounted on the tip of a glass fiber. An initial set of cell constants was calculated from reflections harvested from three sets of 60 frames at 298(2) K on a Bruker 6000 diffractometer. Cell parameters indicated an orthorhombic space group. Subsequent data collection, using 30 second scans/frame and 0.396° steps in Ω, was conducted in such a manner as to completely survey a complete hemisphere of reflections. This resulted in >93% coverage of the total reflections possible to a resolution of 0.83. A total of 10229 reflections were harvested from the total data collection and final cell constants were calculated from a set of 332 strong, unique reflections. Subsequent statistical analysis of the complete reflection data set using the XPREP program indicated the space group was Pca2 1 . The XPREP program is an automatic space determination program included in the SHELXTL-NT-Version 5.10 (1997), which an integrated suite of programs for the determination of crystal structures from diffraction data, that is available from Bruker AXS, Inc., Madison, Wis. 53719, USA. This package includes, among others, XPREP, SHELXS (a structure solution program via Patterson or direct methods), and SHELXL (structure refinement software).
[0016] Crystal data: C 15 H 14 N 2 O 3 , a=15.414(15), b=11.532(11), c=7.201(7) Å, V=1280(2) Å 3 , λ=(Cu Kα)=1.54178 Å, μ (Cu K)=0.817 mm −1 , ρc=1.403 g cm −3 for Z=4 and M r =270.28, F (000)=568. After data reduction, merging of equivalent reflections and rejection of systematic absences, 1885 unique reflections remained (R int =0.5248), of which 315 were considered observed (I o >2 (I o )) and were used in the subsequent structure solution and refinement. An absorption correction was applied to the data with SADBS. (Blessing, R., Acta Cryst., 1995, A51, 33-8.) Direct methods structure determination and refinement were accomplished with the SHELXTL NT ver.V5.10 suite of programs. All non-hydrogen atoms for cribrostatin 6 (3) were located using the default settings of that program. Although the overall connectivity of the non-hydrogen atoms in quinone 3 could be readily established from the X-ray data, the low observed data-to-parameter ratio did not allow a completely unambiguous assignment of the two nitrogen atoms. The location of one of the N atoms at position 9 ( FIG. 1 ; X-ray numbering system) was known with reasonable certainty (due to analogy to previous cribrostatin related compounds), the position of the second N atom was less certain, with positions 11 and 12 both being likely candidates. Refinement of each of these possible isomeric structures (i.e., structures 3 or 4) resulted in nearly identical residual R 1 values (0.0982 vs 0.1002, respectively). Although the former (3) was slightly favored by these results, the final, conclusive structural assignment was based on observed 15 N-NMR experiments. Since the quality of data precluded the direct determination of hydrogen atom positions, the remaining hydrogen atom coordinates were calculated at optimum positions using the program SHELXL. These latter atoms were assigned thermal parameters equal to either 1.2 or 1.5 (depending upon chemical type) of the Uiso value of the atom to which they were attached, then both coordinates and thermal values were forced to ride that atom during final cycles of refinement. All non-hydrogen atoms were refined anisotropically in a full-matrix least-squares refinement process. The final standard residual R 1 value for the model shown in FIG. 1 was 0.0982 (for observed data) and 0.3817 (for all data). The corresponding Sheldrick R values were wR 2 of 0.2174 and 0.2741, respectively. The difference Fourier map showed insignificant residual electron density; the largest difference peak and hole being +0.255 and −0.252 e/Å 3 , respectively. Final bond distances and angles were all within acceptable limits.
[0000] Cancer Cell Growth Inhibition
[0017] Compounds were screened against a panel of human cancer cell lines and mouse cell lines as is shown in Table II. Cribrostatin 6 exhibited cancer cell growth against all lines illustrated.
[0000] Antimicrobial Susceptibility Testing
[0018] Compounds were screened against bacteria and fungi according to established broth microdilution susceptibility assays, pursuant to the National Committee for Clinical Laboratory Standards, Methods for Dilution Antimicrobial Susceptibility Tests for Bacteria that Grow Aerobically, Approved Standard M7-A4, Wayne, Pa.: NCCLS, 1997, and the National Conmnittee for Clinical Laboratory Standards, Reference Method for Broth Dilution Antifungal Susceptibility Testing of Yeasts, Approved Standard M27-A, Wayne, Pa.: NCCLS, 1997. The results of such screening are shown in Table III. The minimum inhibitory concentration was defined as the lowest concentration of compound that inhibited all visible growth of the test organism (optically clear). Assays were repeated on separate days.
ADMINISTRATION
[0000] Dosages
[0019] The dosage of the presently disclosed compounds to be administered to humans and other animals requiring treatment will depend upon numerous factors, including the identity of the neoplastic disease or microbial infection; the type of host involved, including its age, health and weight; the kind of concurrent treatment, if any; the frequency of treatment and therapeutic ratio. Hereinafter are described various possible dosages and methods of administration, with the understanding that the following are intended to be illustrative only, and that the actual dosages to be administered, and methods of administration or delivery may vary therefrom. The proper dosages and administration forms and methods may be determined by one of skill in the art.
[0020] Illustratively, dosage levels of the administered active ingredients are: intravenous, 0.1 to about 20 mg/kg; intramuscular, 1 to about 50 mg/kg; orally, 5 to about 100 mg/kg; intranasal instillation, 5 to about 100 mg/kg; and aerosol, 5 to about 100 mg/k of host body weight.
[0021] Expressed in terms of concentration, an active ingredient can be present in the compositions of the present invention for localized use about the cutis, intranasally, pharyngolaryngeally, bronchially, intravaginally, rectally, or ocularly in concentration of from about 0.01 to about 50% w/w of the composition; preferably about 1 to about 20% w/w of the composition; and for parenteral use in a concentration of from about 0.05 to about 50% w/v of the composition and preferably from about 5 to about 20% w/v.
[0022] The compositions of the present invention are preferably presented for administration to humans and animals in unit dosage forms, such as tablets, capsules, pills, powders, granules, suppositories, sterile parenteral solutions or suspensions, sterile non-parenteral solutions of suspensions, and oral solutions or suspensions and the like, containing suitable quantities of an active ingredient. Other dosage forms known in the art may be used.
[0023] For oral administration either solid or fluid unit dosage forms can be prepared.
[0024] Powders are prepared quite simply by comminuting the active ingredient to a suitably fine size and mixing with a similarly comminuted diluent. The diluent can be an edible carbohydrate material such as lactose or starch. Advantageously, a sweetening agent or sugar is present as well as a flavoring oil.
[0025] Capsules are produced by preparing a powder mixture as hereinbefore described and filling into formed gelatin sheaths. Advantageously, as an adjuvant to the filling operation, a lubricant such as talc, magnesium stearate, calcium stearate and the like is added to the powder mixture before the filling operation.
[0026] Soft gelatin capsules are prepared by machine encapsulation of a slurry of active ingredients with an acceptable vegetable oil, light liquid petrolatum or other inert oil or triglyceride.
[0027] Tablets are made by preparing a powder mixture, granulating or slugging, adding a lubricant and pressing into tablets. The powder mixture is prepared by mixing an active ingredient, suitably comminuted, with a diluent or base such as starch, lactose, kaolin, dicalcium phosphate and the like. The powder mixture can be granulated by wetting with a binder such as corn syrup, gelatin solution, methylcellulose solution or acacia mucilage and forcing through a screen. As an alternative to granulating, the powder mixture can be slugged, i.e., run through the tablet machine and the resulting imperfectly formed tablets broken into pieces (slugs). The slugs can be lubricated to prevent sticking to the tablet-forming dies by means of the addition of stearic acid, a stearic salt, talc or mineral oil. The lubricated mixture is then compressed into tablets.
[0028] Advantageously, the tablet can be provided with a protective coating consisting of a sealing coat or enteric coat of shellac, a coating of sugar and methylcellulose and polish coating of carnauba wax.
[0029] Fluid unit dosage forms for oral administration such as in syrups, elixirs and suspensions can be prepared wherein each teaspoonful of composition contains a predetermined amount of an active ingredient for administration.
[0030] The water-soluble forms can be dissolved in an aqueous vehicle together with sugar, flavoring agents and preservatives to form a syrup. An elixir is prepared by using a hydroalcoholic vehicle with suitable sweeteners together with a flavoring agent. Suspensions can be prepared of the insoluble forms with a suitable vehicle with the aid of a suspending agent such as acacia, tragacanth, methylcellulose and the like.
[0031] For parenteral administration, fluid unit dosage forms are prepared utilizing an active ingredient and a sterile vehicle, water being preferred. The active ingredient, depending on the form and concentration used, can be either suspended or dissolved in the vehicle. In preparing solutions the water-soluble active ingredient can be dissolved in water for injection and filter sterilized before filling into a suitable vial or ampule and sealing. Advantageously, adjuvants such as a local anesthetic, preservative and buffering agents can be dissolved in the vehicle. Parenteral suspensions are prepared in substantially the same manner except that an active ingredient is suspended in the vehicle instead of being dissolved and sterilization cannot be accomplished by filtration. The active ingredient can be sterilized by exposure to ethylene oxide before suspending in the sterile vehicle. Advantageously, a surfactant or wetting agent is included in the composition to facilitate uniform distribution of the active ingredient.
[0032] In addition to oral and parenteral administration, the rectal and vaginal routes can be utilized. An active ingredient can be administered by means of a suppository. A vehicle which has a melting point at about body temperature or one that is readily soluble can be utilized. For example, cocoa butter and various polyethylene glycols (Carbowaxes) can serve as the vehicle.
[0033] For intranasal installation, a fluid unit dosage form is prepared utilizing an active ingredient and a suitable pharmaceutical vehicle, preferably P.F. water, a dry powder, can be formulated when insulation is the administration of choice.
[0034] For use as aerosols, the active ingredients can be packaged in a pressurized aerosal container together with a gaseous or liquefied propellant, for example, dichlorodifluoromethane, carbon dioxide, nitrogen, propane, and the like, with the usual adjuvants such as cosolvents and wetting agents, as may be necessary or desirable. The term “unit dosage form” as used in the specification and claims refers to physically discrete units suitable as unitary dosages for human and animal subjects, each unit containing a predetermined quantity of active material calculated to produce the desired therapeutic effect in association with the required pharmaceutical diluent, carrier or vehicle. The specifications for the novel unit dosage forms of this invention are dictated by and are directly dependent on (a) the unique characteristics of the active material and the particular therapeutic effect to be achieved, and (b) the limitation inherent in the art of compounding such an active material for therapeutic use in humans, as disclosed in this specification, these being features of the present invention. Examples of suitable unit dosage forms in accord with this invention are tablets, capsules, troches, suppositories, powder packets, wafers, cachets, teaspoonfuls, tablespoonfuls, dropperfuls, ampules, vials, segregated multiples of any of the foregoing, and other forms as herein described.
[0035] The active ingredients to be employed as antineoplastic and/or antimicrobial agents can be easily prepared in such unit dosage form with the employment of pharmaceutical materials which themselves are available in the art and can be prepared by established procedures. The following preparations are illustrative of the preparation of the unit dosage forms of the present invention, and not as a limitation thereof. The following are examples of several dosage forms, in which the notation “active ingredient” signifies Cribrostatin 6.
COMPOSITION “A”
Hard-Gelatin Capsules
[0036] One thousand two-piece hard gelatin capsules for oral use, each capsule containing 200 mg of an active ingredient are prepared from the following types and amounts of ingredients:
Active ingredient, micronized 20 g Corn Starch 20 g Talc 20 g Magnesium stearate 2 g
[0037] The active ingredient, finely divided by means of an air micronizer, is added to the other finely powdered ingredients, mixed thoroughly and then encapsulated in the usual manner.
[0038] The foregoing capsules are useful for treating a neoplastic disease by the oral administration of one or two capsules one to four times a day.
[0039] Using the procedure above, capsules are similarly prepared containing an active ingredient in 5, 25, and 50 mg amounts by substituting 5 g, 25 g and 50 g of an active ingredient for the 20 g used above.
COMPOSITION “B”
Soft Gelatin Capsules
[0040] One-piece soft gelatin capsules for oral use, each containing 20 mg of an active ingredient, finely divided by means of an air micronizer, are prepared by first suspending the compound in 0.5 ml of corn oil to render the material capsulatable and then encapsulating in the above manner.
[0041] The foregoing capsules are useful for treating a neoplastic disease by the oral administration of one or two capsules one to four times a day.
COMPOSITION “C”
Tablets
[0042] One thousand tablets, each containing 20 mg of an active ingredient, are prepared from the following types and amounts of ingredients:
Active ingredient, micronized 20 g Lactose 300 g Corn starch 50 g Magnesium stearate 4 g Light liquid petrolatum 5 g
[0043] The active ingredient, finely divided by means of an air micronizer, is added to the other ingredients and then thoroughly mixed and slugged. The slugs are broken down by forcing them through a Number Sixteen screen. The resulting granules are then compressed into tablets, each tablet containing 20 mg of the active ingredient.
[0044] The foregoing tablets are useful for treating a neoplastic disease by the oral administration of one or two tablets one to four times a day.
[0045] Using the procedure above, tablets are similarly prepared containing an active ingredient in 25 mg and 10 mg amounts by substituting 25 g and 10 g of an active ingredient for the 20 g used above.
COMPOSITION “D”
Oral Suspension
[0046] One liter of an aqueous suspension for oral use, containing in each teaspoonful (5 ml) dose, 50 mg of an active ingredient, is prepared from the following types and amounts of ingredients:
Active ingredient, micronized 1 g Citric acid 2 g Benzoic acid 1 g Sucrose 790 g Tragacanth 5 g Lemon Oil 2 g Deionized water, q.s. 1000 ml
[0047] The citric acid, benzoic acid, sucrose, tragacanth and lemon oil are dispersed in sufficient water to make 850 ml of suspension. The active ingredient, finely divided by means of an air micronizer, is stirred into the syrup unit uniformly distributed. Sufficient water is added to make 1000 ml.
[0048] The composition so prepared is useful for treating a neoplastic disease at a dose of 1 teaspoonful (15 ml) three times a day.
COMPOSITION “E”
Parenteral Product
[0049] A sterile aqueous suspension for parenteral injection, containing 3 mg of an active ingredient in each milliliter for treating a neoplastic disease, is prepared from the following types and amounts of ingredients:
Active ingredient, micronized 3 g POLYSORBATE 80 5 g Methylparaben 2.5 g Propylparaben 0.17 g Water for injection, q. s. 1000 ml.
[0050] All the ingredients, except the active ingredient, are dissolved in the water and the solution sterilized by filtration. To the sterile solution is added the sterilized active ingredient, finely divided by means of an air rnicronizer, and the final suspension is filled into sterile vials and the vials sealed.
[0051] The composition so prepared is useful for treating a neoplastic disease at a dose of 1 milliliter (1 ml) three times a day.
COMPOSITION “F”
Suppository, Rectal and Vaginal
[0052] One thousand suppositories, each weighing 2.5 g and containing 20 mg of an active ingredient are prepared from the following types and amounts of ingredients:
Active ingredient, micronized 1.5 g Propylene glycol 150 g Polyethylene glycol #4000, q.s. 2,500 g
[0053] The active ingredient is finely divided by means of an air micronizer and added to the propylene glycol and the mixture passed through a colloid mill until uniformly dispersed. The polyethylene glycol is melted and the propylene glycol dispersion is added slowly with stirring. The suspension is poured into unchilled molds at 40° C. The composition is allowed to cool and solidify and then removed from the mold and each suppository foil wrapped.
[0054] The foregoing suppositories are inserted rectally or vaginally for treating a neoplastic disease.
COMPOSITION “G”
Intranasal Suspension
[0055] One liter of a sterile aqueous suspension for intranasal instillation, containing 2 mg of an active ingredient in each milliliter, is prepared from the following types and amounts of ingredients:
Active ingredient, micronized 1.5 g POLYSORBATE 80 5 g Methylparaben 2.5 g Propylparaben 0.17 g Deionized water, q.s. 1000 ml.
[0056] All the ingredients, except the active ingredient, are dissolved in the water and the solution sterilized by filtration. To the sterile solution is added the sterilized active ingredient, finely divided by means of an air micronizer, and the final suspension is aseptically filled into sterile containers.
[0057] The composition so prepared is useful for treating a neoplastic disease, by intranasal instillation of 0.2 to 0.5 ml given one to four times per day.
[0058] An active ingredient can also be present in the undiluted pure form for use locally about the cutis, intranasally, pharyngolaryngeally, bronchially, or orally.
COMPOSITION “H”
Powder
[0059] Five grams of an active ingredient in bulk form is finely divided by means of an air micronizer. The micronized powder is placed in a shaker-type container.
[0060] The foregoing composition is useful for treating a neoplastic disease, at localized sites by applying a powder one to four times per day.
COMPOSITION “I”
Oral Powder
[0061] One hundred grams of an active ingredient in bulk form is finely divided by means of an air micronizer. The micronized powder is divided into individual doses of 20 mg and packaged.
[0062] The foregoing powders are useful for treating a neoplastic disease, by the oral administration of one or two powders suspended in a glass of water, one to four times per day.
COMPOSITION “J”
Insufflation
[0063] One hundred grams of an active ingredient in bulk form is finely divided by means of an air micronizer. The foregoing composition is useful for treating a neoplastic disease, by the inhalation of 30 mg one to four times a day. It is of course understood that such modifications, alterations and adaptations as will readily occur to the artisan confronted with this disclosure are intended within the spirit of the present invention.
TABLE I High Field (500 MHz) NMR Assignments for Cribrostatin 6 (3), (3,8-dimethyl-9-ethoxy-imidazo[5,1-a]isoquinoline-7,10-dione) in CDCl 3 1 H HMBC GOESY δ(mult, 13 C j1xh = 140, mix = Position J, #H) and 15 N jnxh = 8 COSY .3 1 8.29s, 1H 125.68 C-3 2 3 137.64 4 5 7.90d, 124.73 C-3, C-6, H-6 H-6, 7.5Hz, 1H C-6a H-11 6 7.26d, 107.73 C-6a, C-7, H-5 7.5Hz, 1H C-10a 6a 125.00 7 184.86 8 130.06 9 156.16 10 180.58 10a 123.49 10b 123.87 11 2.75s, 3H 12.57 C-3 H-5 12 2.06s, 3H 9.15 C-7, C-8, C-9 13 4.40q, 69.64 C-9, C-14 H-14 6.9Hz, 2H 14 1.41t, 15.97 C-13 H-13 6.8Hz, 3H N-4 189.5 N-2 273.9
[0064]
TABLE II
Cribrostatin 6 (3) Inhibitory Activity (GI 50 , μg/ml) Against
a Panel of Human Cancer Cell Lines and Mouse Leukemia
Cell Type
Cell Line
Cribrostatin-6
Pancreas-adenocarcinoma
BXPC-3
>1
Breast-adenocarcinoma
MCF-7
0.21
CNS Glioblastoma
SF-268
0.24
Lung-NSC
NCI-H460
>1
Colon-adenocarcinoma
KM20L2
>1
Prostate
DU-145
0.38
Mouse Leukemia
P388
0.29
[0065]
TABLE III
Antimicrobial Activities of Cribrostatin 6.
Minimum Inhibitory
Concentration
Microorganism
(μg/ml)
Candida albicans (ATCC 90028)
64
Cryptococcus neoformans (ATCC 90112)
2
Micrococcus luteus (Presque Isle 456)
16
Staphylococcus aureus (ATCC 29213)
16
Methicillin-resistant S. aureus
16
(clinical isolate)
Enterococcus faecalis (ATCC 29212)
32
Vancomycin-resistant E. faecalis
32
(clinical isolate)
Bacillus subtilis (clinical isolate)
2
Streptococcus pneumoniae (ATCC 6303)
0.5
Penicillin-resistant S. pneumoniae
2
(clinical isolate)
Invasive S. pneumoniae (clinical isolate)
1
Group A Streptococcus (clinical isolate)
16
Stenotrophomonas maltophilia (ATCC 13637)
>64
Escherichia coli (ATCC 25922)
>64
Enterobacter cloacae (ATCC 13047)
>64
Neisseria gonorrhoeae (ATCC 49226)
0.0625
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Cribrostatin 6, a dark blue cancer cell growth inhibiting constituent of the Republic of Maldives marine sponge Cribrochalina sp. has been isolated, and its structure (shown below) elucidated, based on a combination of RMS, high field (500 MHz, HMBC, and GOESY experiments) 15N, 1 H- and 13C NMR, and X-ray crystal structure analyses. Cribrostatin 6 also was found to inhibit the growth of a number of pathogenic bacteria and fungi.
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FIELD OF THE INVENTION
This invention relates to a loading hose for use in a paper machine doctor or coating device, which loading hose lies between the doctor's or coating device's blade supports and rotatable blade holder. The loading hose is arranged to load the blade of the doctor or the coating blade of the coating device, and has a flexible, pressure-resistant casing of uniform cross-section.
BACKGROUND OF THE INVENTION
In a hose-loaded doctor in a paper machine, the contact force of the doctor blade on the surface of the roll being cleaned, or, in coating devices, the contact force of the coating blade on the surface being coated, is increased by means of loading hoses acting on the blade holder. Generally, two loading hoses are used in the blade holders in question. The parts of the doctor and the loading hoses are arranged so that one loading hose loads the blade and the other releases it. The return movement loading hose can also be used to create a counter-pressure, allowing a higher and more easily regulated pressure to be used in the loading hose. This is important, because the essential factor in adjustment and loading is the pressure difference, and not the pressure level. The usual pressure medium is air.
Loading hoses normally have an oval cross-section. The loading hose is set between the turning blade holder and its support. Generally, the loading hose is supported by its widest sides against the support surfaces. Over a certain distance, the loading hose operates as desired, in other words, the thickness of the hose increases, while its width remains essentially the same. However, in known loading hoses, this operational distance is short, and, as the distance between the support surfaces increases further, the loading hose assumes an increasingly round shape. In this case, the force created by the loading hose suddenly drops, which is extremely disadvantageous in terms of loading. In addition, known loading hoses are flexible in all directions, so that when the loading varies they move between the blade holder and the support and can even hang partly outside these. This causes variations in the loading force over the length of the doctor. In addition, when the blade returns, the part of the loading hose that is hanging loosely can be squeezed, and even broken, between the parts of the doctor or coating device.
SUMMARY OF THE INVENTION
The present invention provides a new type of loading hose for use in the doctor or coating device of a paper machine, which eliminates the defects of the prior art and creates the desired loading profile in the blade.
More specifically, the present invention provides a loading hose for use in a paper machine doctor or coating device, which loading hose is located between the doctor's or coating device's blade support and rotatably arranged blade holder. The loading hose is arranged to load the doctor blade of the doctor or the coating blade of the coating device, and incorporates a flexible casing, which is pressure-resistant and of a uniform cross-section. The loading hose includes at least one stiffening member attached to the casing, which is arranged to lie against one of the blade support or the blade holder.
The stiffening member comprises stiffening plates, at least one of which is manufactured from a composition material to create a friction or sliding effect. Alternatively, the stiffening member comprises stiffening plates, on top of one of which a layer is arranged to create a friction or sliding effect. The layer may comprise friction or sliding plates, which are narrower than the stiffening plate or the friction or sliding plates may comprise at least two narrow parts.
In yet another arrangement the layer is a surfacing.
Additional plates may be provided inside the loading hose at the location of the stiffening members, the width of which is essentially the same as that of the stiffening members.
Part of the cross-section of a loading hose according to the invention is rigid, so that it cannot become detrimentally rounded. The hose is also stiff enough longitudinally to ensure that it remains in place, even if contact is lost with the support surfaces. This makes it less probable that the hose will hang loosely and be broken. In addition, there is less variation in the level of force arising from changes in the distance between the moment point and the loading hose. The loading profile of the blade also remains as desired over the entire length of the doctor or coating device while the installation of the loading hose is facilitated. In addition, the friction properties of the loading hose can be altered if required, which also facilitates installation, among other things.
These and other features and advantages of the invention will be more fully understood from the following detailed description of the invention taken together with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a side view of a hose-loaded doctor, illustrating cross-sections of loading hoses according to the invention installed in it; and
FIGS. 2-4 are cross-sectional views of various embodiments of the loading hose according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawings in detail, FIG. 1 shows a side view of a conventional hose-loaded doctor. The doctor includes a blade holder 10 and blade support 11 , which is attached to the frame of the doctor (not shown) . The actual doctor blade 12 is fitted to blade holder 10 , and is used to doctor the surface of roll 13 . In a hose-loaded doctor, blade holder 10 is jointed to rotate in blade support 11 , while loading hoses 14 are located between them. Loading hoses 14 are used to rotate doctor blade 12 in relation to joint 15 .
Compressed air is fed to loading hoses 14 , later referred to simply as hoses, when they thicken and thus create a force in their counter-surfaces. Here, the counter-surfaces are the blade holder 10 and the blade support 11 . Usually, the actual loading hose is further from the doctor blade and the return hose is closer to it. Normally, both hoses are of the same kind, so that there are as few hose models as possible in use and it is possible to change the hoses around.
Though hoses 14 are not actually attached to blade support 11 , their movement is nevertheless restricted. Suitably shaped blade support 11 and blade holder 10 limit the space available to hoses 11 , and, if necessary, various kinds of stops 16 , 16 ′ are used to hold hoses 14 in place. The movement created in the doctor blade by the hoses is relatively short, so that the entire doctor blade is usually jointed to rotate. This allows the doctor to be moved a sufficient distance from the roll, for example, when changing the roll. By turning the doctor backwards a short distance from the roll, it is possible to use the hoses to finally load the doctor blade with a suitable and adjustable force. If necessary, the return hose can be used to lift the doctor blade off the surface of the roll.
FIGS. 2-4 show cross-sections of various embodiments of a loading hose according to the present invention. According to the invention, loading hose 14 includes at least one stiffening member 18 attached to casing 17 , which is arranged to lie against either blade support 11 or blade holder 10 . The counter-surfaces can be suitably shaped to partly eliminate the rounding of the hose, in which case a single stiffening member is sufficient. Preferably, however, stiffening members 18 are attached to both sides of the casing 17 of hose 14 . Thus, hose 14 cannot become detrimentally rounded, so that no sudden changes will take place in the loading profile of doctor blade 12 . In the same way, hose 14 will also be stiffened longitudinally, making it easier to install. Hose 14 also remains in place better and parallel to the doctor. Stiffening members 18 are preferably attached by gluing. One of the stiffening members 18 is arranged to lie on blade support 11 and the other on blade holder 10 (FIG. 1 ). Thus, when the pressure is increased, only the thickness of hose 14 increases, so that the loading acts in the correct direction. The casing of the hose can bulge outward, as is usually the case. Alternatively, there may be folds in casing 17 according to the examples, so that its width remains nearly constant while its thickness changes. The stiffening members cover most of the circumference of the hose. If the width of the stiffening members is increased, however, the operating movement of the hose will correspondingly shorten. The optimum width is determined for each individual case. The casing of the hose itself is resistant to pressure and thus airtight.
FIG. 2 shows the basic model of the loading hose according to the invention. Here, stiffening plates 19 are attached to both sides of casing 17 , and prevent hose 14 from becoming rounded. Stiffening plate 19 can be, for instance, made from fibre-reinforced plastic, in which staple or oriented reinforcing fibers are used. FIG. 3 shows the next embodiment of hose 14 . Generally, the stiffening members 18 comprise stiffening plates 19 , of which either one or both are manufactured from composition material, to provide friction or sliding characteristics. Here, the upper stiffening member is made from a composition material. The use of a composition material mainly affects the friction and sliding characteristics of the stiffening plate, as well as its wear resistance. This allows the hose to be made as required either to remain in place as firmly as possible or to slide as easily as possible in relation to its counter-surface. For example, in oscillation embodiments, the properties of the stiffening members can be selected to give a high degree of friction between the blade support and the corresponding stiffening member. Similarly, there can be low friction between the blade holder and the corresponding stiffening member. Thus, the hose will remain firmly in place and not hang loosely. The blade holder will, however, slide easily over the upper surface of the hose. In holder oscillations, this will reduce both the force required for the oscillation and the wear in the hose.
Besides a composition material, separate layers can also be used to create a friction or sliding effect. A friction or sliding effect refers not only to the desired slipping or grip of the stiffening plate, but also its resistance to wear. In practice, such stiffening members are formed by stiffening plates, on the surface of one or other of which the aforesaid layer is arranged. In FIG. 4, the upper layer is formed by friction or sliding plate 20 , which is narrower that stiffening plate 19 . Correspondingly, the lower friction or sliding plate 20 ′ is formed of two parts. The friction or sliding plate can also comprise several parts or be as wide as the stiffening plate. By using friction or sliding plates of varying width, it is possible to vary the friction and sliding properties and loading points of the hose. In addition, a full-width friction or sliding plate will increase the stiffness of the hose. Alternatively, the aforesaid layer can be a surfacing 21 (FIG. 3 ). For example, the surfacing can be fluor and PTFE plastics, so that the stiffened surface can be made slippery. Surfacing can also be used to increase friction. It is easy to add a surfacing on top of the stiffening plate while scarcely increasing the total weight of the hose.
Inside the hose in FIG. 4, there are also corresponding additional plates 22 at the locations of stiffening members 18 . The additional plates are essentially the same width as the stiffening members. In this case, the internal pressure of the hose presses the additional plates 22 against the stiffening plates 19 , increasing the retention of the stiffening plates 19 . The effect of additional plates 22 is great precisely at the edges of stiffening plates 19 , where the greatest stress arises in the gluing, when hose 14 expands. The additional plates 22 do not require particularly strong attachment, as the pressure pushes them against casing 17 .
A loading hose according to the invention remains firmly in place and is easy to install. In addition, there are no sudden changes in the doctor blade loading profile created by the hose, so that the loading can be precisely adjusted over the entire operating area of the hose-loaded doctor. In the case of the friction or sliding plates and additional plates, various combinations can be made as required. However, a loading hose according to the invention always includes at least one stiffening member attached to the casing, to prevent rounding.
Although the invention has been described by reference to a specific embodiment, in connection with doctors and doctor blades, it should be understood that numerous changes may be made within the spirit and scope of the inventive concepts described such as being equally suitable for use in connection with hose-loaded coating devices and their coating blades.
Accordingly, it is intended that the invention not be limited to the described embodiments, but that it have the full scope defined by the language of the following claims.
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A loading hose for use in a paper machine doctor or coating device, which loading hose is located between the doctor's or coating device's blade support and rotatably arranged blade holder, is arranged to load the doctor blade of the doctor or the coating blade of the coating device. The loading hose incorporates a flexible casing, which is pressure-resistant and of a uniform cross-section. The loading hose includes at least one stiffening member attached to the casing and arranged to lie against either the blade support or the blade holder.
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CROSS RELATED APPLICATION
[0001] This application is a continuation of U.S. patent application Ser. No. 10/478,718 filed Nov. 24, 2003, which is a U.S. national phase of international application PCT/IL02/00402, filed in English on 22 May 2002, which designated the US. PCT/IL02/00402 claims priority to IL Application No. 143318, filed 23 May 2001. The entire contents of these applications are incorporated herein by reference
FIELD OF THE INVENTION
[0002] The present invention relates to herbal compositions useful for the treatment of mucosal lesions. Although primarily intended for oral use the composition may also be used on the labial, genital and other mucosal surfaces, as well as on the skin.
BACKGROUND OF THE INVENTION
[0003] Historically, the plant world has been the most important source of medicinal agents for the treatment of human and animal disease, and for use as preventative agents in maintaining good health. However, for at least the last 150 years, Western medicine has been dominated by synthetic and/or highly purified chemical agents.
[0004] It is now being increasingly recognized, however, that plant extracts may be highly effective agents for the prevention and treatment of disease. This is particularly true when one considers the low toxicity and greatly reduced incidence of adverse effects associated with plant-based medicines as compared with many synthetic or highly purified drugs. In addition, as the plant possesses a large number of pharmaceutically active agents, extracts obtained therefrom exert their activities on a variety of physiologic processes, increasing the range of the desired therapeutic effect.
[0005] Although traditional reference sources of herbal medicine are valuable guides to the safe and effective use of plant extracts, the appropriate selection and combination of extracted material is still a major challenge to the development of new, highly effective herbal medicines. The scale of this challenge may be more clearly appreciated when it is realized that there are approximately 750,000 species of flowering plants on earth, only very few of which have been scientifically studied for their potential therapeutic value.
[0006] Oral diseases constitute a diverse group of conditions that are responsible for much human suffering. In addition to diseases of the hard tissues of the oral cavity (e.g. dental caries), there are many different pathological conditions affecting the oral mucosa and periodontal tissues. This group includes the commonly found conditions such as gingivitis, periodontal disease, aphthous ulceration and Herpes simplex lesions, as well as the oral manifestations of the less common vesicular-bullous conditions such as bullous pemphigoid, pemphigus, erytheme multiforme and lichen planus, as well as other autoimmune conditions.
[0007] The significance of host-related factors in the pathogenesis of conditions such as periodontal disease is being increasingly recognized. Far from being a passive recipient of pathogenic agents released by plaque bacteria, the host tissues themselves (including the biochemical and immunological factors contained therein) are now known to make an active contribution to disease initiation and progression. One group of host factors which have recently received some attention in relation to the pathogenesis of periodontal disease is the group consisting of various tissue-destroying and tissue-remodelling enzymes. Of particular interest is the large group of matrix metalloproteinases (Page, R. C. (1999) J. Periodont. Res. 34: 331-339). It is now believed that certain, defined, metalloproteinases such as matrix metalloproteinases 1-9 are of particular importance for the development and progression of periodontal disease.
[0008] Although many pharmaceutical agents have been used in the management of mucosal lesions, many of these have been relatively ineffective, while some (in particular, the systemic regimes) are associated with unacceptable adverse effects. There thus exists a need for new, efficacious and safe modes of treatment for many of the aforementioned mucosal diseases. There is a particular need for a safe, effective topical treatment.
[0009] It is a purpose of the present invention to respond to the aforementioned need by providing plant-based compositions for the treatment of mucosal diseases.
[0010] It is another purpose of the invention to provide plant-based anti-viral compositions for use in the treatment of oral and genital lesions.
[0011] It is a further purpose of the invention to provide compositions for the treatment of mucosal diseases having higher efficacy and more rapid onset than compositions previously known in the art.
[0012] It is a still further purpose of the invention to provide compositions having lower toxicity and incidence of adverse effects than pharmaceutical compositions for the treatment of mucosal diseases that have been previously described in the art.
[0013] Further objects and advantages of the present invention will become apparent as the description proceeds.
SUMMARY OF THE INVENTION
[0014] It has now been unexpectedly found that certain compositions comprising particular combinations of plant extracts are highly effective in the treatment of certain mucosal lesions, particularly those of the oral, anal and genital mucosa, as well as in the treatment of certain skin lesions. It is to be noted that the compositions, medicaments and treatment methods of the present invention which will presently be disclosed, described and exemplified, have been unexpectedly found to cause a dramatic improvement in two significant clinical parameters associated with the mucosal and skin lesions being treated thereby. Firstly, it has been surprisingly found that said compositions, medicaments and treatment methods lead to unexpectedly rapid resolution of the mucosal and skin lesions that are being treated. Secondly, the compositions, medicaments and treatment methods of the present invention have also been surprisingly found to cause a dramatic reduction of the pain associated with the mucosal and skin lesions being treated thereby.
[0015] The present invention is primarily directed to a therapeutic composition comprising extracts of the plant species Echinacea purpurea and Sambucus nigra and the extract(s) of at least one further plant selected from the group consisting of Hypericum perforatum, Commiphora molmol and Centella asiatica.
[0016] In one preferred embodiment of the therapeutic composition of the present invention, the extract(s) of the at least one further plant are extracts of the plant species Hypericum perforatum and Commiphora molmol.
[0017] While it is not intended that the use of the composition of the abovementioned preferred embodiment of the composition of the invention be bound to, or limited by any particular theory regarding its chemical or pharmacological mode of action, the present invention is particular directed to an anti-viral composition comprising extracts of the plant species Echinacea purpurea, Sambucus nigra, Hypericum perforatum and Commiphora molmol.
[0018] In a preferred embodiment of the invention, the above-mentioned anti-viral composition further comprises extracts of plants selected from the group consisting of Uncaria tomentosa, Thymus vulgaris, Matricaria recutita, Salix alba, Calendula officinalis, Usnea barbata, Ligusticum porterii - osha, Gaultheria procumbens, Camellia sinensis, Vaccinium myrtillus, Melissa officinalis, Allium sativum, Camellia sinensis and Krameria triandra.
[0019] In a particularly preferred embodiment of the invention, the above-mentioned anti-viral composition comprises extracts of the plant species Echinacea purpurea, Sambucus nigra, Hypericum perforatum, Commiphora molmol and Uncaria tomentosa.
[0020] The present invention also provides a therapeutic composition comprising extracts of the plant species Echinacea purpurea and Sambucus nigra together with an extract of the plant species Centella asiatica.
[0021] In a preferred embodiment of the invention, the immediately preceding therapeutic composition is intended for use in the treatment of diseases of the oral mucosa. In a more preferred embodiment of the invention, said therapeutic composition is intended for use in the treatment of an oral mucosal disease selected from the group consisting of periodontal disease, gingivitis, aphthous ulceration, mechanical trauma, thermal trauma, lichen planus, bullous pemphigoid, pemphigus vulgaris, dermatitis herpetiformis, angular chelitis and recurrent herpes.
[0022] In a further preferred embodiment, the above therapeutic composition is intended for use in the treatment of skin lesions. In one preferred embodiment of the invention, said therapeutic composition is intended for use in the treatment of dermal trauma. In another preferred embodiment, the therapeutic composition is intended for use in the treatment of insect bites and other local, superficial irritations.
[0023] In a still further preferred embodiment of the invention, the above therapeutic composition is intended for use in the treatment of anal lesions. In a more preferred embodiment of the invention, said therapeutic composition is intended for use in the treatment of an anal lesion associated with a condition selected from the group consisting of anal fissures, hemorrhoids and non-specific irritation.
[0024] While it is not intended that the mechanism of action of the therapeutic composition for treating mucosal diseases that is disclosed immediately hereinabove be bound to any particular pharmacological or pathophysiological mechanism or mechanisms, it is believed that said composition exerts at least some of its desired effects by inhibiting one or more matrix metalloproteinase (MMP) enzymes that are present in the oral mucosal and periodontal tissues, and/or by increasing collagen production at or close to the mucosal site to which said composition is applied. In particular, it is believed that said therapeutic compositions may exert at least some of their desired effects by the specific inhibition of certain specific enzymes of the MMP group. More specifically, it is believed that the therapeutic compositions of the present invention are specific inhibitors of MMP subclasses 1-9, still more specifically of subclasses 1, 2, 8 and 9.
[0025] Thus, the invention is also directed to a therapeutic composition comprising extracts of the plant species Echinacea purpurea, Sambucus nigra and Centella asiatica described hereinabove, for the inhibition of one or more matrix metalloproteinases.
[0026] It is to be noted that the term “inhibition of one or more matrix metalloproteinases” as used immediately hereinabove and hereinabove is intended to convey the meaning of the inhibition of the activity of these enzymes on their substrates.
[0027] In a preferred embodiment of this aspect of the invention, the one or more matrix metalloproteinases to be inhibited are selected from the group consisting of matrix metalloproteinases 1-9. In a more preferred embodiment, said one or more matrix metalloproteinases are selected from the group consisting matrix metalloproteinases 1, 2, 8 and 9. Still more preferably, the matrix metalloproteinase to be inhibited is matrix metalloproteinase 2. In a still further preferred embodiment of this aspect of the present invention, the matrix metalloproteinase-inhibiting therapeutic compositions described immediately hereinabove are intended for use in the treatment of a disease of the oral mucosa selected from the group consisting of periodontal disease and aphthous ulceration.
[0028] In a further preferred embodiment of the invention, the aforementioned therapeutic compositions for treating conditions of the oral or anal mucosal tissues, as well as the aforementioned therapeutic compositions for inhibiting matrix metalloproteinases further comprise extracts of plants selected from the group consisting of Uncaria tomentosa, Thymus vulgaris, Matricaria recutita, Salix alba, Calendula officinalis, Usnea barbata, LigustLicum porterii - osha, Gaultheria procumbens, Camellia sinensis, Vaccinium myrtlillus, Melissa officinalis, Allium satlivum, Camellia sinensis and Krameria triandra.
[0029] In another aspect, the present invention is directed to the use of a combination of extracts of the plant species Echinacea purpurea and Sambucus nigra and of at least one further plant species selected from the group consisting of Hypericum perforatum, Commiphora molmol and Centella asiatica in the preparation of a medicament.
[0030] In one preferred embodiment, the invention is directed to the use of the combination of plant extracts described immediately hereinabove in the preparation of a medicament, wherein said extracts of at least one further plant are extracts of Hypericum perforatum and Commiphora molmol . Preferably, this combination of plant extracts is used in the preparation of an anti-viral medicament.
[0031] In a further preferred embodiment, the present invention is directed to the use of extracts of plants selected from the group consisting of Uncaria tomentosa, Thymus vulgaris, Matricaria recutita, Salix alba, Calendula officinalis, Usnea barbata, Ligusticum porterii - osha, Gaultheria procumbens, Camellia sinensis, Vaccinium myrtillus, Melissa officinalis, Allium sativum, Camellia sinensis and Krameria triandra , in addition to the extracts mentioned hereinabove, in the preparation of an anti-viral medicament.
[0032] In a particularly preferred embodiment the present invention is directed to the use of a combination of extracts of the plant species Echinacea purpurea, Sambucus nigra, Hypericum perforatum, Commiphora molmol and Uncaria tomentosa in the preparation of an anti-viral medicament.
[0033] The present invention also provides for the use of the above combination of plant extracts in the preparation of a medicament, said extract of at least one further plant being an extract of Centella asiatica . Preferably, this combination of plant extracts is used in the preparation of a medicament for the treatment of a disease of the oral mucosa. In one embodiment of the invention, said disease of the oral mucosa is selected from the group consisting of periodontal disease, gingivitis, aphthous ulceration, mechanical trauma, thermal trauma, lichen planus, bullous pemphigoid, pemphigus vulgaris, dermatitis herpetiformis, angular chelitis and recurrent herpes.
[0034] In another preferred embodiment, the invention also provides for the use of the above combination of plant extracts in the preparation of a medicament for the treatment of a skin lesion. In one preferred embodiment, the skin lesion to be treated is a lesion arising from dermal trauma. In a further preferred embodiment, the skin lesion to be treated is an insect bite.
[0035] In another preferred embodiment of the invention, the abovementioned combination of plant extracts is used in the preparation of a medicament for the treatment of a disease of the anal mucosa. In one embodiment of the invention, said disease of the anal mucosa is selected from the group consisting of anal fissures, hemorrhoids and non-specific irritation.
[0036] In another aspect the invention provides for the use of a combination of extracts of the plant species Echinacea purpurea, Sambucus nigra and Centella asiatica in the preparation of a medicament for inhibiting one or more matrix metalloproteinases. Preferably, said matrix metalloproteinases are selected from the group consisting of matrix metalloproteinases 1 to 9. Most preferably, the one or more matrix metalloproteinases to be inhibited are selected from the group consisting of matrix metalloproteinases 1, 2, 8 and 9. In a preferred embodiment, the abovementioned metalloproteinase-inhibiting medicament is used to treat a disease of the oral mucosa selected from the group consisting of periodontal disease and aphthous ulceration.
[0037] In a further preferred embodiment, the invention is directed to the use of the above combination of plant extracts in combination with further extracts of plants selected from the group consisting of Uncaria tomentosa, Thymus vulgaris, Matricaria recutita, Salix alba, Calendula officinalis, Usnea barbata, Ligusticum porterii - osha, Gaultheria procumbens, Camellia sinensis, Vaccinium myrtillus, Melissa officinalis, Allium sativum, Camellia sinensis and Krameria triandra , in the preparation of medicaments for the treatment of a diseases of the oral and/or anal mucosal tissues, and in the preparation of medicaments for inhibiting the abovementioned one or more matrix metalloproteinases.
[0038] In another aspect, the present invention is directed to a combination of extracts of the plant species Echinacea purpurea and Sambucus nigra and of at least one further plant species selected from the group consisting of Hypericum perforatum, Commiphora molmol and Centella asiatica for use as a medicament.
[0039] In a preferred embodiment, the invention is directed to a combination of extracts as disclosed immediately hereinabove, wherein the extracts of the at least one further plant are extracts of Hypericum perforatum and Commiphora molmol . In a preferred embodiment, the invention is directed to said combination of extracts for use as an anti-viral medicament. In a further preferred embodiment, said combination of extracts is further supplemented by extracts of one or more plants selected from the group consisting of Uncaria tomentosa, Thymus vulgaris, Matricaria recutita, Salix alba, Calendula officinalis, Usnea barbata, Ligusticum porterii - osha, Gaultheria procumbens, Camellia sinensis, Vaccinium myrtillus, Melissa officinalis, Allium sativum, Camellia sinensis and Krameria triandra.
[0040] In a particularly preferred embodiment, the invention is directed to a combination of extracts of the plant species Echinacea purpurea, Sambucus nigra, Hypericum perforatum, Commiphora molmol and Uncaria tomentosa for use as an anti-viral medicament.
[0041] The invention also provides a combination of plant extracts as disclosed hereinabove for use as a medicament, said extract of the at least one further plant being an extract of Centella asiatica . Preferably, this combination of extracts is provided for use as a medicament for the treatment of diseases of the oral mucosa. While said combination of plant extracts may be used as a medicament for the treatment of many different conditions of the oral mucosa, in a preferred embodiment, the disease to be treated is selected from the group consisting of periodontal disease, gingivitis, aphthous ulceration, mechanical trauma, thermal trauma, lichen planus, bullous pemphigoid, pemphigus vulgaris, dermatitis herpetiformis, angular chelitis and recurrent herpes. In another preferred embodiment, the combination of plant extracts is provided for use as a medicament for the treatment of skin lesions. In one preferred embodiment, the skin lesions are lesions arising from dermal trauma. In another preferred embodiment, the skin lesions are insect bites. In yet another preferred embodiment, the aforementioned combination of extracts is provided for use as a medicament for the treatment of diseases of the anal mucosa. While said combination of plant extracts may be used as a medicament for the treatment of many different conditions of the anal mucosa, in a preferred embodiment, the disease to be treated is selected from the group consisting of anal fissures, hemorrhoids and non-specific irritation.
[0042] In another aspect, the above-described combination of extracts is used as a medicament for inhibiting one or more matrix metalloproteinases. Preferably, the one or more matrix metalloproteinases are selected from the group consisting of matrix metalloproteinases 1 to 9. More preferably, said metalloproteinases are selected from the group consisting of matrix metalloproteinases 1, 2, 8 and 9. In a preferred embodiment, the abovementioned combination of extracts for inhibiting metalloproteinases is used in the treatment of a disease of the oral mucosa selected from the group consisting of periodontal disease and aphthous ulceration.
[0043] In yet another embodiment of the invention, the plant extracts used in the aforementioned combination of extracts are further supplemented by extracts of plants selected from the group consisting of Uncaria tomentosa, Thymus vulgaris, Matricaria recutita, Salix alba, Calendula officinalis, Usnea barbata, Ligusticum porterii - osha, Gaultheria procumbens, Camellia sinensis, Vaccinium myrtillus, Melissa officinalis, Allium sativum, Camellia sinensis and Krameria triandra.
[0044] The present invention also encompasses a method of treatment of mucosal and/or skin lesions comprising the application of a therapeutically-effective amount of a mixture of extracts of the plant species Echinacea purpurea and Sambucus nigra and the extract(s) of at least one further plant selected from the group consisting of Hypericum perforatum, Commiphora molmol and Centella asiatica to the mucosal lesions and surrounding tissue of a subject in need of such treatment. In a preferred embodiment of this method of treatment, said extracts of at least one further plant are extracts of Hypericum perforatum and Commiphora molmol . In a preferred embodiment, the lesions to be treated by this method of treatment are viral lesions.
[0045] In a further preferred embodiment, the present invention also provides a method of treatment of viral lesions as described hereinabove, wherein the aforementioned plant extracts are supplemented by extracts of plants selected from the group consisting of Uncaria tomentosa, Thymus vulgaris, Matricaria recutita, Salix alba, Calendula officinalis, Usnea barbata, Ligusticum porterii - osha, Gaultheria procumbens, Camellia sinensis, Vaccinium myrtillus, Melissa officinalis, Allium sativum, Camellia sinensis and Krameria triandra.
[0046] In a particularly preferred embodiment, the present invention provides a method of treatment of mucosal and/or skin lesions of viral origin comprising the application of a therapeutically-effective amount of a mixture of extracts of the plant species Echinacea purpurea, Sambucus nigra, Hypericum perforatum, Commiphora molmol and Uncaria tomentosa.
[0047] In another preferred embodiment of the method of the invention, the extract of the at least one further plant is an extract of Centella asiatica . In one preferred embodiment of this aspect of the invention, the lesions to be treated are oral lesions associated with a disease selected from the group consisting of periodontal disease, gingivitis, aphthous ulceration, mechanical trauma, thermal trauma, lichen planus, bullous pemphigoid, pemphigus vulgaris, dermatitis herpetiformis, angular chelitis and recurrent herpes. In another preferred embodiment, the lesions to be treated are skin lesions. In one more preferred embodiment, the skin lesions to be treated are lesions arising from dermal trauma. In a further preferred embodiment, the lesions are insect bites. In another preferred embodiment of this aspect of the invention, the lesions to be treated are anal lesions associated with a disease selected from the group consisting of anal fissures, hemorrhoids and non-specific irritation.
[0048] In a further aspect, the present invention is directed to a method of inhibiting one or more matrix metalloproteinases in mucosal and/or skin lesions of a subject in need of such treatment, comprising the application of a therapeutically-effective amount of a mixture of extracts of the plant species Echinacea purpurea, Sambucus nigra and Centella asiatica to said mucosal and/or skin lesions and surrounding tissue. Preferably, the one or more matrix metalloproteinases are selected from the group consisting of matrix metalloproteinases 1 to 9. More preferably, the one or more matrix metalloproteinases are selected from the group consisting of matrix metalloproteinases 1, 2, 8 and 9. In a preferred embodiment of this aspect of the invention, the aforementioned inhibition of the one or more matrix metalloproteinases is used in the treatment of periodontal disease. In another preferred embodiment, the inhibition of the one or more matrix metalloproteinases is used in the treatment of aphthous ulceration.
[0049] In each of the above-described methods, the mixture of plant extracts used may further comprise extracts of plants selected from the group consisting of Gotu kola, Uncaria tomentosa, Thymus vulgaris, Matricaria recutita, Salix alba, Calendula officinalis, Usnea barbata, Ligusticum porterii - osha, Gaultheria procumbens, Camellia sinensis, Vaccinium myrtillus, Melissa officinalis, Allium sativum, Camellia sinensis and Krameria triandra.
[0050] In one preferred embodiment of the invention, the anti-viral compositions, medicaments and treatment methods are used in the treatment or management of viral lesions of the oral cavity.
[0051] In another preferred embodiment of the invention, the anti-viral compositions, medicaments and treatment methods are used in the treatment or management of perioral lesions of viral origin.
[0052] In yet another preferred embodiment of the invention, the anti-viral compositions, medicaments and treatment methods are used in the treatment or management of genital lesions of viral origin.
[0053] In yet another preferred embodiment of the invention, the anti-viral compositions, medicaments and treatment methods are used in the treatment or management of viral lesions caused by the Herpes simplex virus.
[0054] In yet another preferred embodiment of the invention, the anti-viral compositions, medicaments and treatment methods are used in the treatment or management of viral lesions of the skin.
[0055] In another aspect, the present invention also encompasses a method for inhibiting one or more matrix metalloproteinases in vitro, comprising contacting an effective amount of a mixture of extracts of the plant species Echinacea purpurea, Sambucus nigra and Centella asiatica with said one or more matrix metalloproteinases. In one embodiment of this aspect of the invention, the one or more matrix metalloproteinases to be inhibited are selected from the group consisting of matrix metalloproteinases 1 to 9. In another embodiment, the one or more matrix metalloproteinases to be inhibited are selected from the group consisting of matrix metalloproteinases 1, 2, 8 and 9.
[0056] All the above and other characteristics and advantages of the present invention will be further understood from the following illustrative and non-limitative examples of preferred embodiments thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
[0057] FIG. 1 graphically illustrates the reduction in ulcer-associated pain following treatment with an herbal composition of the invention.
[0058] FIG. 2 shows a typical gelatin zymogram indicating the inhibitory effects of composition of the invention on the activity of a mixture of matrix metalloproteinases.
[0059] FIG. 3 graphically illustrates the reduction in insect bite-associated pain and irritation following treatment with an herbal composition of the invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0060] The compositions and medicaments of the present invention are based on mixtures of plant extracts. It is to be noted that the term “extract” is used herein to include all of the many types of preparations containing some or all of the active ingredients found in the relevant plants. Thus the extracts may be produced by cold extraction techniques using a variety of different extraction solvents including, but not limited to, water, fatty solvents (such as olive oil), and alcoholic solvents (e.g. 70% ethanol). Cold extraction techniques are usefully applied to softer parts of the plant such as leaves and flowers, or in cases wherein the desired active components of the plant are heat labile. Alternatively, the aforementioned solvents may be used to produce extracts of the desired plants by a hot extraction technique, wherein said solvents are heated to a high temperature, the precise value of said temperature being dependent on the properties of the chosen solvent, and maintained at that temperature throughout the extraction process. Hot extraction techniques are more commonly applied to the harder, tougher parts of the plant, such as bark, woody branches and larger roots. In some cases, sequential extractions need to be performed in more than one solvent, and at different temperatures.
[0061] Standard procedures for producing plant extracts (including hot extraction, cold extraction and other techniques) are described in many publications including “Medicinal plants: a field guide to the medicinal plants of the Land of Israel (in Hebrew), author: N. Krispil, Har Gilo, Israel, 1986” and “Making plant medicine, author: R. Cech, pub. by Horizon Herbs, 2000”.
[0062] Compositions and medicaments containing mixtures of extracts of different plant species, such as those of the present invention may be prepared using different ratios of each extract. For example, the antiviral medicaments and compositions of the present invention preferably comprise extracts of Echinacea purpurea, Sambucus nigra, Commiphora molmol and Hypericum perforatum in the following range of weight ratios:
2-6:2-4: 3-6:2-6
[0064] More preferably, these components are present in the weight ratio of 4:3:5:4.
[0065] Similarly, the compositions of the invention used to treat mucosal diseases preferably comprise extracts of Centella asiatica, Echinacea purpurea and Sambucus nigra in the following range of weight ratios:
[0000] 0.5-3:0.5-3:2:15
[0066] More preferably, these extracts are present in the weight ratio of 1.5:1.5:7
[0067] In order to treat a patient with a therapeutic composition or medicament containing a mixture of herbal extracts as described hereinabove, it is necessary to administer said composition or said medicament in a therapeutically-effective amount, that is, in an amount that will provide a concentration of the herbal extracts at the treatment site that is capable of exerting the desired therapeutic effect. It has been found, in general terms, that the compositions and medicaments of the present invention need to be administered in amounts such that, typically, each topical dose contains between 0.1 mg and 10 mg (dry weight) of each herbal extract, the precise values depending on the particular combination of extracts used, and on the mode of topical delivery. Thus, in the case of the therapeutic composition of the present invention that is used in the treatment of mucosal lesions, the weights of the original plant material used to prepare a controlled-release delivery device (as described in Example 2, hereinbelow) are:
[0000] Centella asiatica 1.6 mg
Echinacea purpurea 1.6 mg
Sambucus nigra 7.56 mg
[0068] In the case of compositions and medicaments intended primarily for topical use (such as those of the present invention), it is necessary to administer said compositions and medicaments for periods of time that are sufficient to allow optimal contact of the therapeutically effective amounts of the herbal extracts with the lesions to be treated. When the compositions and medicaments are to be given by incorporation into a controlled-release intra-oral device (as described in Example 2 hereinbelow), said device needs to remain in contact with the lesion to be treated for a period of between 1 and 5 hours. This treatment may be repeated up to 5 times each day, as required, and as determined by a competent clinician.
[0069] Mouthwashes containing the compositions and medicaments of the present invention should be taken in quantities of between 5 ml and 15 ml and allowed to remain in contact with the lesions to be treated for periods of between 30 seconds and one minute. This treatment regime may be repeated up to 5 times per day.
[0070] Lozenges, pastilles, candies and other solid, soluble formulations are to be placed in the mouth, if possible in close proximity to the lesions to be treated, and allowed to dissolve at the natural rate determined by the additives present in said formulations.
[0071] The compositions and medicaments of the present invention as disclosed hereinabove and exemplified hereinabove may be prepared and delivered in a number of different forms.
[0072] In a preferred embodiment of the invention, medicaments and compositions are intended for topical application at the site of the mucosal lesion. Dosage forms suitable for topical application to mucosal surfaces include ointments, pastes, lotions, creams, mouthwashes, lozenges, candies, chewing gums, solutions, gels and sprays. Thus, in addition to the active ingredients, the compositions of the present invention may also contain excipients such as zinc, zinc oxide, silicones, calcium silicate, aluminum hydroxide, polyethylene glycols, fats of animal or vegetable origin, oils, waxes gums, starch and cellulose or cellulose derivatives.
[0073] In other embodiments of the invention, compositions for vaginal administration or for anal administration may be prepared by mixing the active plant-derived components with suitable non-toxic, non-irritating carriers such as suppository wax, polyethylene glycol or cocoa butter.
[0074] In a preferred embodiment of the invention, the compositions and medicaments are administered by means of a localized delivery system that allows topical release of the active constituents of said compositions and medicaments. Any suitable local delivery device may be used to administer the compositions and medicaments to the mucosal surface. However, in a particularly preferred embodiment of the invention the local delivery device is a slow release device such as illustrated hereinbelow in Example 2.
[0075] The following examples are provided for illustrative purposes and in order to more particularly explain and describe the present invention. The present invention, however, is not limited to the particular embodiments disclosed in the examples.
Example 1
Effect of the Anti-Viral Composition on the Formation of Viral Plaques In Vitro
Method:
[0076] The antiviral composition was prepared as follows: 2 ml of a 1:1 hydroalcoholic extract of Echinacea purpurea was mixed with 7.5 ml of a 1:5 hydroalcoholic extract of Sambucus nigra, 8 ml of a 1:4 hydroalcoholic extract of Commiphora molmol , 10 ml of a 1:4 preparation of a hydroalcoholic extract of Uncaria tomentosa and 20 ml of a 1:10 hydroalcoholic extract of Hypericum perforatum . The term “a 1:x hydroalcoholic extract” as used herein indicates that 1 gram of plant material was extracted with x volumes of the alcoholic extraction medium. In the case of all of the plant extracts used in the present example, the extraction medium was a “hydroalcohol”. For the present purposes, the term “hydroalcohol” is defined as an aqueous solution of a lower alcohol. Preferably, the lower alcohol used was ethanol, which was generally prepared as a 50% solution. In some preparations, ethanol was prepared at a different aqueous dilution within the range of 25-90% (v/v), with respect to the ethanol. The weight ratio of E. purpurea:S. nigra:C. molmol:U. tomentosa:H. perforatum in this mixture is 4:3:4:5:4. The above-mentioned alcoholic extracts were purchased either from Herbal Apothecary, Syston, Leicester, U.K. or from Analit Extracts Ltd, M.P. Hefer 38100, Israel.
[0077] Disks of 3 MM filter paper (Whatman Inc.) (5 mm diameter) were soaked in a solution of the compositions to be tested, and placed on a semi-solid agar-containing culture medium covering a monolayer of BSC-1 (green monkey kidney) cells infected with a partially confluent dose of either Herpes simplex type 1 virus (HSV-1) or Herpes simplex type 2 virus (HSV-2). Following 3-4 days incubation at 37° C., the cells were fixed with formaldehyde (20% aqueous solution) and stained with crystal violet (0.1% solution in 0.1M citric acid). The presence of a white color in the central area of the culture indicated toxic damage of the cultured cells due to the anti-viral compositions. Inhibition of viral plaque formation indicated that the composition tested possesses anti-viral activity.
[0078] Acyclovir (ACG), a known and commonly used drug against herpes viruses, was included in the assay as a positive control.
Results:
[0079] The results of a typical plaque assay are given below.
[0000]
anti-
anti-
Extract
Toxicity
HSV1
HSV2
Virosyn
0-10
2-11
3-11
Hypericum
5
4-7
3-12
Uncaria
0
0-8
7-8
Note 1:
Virosyn is the herbal composition described hereinabove comprising extracts of the following five plant species: Echinacea purpurea , Hypericum perforatum , Commiphora molmol , Uncaria tomentosa and Sambucus nigra .
Note 2:
The numerical results in the above table are the diameters of the plaques (in mm) after treatment of the cell cultures with the disks soaked with extracts. Each virus inhibition or cell toxicity experiment was performed in triplicate.
Note 3:
The toxicity of each extract was assessed by measuring the diameter of the blue-stained plaque in the center of cell cultures that did not receive virus.
[0080] The above results indicate that the herbal extract mixture tested possess antiviral activity for both HSV1 and with minimal toxicity to the cultured mammalian cells.
Example 2
Topical Slow-Release Device for Delivery of the Compositions to the Oral Mucosa
[0081] This example demonstrates the preparation of a slow-release device and the incorporation therein of a plant extract mixture containing Centella, Echinacea and Sambucus.
[0082] The slow release device consists of a mixture of carbomer (carbopol), hydroxypropyl cellulose and magnesium stearate blended as described hereinbelow. Magnesium stearate is used as a protective coating to reduce the solubility and adhesiveness of the device.
[0083] The device is prepared as follows:
[0084] 1. The plant extract mixture is prepared by mixing 6 ml of a 1:4 hydroalcoholic extract of Centella asiatica with 1.5 ml of a 1:1 hydroalcoholic extract of Echinacea purpurea and 35 ml of a 1:5 hydroalcoholic extract of Sambucus nigra . The weight ratio of C. asiatica:E. purpurea:S. nigra in this mixture is 15:15:70. The hydroalcoholic extracts of Centella asiatica and Echinacea purpurea were purchased from Herbal Apothecary, Syston, Leicester, U.K., while the hydroalcoholic extract of Sambucus nigra was purchased from Analit Extracts Ltd., M.P. Hefer 38100, Israel. It is be noted that the abovementioned extract values of the form 1:x indicate that 1 g of the plant material was dissolved in x liters of solvent. The term “hydroalcoholic extract” indicates that the plant material was extracted using ethanol at concentrations of between 25% and 50% in water.
[0085] 2. The plant extract mixture is mixed with 2 g sucrose and evaporated to dryness at 40° C. The residue is dissolved in 2 ml water, a further small volume of water added, and the solution lyophilized overnight.
[0086] 3. A mixture of the carbomer compound Carbopol® 934 P (B.F. Goodrich, Cleveland, Ohio, USA) (2 g) and hydroxypropyl cellulose (Klucel Type HF, Hercules BV, Rijswijk, Holland) (1 g) is prepared by crushing the two components together.
[0087] 4. A 1 g aliquot of the carbomer-hydroxypropyl cellulose mix (prepared in step 3.) is mixed together with 100 mg of the lyophilized plant extract powder (prepared in step 2).
[0088] 5. Magnesium stearate (pharmaceutical grade, obtained from Riedel-De Haen, Germany) (1 g) is mechanically mixed with 2 g of the carbomer-hydroxypropyl cellulose mix.
[0089] 6. 14 mg of the magnesium stearate-polymer mix (step 5.) is placed on the bottom of the plunger (13 mm diameter die manufactured by Perkin-Elmer, U.K.) of a mechanical press (Spex Industries, Mutuchen, N.J., USA) and overlaid with 70 mg of the plant extract-polymer mix (step 4.). Pressure (10 tons force) is applied for 30 seconds.
[0090] In addition to the active herbal ingredients, various flavorings, excipients and colorings may be added in order to modify the taste, consistency and color of the preparation.
[0091] The side of the device containing the herbal ingredients (i.e. the side not containing the magnesium stearate) is applied directly to the mucosal surface containing the lesion to be treated. Alternatively, the mucosal surface may be pre-moistened with water or saline before application of the device. Following application, the device is held in place with gentle pressure for approximately 10 seconds. After releasing the gentle pressure, the device adheres to the mucosal tissue for a period of up to five hours.
[0092] Depending on the mucosal lesion to be treated, the device containing the herbal mixture described hereinabove may be used several times per day (e.g. 3 times per day) for periods of between two days and one month.
Example 3
Use of an Herbal Composition of the Invention to Reduce the Pain Associated with Oral Mucosal Lesions
[0093] A convenient, non-random sample of 57 dental patients presenting in a private dental clinic with painful oral ulcers of either traumatic or aphthous origin were treated by applying to the affected site a slow-release device containing a herbal composition of the invention (as described in Example 2 hereinabove). The device was left in place for a 24 hour period. The ulcer-associated pain experienced by the patients was recorded and expressed on a visual analog scale (S. Chrubasik et al. (2000) Am. J. Med. 109: 9-14), as depicted in FIG. 1 . The clinical correlates of the pain index values used in this scale are as follows: 0=no pain; 50=requires analgesic; 100=requires anesthetic. The highest recorded pain index reported by an individual patient in this study was 90.
[0094] It may be seen from these results that the patients experienced an almost immediate decrease in pain (with a mean decrease of greater than 50%). This decrease in pain levels continued over the following 6 hours, achieving a mean pain decrease of greater than 70%. The painful symptoms did not recur following cessation of treatment.
Example 4
Effect of an Herbal Composition of the Invention on the Size of Mucosal Lesions
[0095] Operating as in the study presented in Example 3, the effect of the herbal composition used therein on the healing of the oral ulceration experienced by the patients was determined by quantification of lesion size using a Scion image analysis system. Briefly, lesions were photographed and digitized using a digital camera and associated Smartcard. The image files obtained thereby were processed using the Photoshop software package (Adobe Systems Inc.) running in Microsoft Windows ME on an IBM-compatible personal computer. The periphery of each lesion was outlined and copied into a new window of the NIH Image software package (National Institutes of Health, Bethesda, Md.), where, following thresholding, the lesion area was automatically calculated.
[0096] Results from a sequential study of 45 patients with oral ulceration demonstrate that the treatment with the herbal composition caused a mean 60% decrease in lesional size over a 24-36 hour period.
Example 5
Anticollagenase Activity of an Herbal Composition of the Invention
Anticollagenase Testing:
Procedure:
[0097] Protease activity was assessed on gelatin zymograms. Twelve percent polyacrylamide gels (0.75 mm thickness) were cast containing 10% gelatin as a substrate for the collagenase enzymes, which were applied to the gels under non-reducing conditions without heating. The gels were run, soaked in 200 ml of 2% Triton X-100 in distilled water on a gyratory shaker (0.5 hours, 20° C.), and incubated in developing buffer (50 mM Tris [pH 8.0], 1 mM CaCl 2 ), unless otherwise indicated, for 15 hours at 37° C. The gels were examined following staining with Coumassie blue. Protease activity shows up as clear bands (indicative of cleavage of the gelatin substrate) on a blue background. For inhibition studies, either specific protease inhibitors (DFP (1 Mm), EDTA (5 Mm), BBI (10 mg/ml), phenylmethyl sulfonyl fluoride (PMFS) (50 Mm) or tetracyclines (0.1 and 0.25 Mm)) or a composition comprising a mixture of Echinacea purpurea, Sambucus nigra and Centella asiatica (prepared as described in Example 2, hereinabove) were added to the developing buffer after the run but before the gel was incubated in said developing buffer. In the latter case, the herbal composition was added to the buffer at a concentration of one volume composition to 50 volumes buffer. To determine protease activity as a function of pH, samples were run on zymograms and subsequently incubated in the appropriate buffer (50 Mm citrate-phosphate buffer [pH 5], 50 Mm ADA buffer [pH 6 and 7], 50 Mm TRIS [pH 8 and 9] or 50 Mm CAPS [pH 10]), containing 1 Mm CaCl 2 .
Results:
[0098] Preliminary findings have demonstrated strong inhibitory effects of low concentrations of the herbal extracts on a cocktail of proteases (containing high concentrations of matrix metalloproteinases 2, 3, 8 and 9). These results demonstrate a direct inhibitory effect of low doses of herbal extracts on common metalloproteinases.
[0099] Representative results are shown in the gelatin zymogram depicted in FIG. 2 , in which active proteases are indicated as white bands on a dark background. Line 1: 50 ng active metalloproteases are clearly detectable. Line 2 demonstrates definitive inhibition of the same metalloprotease cocktail present in line 1 by a 1/50 dilution of the aforementioned herbal composition.
Example 6
In Vivo Treatment of Gingival Inflammation Using an Herbal Composition of the Invention
Effects on MMP Activity
[0100] This study forms part of a controlled double-blind matched-sample (sixteen patients), three part clinical trial of the use of a herbal composition of the invention in controlling gingival inflammation 1, 4 and 7 days after placement of a transmucosal adhesive patch containing a composition containing Echinacea purpurea, Sambucus nigra and Centella asiatica (prepared as described in Example 2, hereinabove).
[0101] In the control subjects, a placebo treatment comprising a transmucosal adhesive patch containing food color was used.
[0102] Gingival Tissue removed during periodontal surgery was immediately placed on ice and subsequently frozen and stored at −80 degrees C., prior to performing matrix metalloproteinase (MMP) activity analysis thereon, as described hereinabove in Example 5. The gingival samples are prepared for this analysis by homogenizing the thawed tissue in PBS and centrifuging [100000 g×10 min].
[0103] The preliminary results obtained (data not shown) demonstrate that bands were found in the areas consistent with MMP 2,9 which have been identified as proteases associated with periodontal disease. Tissue samples taken from the experimental sites showed no protease activity, indicating complete inhibition by the herbal composition of the invention.
Example 7
In Vivo Effect of an Herbal Composition of the Invention on Localized Irritation Following an Insect Bite
[0104] A subject having a painful insect bite on the skin overlying the upper arm was treated for a period of 24 hours with an adhesive patch comprising a composition containing Echinacea purpurea, Sambucus nigra and Centella asiatica (prepared as described in Example 2, hereinabove). The insect bite-associated pain experienced by the patient was recorded and expressed on a visual analog scale, as depicted in FIG. 3 . The clinical correlates of the pain index values used in this scale are as follows: 0=asymptomatic; 50=requires medication; 100=extreme localized discomfort. The highest recorded pain index reported in this study was 38.
[0105] It may be seen from these results that almost instantaneous relief of the localized irritation was obtained.
Formulations
[0106] The following formulations comprising herbal compositions of the invention are given for purposes of illustration and exemplification only, and are not intended to limit the scope of the invention in any way. Thus, both the concentration of active ingredient within each formulation may be changed without removing said formulation from the scope of the invention. Similarly, other formulations comprising the herbal compositions claimed herein that contain different carriers, diluents, excipients, colorings, flavorings and other additives are still to be considered to be within the scope of the present invention.
[0107] The term “Active ingredient” used in the following formulation tables refers to any combination of herbal extracts that are within the scope of the invention. The weight percentage of the active ingredient is calculated in terms of the dry weight of the herbal composition. Representative examples of such combinations are:
[0108] A) composition comprising Echinacea purpurea, Hypericum perforatum, Commiphora molmol , Uncaria tomentosa and Sambucus nigra in a weight ratio of 4:4:4:5:3.
[0109] B) composition comprising Echinacea purpurea, Sambucus nigra and Centella asiatica in a weight ratio of 15:70:15.
Formulation 1
[0110]
[0000]
Mouthwash
Ingredient
% by weight
Active ingredient
0.15
Glycerin, U.S.P
10.000
Ethanol, 190-proof, U.S.P
7.500
Flavor
0.040
Polyoxythylene (20) sorbitan
0.200
monoisostearate
Sodium saccharin, N.P.
0.050
Boric acid, U.S.P
0.075
FD&C Green (1% solution)
0.045
Distilled water
balance
Formulation 2
[0111]
[0000]
Lozenge
Ingredient
% by weight
Active ingredient
0.25
Sorbitol
17.5
Mannitol
17.5
Starch
13.6
Sugar substitute
1.2
Flavor
11.7
Color
0.1
Corn syrup
Balance
Formulation 3
[0112]
[0000]
Chewing Gum
Ingredient
% by weight
Active ingredient
0.25
Gum base (30 parts Eastergum,
30.00
45 parts Coumarone resin,
15 parts dry latex, 10 parts
Paraffin wax)
Sugar
50.00
Corn syrup
18.00
Citric acid
1.00
Flavor
balance
Formulation 4
[0113]
[0000]
Toothpaste
Ingredient
% by weight
Active ingredient
0.5
Sorbitol
33.00
Saccharin
0.46
Silica
22.00
NaF
0.243
Glycerin
9.00
NaOH (50%)
0.20
Carbopol
0.20
Keltrol
0.60
TiO 2
0.50
Sodium alkyl sulphate (28%
4.00
solution)
PEG 6
3.00
FD&C Blue# 1 (1% solution)
0.05
Flavor
1.1
Water
Balance
[0114] While specific embodiments of the invention have been described for the purpose of illustration, it will be understood that the invention may be carried out in practice by skilled persons with many modifications, variations and adaptations, without departing from its spirit or exceeding the scope of the claims.
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The present invention provides therapeutic compositions comprising extracts of the plant species Echinacea purpurea and Sambucus nigra and the extract(s) of at least one further plant selected from the group consisting of Hypericum perforatum, Commiphora molmol and Centella asiatica . The compositions of the invention are of particular utility in the management of inflammatory mucosal diseases of both viral and non-viral origin.
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BACKGROUND
[0001] Embodiments of the present invention relate to a can closure, particularly for a milk can, a can lid and a can having a can closure and/or can lid.
[0002] Typical condensed milk cans are typically opened by piercing a pouring opening in the can lid near the edge and a ventilation opening on the diametrically opposing side.
[0003] Known condensed milk cans of this type have the problem of the can fold seam projecting next to the pouring opening at the can edge, which obstructs clean pouring of the condensed milk and thus makes the desired metering of the condensed milk more difficult. In addition, condensed milk residues may collect on the can edge, which is unhygienic and impairs the visual impression of the condensed milk can. Finally, in the known condensed milk cans, the pouring opening or the ventilation opening may clog, which requires renewed opening.
[0004] Furthermore, beverage cans are known for beer or caffeinated soft drinks, for example, which have a ring-pull closure or a press-in closure. For this purpose, a typically triangular wall part is provided in the can lid, which is delimited from the remaining can lid by a weakening line and may be torn open using a tab or pressed into the beverage can in order to expose a pouring opening in the can lid. Press-in or ring-pull closures of this type are not used in condensed milk cans, however, since the resulting pouring openings would typically be too large. In addition, the can fold projecting at the can edge would also lead to the problems described at the beginning with a press-in closure or ring-pull closure of this type.
[0005] A pourer for Europacks, which has a closure bottom having a pouring opening and a foldable closure top, is known from DE 100 17 467 A1.
SUMMARY
[0006] An embodiment of the present invention is therefore based on the object of providing a can closure which allows clean pouring from a condensed milk can and prevents contamination by adhering condensed milk residues.
[0007] The object is achieved, for example, by a can closure according to Claim 1 , a can lid according to Claim 13 , and a corresponding can according to Claim 16 , respectively.
[0008] The present invention comprises the general technical teaching of providing a can closure which at least partially comprises plastic and has a pouring opening that may be opened manually by user without tools, the pouring opening preferably being spaced apart from the can lid.
[0009] The positioning of the pouring opening spaced apart from the can lid offers the advantage that clean pouring is possible and contamination of the can lid by residues of the liquid poured out is prevented.
[0010] In contrast, manufacturing the can closure according to the present invention from plastic offers the advantage that the closure may be inserted into a cutout in the can lid and seals the cutout at the same time.
[0011] If the can closure is manufactured from plastic, the can bottom preferably comprises two components which have different hardnesses. The softer component of the can bottom is used in this case as a gasket and presses against the edge of the cutout in the mounted state in the can lid.
[0012] For this purpose, the gasket preferably not only presses against the edge of the cutout positioned in the can lead, but rather encloses the edge of the cutout, through which the edge of the cutout is protected from corrosion. It is to be noted in this context that the can sheet metal is typically coated with a protective lacquer layer before processing. When the cutout is stamped into the can lid, this protective lacquer layer is damaged at the edge of the cutout, however, which may lead to corrosion there. In this variation of the present invention, corrosion at the edge of the cutout in the can lid is thus advantageously prevented because the cut edge is enclosed by the gasket of the can closure according to the present invention.
[0013] Polyethylene (PE) and polypropylene (TP) are especially advantageously suitable as a material for the can closure according to the present invention, however, the present invention is not restricted to these plastics in regard to the material for the can closure, but rather may also be implemented using other plastics.
[0014] In a preferred exemplary embodiment of the present invention, the can closure has a closure bottom and a closure lid, the closure bottom being insertable into a cutout in the can lid and able to be connected to the can lid in a form-fitting way, while the closure lid is connected by a joint to the closure bottom and is pivotable from a transport position into a usage position. For this purpose, a pouring opening is positioned in the closure bottom and the closure lid has means to open the pouring opening in the usage position of the closure lid. For this purpose, i.e., for opening the can closure, the closure lid is preferably folded onto the closure bottom, the pouring opening positioned in the closure bottom automatically being opened.
[0015] The pouring opening in the closure bottom is preferably closed before the initial opening by a cover which has at least one intended breaking point. The closure lid then breaks this intended breaking point upon the initial pivoting from the transport position into the usage position, through which the pouring opening in the closure bottom is exposed.
[0016] The breaking of the intended breaking point in the closure bottom is preferably performed using a piercing rib, which is positioned on the bottom of the closure lid and presses against the cover of the pouring opening positioned in the closure bottom when the closure lid is pivoted out of the transport position into the usage position.
[0017] This piercing rib preferably has a bevel on the side facing toward the joint, the height of the piercing rib falling along the bevel toward the joint.
[0018] The cover of the pouring opening positioned in the closure bottom is prevented from tearing off completely and possibly falling into the can in the usage position of the closure lid.
[0019] In addition, the cover of the pouring opening positioned in the closure bottom is held in a pivoted position, in which the pouring opening in the closure bottom always remains open, by the bevel of the piercing rib.
[0020] In addition, the piercing rib attached in the closure lid is preferably used as a handle to pivot the closure lid from the transport position into the usage position.
[0021] The closure bottom may have a peripheral, preferably grooved depression for attachment to the can lid, in which the mouth edge of a cutout positioned in the can lid engages in a form-fitting way.
[0022] However, it is more favorable for manufacturing to connect the closure bottom to the can lid using a plastic injection procedure.
[0023] In addition, there is also the possibility that the closure bottom is bonded to the can lid by an ultrasonic weld.
[0024] The can closure according to the present invention preferably has a surface contour on its bottom or on the lower side of the closure bottom, in order to produce a form-fitting, intimate connection to a corresponding surface contour on the can lid during a plastic injection procedure. A surface contour of this type may comprise small protrusions, depressions, or holes, for example, which are positioned in the can lid at the edge of the cutout for the closure bottom.
[0025] Furthermore, after the closure lid in the can closure according to the present invention is pivoted from the transport position into the usage position, it preferably automatically remains in the usage position. This may be achieved, for example, if the closure lid forms a press fit with the closure bottom. However, it is also alternatively possible that the closure bottom and the closure lid have catch elements in order to form a catch connection between the closure bottom and the closure lid in the usage position of the closure lid, so that the closure lid remains in the usage position automatically.
[0026] In addition, the can closure according to the present invention is preferably recloseable after the initial opening. For this purpose, a closure flap may be provided, which is positioned on the closure lid and may be pivoted in relation to the closure lid by a joint, such as a film hinge, for example.
[0027] However, the present invention comprises not only the can closure according to the present invention described above, but rather also an appropriately adapted can lid, which has a cutout for receiving the closure bottom and a depression for receiving the closure lid in its transport position.
[0028] The depression for the closure lid is preferably sufficiently large for this purpose that the closure lid does not project upward above the can edge in the mounted state in the transport position. A design of this type of the can closure and the associated can lid is advantageous since the filled cans may thus be stacked one on top of another without the can closure increasing the stack height or impairing the ability to be stacked.
[0029] Preferably, in the can lid according to the present invention, a surface contour is provided at the edge of the cutout for the closure bottom, in order to produce a form-fitting, intimate connection with a corresponding surface contour on the closure bottom during a plastic injection procedure. A surface contour of this type may comprise, for example, protrusions, depressions, or holes which are positioned at the edge of the cutout for the closure bottom.
[0030] Finally, the present invention also comprises a can having a can lid of this type and/or a can closure according to the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0031] Other advantageous refinements of the present invention are characterized in the dependant claims or will be explained in greater detail in the following together with the description of the preferred exemplary embodiment of the present invention on the basis of the figures.
[0032] FIG. 1 shows a can closure according to the present invention in the opened state in a top view,
[0033] FIG. 2 shows a cross-sectional view of a can having the can closure according to the present invention from FIG. 1 in a transport position,
[0034] FIG. 3 shows the region A from FIG. 2 in an enlarged cross-sectional view,
[0035] FIG. 4 shows a cross-sectional view of the can from FIG. 2 in a usage position with the can closure opened,
[0036] FIG. 5 shows an enlarged cross-sectional view of the can closure from FIG. 4 ,
[0037] FIG. 6 shows a milk can having a can closure according to the present invention in a transport position,
[0038] FIG. 7 shows the milk can from FIG. 6 in a usage position,
[0039] FIG. 8 shows a bottom view of the can closure of the milk can from FIGS. 6 and 7 in the opened state,
[0040] FIG. 9 shows a perspective top view of the can closure from FIG. 8 ,
[0041] FIG. 10 shows a can lid having a can closure according to the present invention in the transport position,
[0042] FIG. 11 shows a bottom view of the can lid from FIG. 10 ,
[0043] FIG. 12 shows a perspective top view of the can lid from FIGS. 10 and 11 with the can closure removed,
[0044] FIG. 13 shows a perspective bottom view of the can lid from FIG. 12 ,
[0045] FIG. 14 shows a perspective view of an alternative exemplary embodiment of the can closure according to the present invention, and
[0046] FIG. 15 shows a cross-sectional view of the can closure from FIG. 14 in the mounted state on a can.
DESCRIPTION
[0047] FIGS. 1 through 5 show a can closure 1 manufactured from plastic, which essentially comprises a closure bottom 2 and a closure lid 3 .
[0048] The closure bottom 2 is connected via a joint 4 to the closure lid 3 , the joint 4 comprising a film hinge.
[0049] During assembly, the closure bottom 2 —as will be explained later—is attached in a cutout 5 , which is tailored to its shape, within a can lid 6 of a can 7 .
[0050] The closure bottom 2 has a pouring opening 8 , which is provided with a cover 9 in the form of a piercing area in the transport state of the can 7 (see FIG. 2 ). This cover 9 is connected in its regions adjoining the pouring opening 8 to the closure 2 via thin-walled intended break points 10 , while a region of the cover 9 diametrically opposite the pouring opening 8 is designed as a film hinge 11 and acts as a joint after the piercing.
[0051] The closure lid 3 is also provided with a pouring opening 12 , which is closeable again in the usage state of the can 7 using a linked closure flap 13 . In the central region of the pouring opening 12 in the closure lid 3 , a piercing rib 14 is positioned, which overlaps the pouring opening 12 perpendicularly and whose function will be discussed later.
[0052] FIG. 2 shows the can closure 1 integrated into the can lid 6 of the can 7 , the cover 9 still being connected to the closure bottom 2 . As may also be seen from this figure, the cutout 5 is located in the can lid 6 , into which the closure bottom 2 is introduced using an injection procedure and is therefore supported in a form-fitting way in the can lid 6 . The possibility arises of providing small protrusions and/or depressions or small holes on the inner contours of the cutout 5 for this purpose, in order to produce an intimate bond between the closure bottom 2 and the can lid 6 .
[0053] The can lid 6 also has a depression 15 tailored to the contours of the closure lid 3 , into which the closure lid 3 is introduced in the transport state of the can 7 . It is thus possible to stack multiple cans 7 one on top of another for transport purposes, without the closure 1 having an interfering effect on the stack height. The depression 15 is therefore deep enough that the closure lid 3 does not project above the edge of the can 7 in the transport position.
[0054] In the usage position of the can 7 shown in FIGS. 4 and 5 , the closure lid 3 is removed from the depression 15 of the can lid 6 by pulling on the piercing rib 14 and pivoted in the direction toward the closure bottom 2 . During this procedure, the cover 9 is pressed far enough in the direction of the can interior because of its intended break points 10 , using the piercing rib 14 , which has a bevel 16 (see FIG. 3 ) in the region of the joint 4 , until the cover 9 comes to rest on the bevel 16 of the closure lid 3 . The cover 9 pivots at the same time around the region 8 between the closure bottom 2 and the cover 9 . In this state, the closure lid 3 engages with the closure bottom 2 .
[0055] Furthermore, a peripheral catch edge 17 positioned on the closure bottom 2 may be seen from FIG. 5 , which cooperates with a catch receiver 18 , which is also peripheral, positioned on the closure lid 3 .
[0056] The pouring opening 12 in the closure lid 3 is covered using a closure flap 13 which allows reclosure. In the usage position of the can 7 shown in FIGS. 4 and 5 , the liquid provided in the can 7 may be removed via the pouring opening 8 and the pouring opening 12 , the metering of the liquid able to be influenced by the piercing rib 9 . After the emptying procedure has ended, the pouring opening 12 of the closure lid 3 is covered using the closure flap 13 . This closure flap 13 may also be pivotably connected to the closure lid 3 via a film hinge 19 and engages with closure lid 3 when it is pressed on.
[0057] For more comfortable handling, the closure lid 3 also has a handle-like projection 20 , using which the closure lid 3 may be removed from the closure bottom 2 again.
[0058] The exemplary embodiment of a can closure 1 ′ according to the present invention illustrated in FIGS. 6 to 13 largely corresponds with the exemplary embodiment described above and illustrated in FIGS. 1 through 5 , so that in the following reference is largely made to the above description to avoid repetition and the same reference numbers are used for corresponding components, which are identified only by an apostrophe for differentiation.
[0059] A special feature of this exemplary embodiment is that a slotted depression 21 ′ is positioned in the closure bottom 2 ′, which is covered on its lower side by a cover 22 ′ before the initial opening, the cover 22 ′ being connected by intended break points to the closure bottom 2 ′. When the closure lid 3 ′ is pivoted from the transport position illustrated in FIGS. 6 , 8 , 9 , and 10 into the usage position illustrated in FIG. 7 , the piercing rib 14 ′ is inserted into the slotted depression and breaks the intended break points between the cover 22 ′ on the lower side of the slotted depression 21 ′ and the closure bottom 2 ′, through which a pouring opening is exposed.
[0060] In addition, it may be seen from FIG. 8 that small protrusions 23 ′ are molded onto the lower side of the closure bottom 2 ′, which, in the mounted state, engage in corresponding depressions 24 ′, which are attached in the closure lid 3 ′ in the edge of the cutout 5 ′ for the closure bottom 2 ′, as may be seen from FIGS. 13 and 14 in particular. The protrusions 23 ′ on the closure bottom 2 ′ result in a form-fitting connection in combination with the holes 24 ′ in the closure lid 3 ′.
[0061] The exemplary embodiment of a can closure 1 ″ according to the present invention illustrated in FIGS. 14 and 15 largely corresponds to the exemplary embodiments described above, so that reference is made to the above description to avoid repetition and the same reference numbers are used in the following for corresponding components, which are only identified by two apostrophes for differentiation.
[0062] A special feature of this exemplary embodiment is that the closure bottom 2 ″ comprises two plastic opponents which have different hardnesses. The harder plastic component forms a gasket 25 ″ for this purpose, which rests on the edge of the cutout in the can lid in the mounted state and thus seals the cutout.
[0063] In addition, the gasket 25 ″ also prevents corrosion at the edge of the cutout of the closure lid because the gasket 25 ″ encloses the cutout edge. This is advantageous because stamping out the cutout damages the protective lacquer layer on the can sheet metal and therefore makes it susceptible to corrosion.
[0064] The present invention is not restricted to the preferred exemplary embodiments described above. Rather, multiple variations and alterations are possible, which also make use of the ideas according to the present invention and therefore fall within the scope of protection.
LIST OF REFERENCE NUMBERS
[0000]
1 , 1 ′, 1 ″ can closure
2 , 2 ′, 2 ″ closure bottom
3 , 3 ′, 3 ″ joint
5 , 5 ′ cutout
6 , 6 ′ can lid
7 , 7 ′, 7 ″ can
8 , 8 ′, 8 ″ pouring opening
9 , 9 ′, 9 ″ cover
10 , 10 ′ intended break points
11 film hinge
12 , 12 ′ pouring opening
13 , 13 ′, 13 ″ closure flap
14 , 14 ′, 14 ″ piercing rib
15 , 15 ′ depression
16 , 16 ′ bevel of the piercing rib
17 , 17 ′ catch edge
18 , 18 ′ catch receiver
19 , 19 ′ film hinge
20 , 20 ′ projection
21 ′ depression
22 ′ cover
23 ′ protrusions
24 ′ depressions
25 ″ gasket
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The invention relates to a container seal, in particular for a milk container ( 7 ′), whereby said container seal may be mounted in a container lid ( 6 ′) and manually operated without tools. According to the invention, the container seal is at least partly made from plastic and may be inserted in a cut-out in the container lid ( 6 ′), whereby the container seal seals the cut-out in the container lid ( 6 ′) and comprises a pouring opening. The invention further relates to a corresponding container lid ( 6 ) and a container with said container seal.
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FIELD OF THE INVENTION
The present invention relates to building blocks for constructing model structures wherein the individual building blocks interconnected by means of connecting elements which connect the blocks to one another yet permit limited lateral movement of the blocks with respect to each other so that a straight wall constructed of such blocks can be manipulated into a wall having curves.
BACKGROUND OF THE INVENTION
Typical building blocks for constructing model structures have a solid rectangular shape with flat, planar, mutually orthogonal outer surfaces. Some blocks are provided with interlocking or connecting structure for interconnecting a plurality of the blocks into a desired structural shape. Typical interconnecting structures positively lock the blocks to one another and permit no lateral movement, or play, of the blocks with respect to each other. Moreover, the blocks and associated interconnecting structures are configured such that flat top, bottom, and end surfaces of the blocks are in contact with top, bottom, and end flat surfaces of adjacent blocks. Accordingly, the structures which can be constructed with such blocks are limited to those having straight, vertical walls and 90 degree corners.
Further, because the interconnecting structures permit no lateral play between mutually interconnected blocks, a plurality of blocks, once assembled into a straight, vertical wall, cannot thereafter be manipulated into other curved and/or sloped walls. Curved and/or sloped walls can only be built using specially shaped blocks. Accordingly, the variety of model structures which can be constructed by such typical building blocks is necessarily limited.
Past proposals for providing curved wall capability have included trapezoidal or wedge-shaped blocks or combinations of straight and trapezoidal or wedge-shaped blocks.
On the other hand, rectangular building blocks having no interconnecting elements, i.e., those blocks wherein each block merely rests on the blocks below it and all blocks are held together by only gravity and friction, are capable of being arranged in curved patterns and non-orthogonal corners. Because such blocks lack interconnecting elements, however, structures built from such blocks are usually unstable and easily knocked down.
Accordingly, a need exists for building blocks that are interconnectable with each other yet may be manipulated after they are interconnected.
SUMMARY OF THE INVENTION
The present invention seeks to overcome the limitations presented by conventional building blocks. This object is achieved by providing a set of building blocks useful for constructing model structures, each of a plurality of the set comprising a block body and block interconnecting structure fixed to the block body. The block interconnecting structure is constructed and arranged to detachably connect the block body to a block body of an adjacent building block of the plurality of building blocks by resisting movement of the block body of the building block in a first direction with respect to the block body of the adjacent building block when the block interconnecting structure of the building block is connectively engaged with block interconnecting structure of the adjacent building block. The interconnecting structure is also constructed and arranged to permit limited play of the building block with respect to the adjacent building block in a second direction substantially transverse to the first direction when the interconnecting structure of the building block is connectively engaged with the interconnecting structure of the adjacent building block to enable interconnected building blocks of the plurality of building blocks to be manipulated.
Further, the object of the present invention is achieved by providing a connecting element for installation in a respective aperture in each of a plurality of building blocks useful for constructing model structures. The connecting element is constructed and arranged to enable a building block of the plurality of building blocks to be interconnected with an adjacent building block of the plurality of building blocks such that separation of the building block from the adjacent building block in a first direction is resisted by the connecting element while limited movement of the building block with respect to the adjacent building block in a second direction substantially transverse to the first direction is permitted by the connecting element. The connecting element includes connecting element retaining structure constructed and arranged to frictionally retain the connecting element in the aperture when the connecting element is installed in the aperture. An insert structure is disposed at one end of the connecting element and extends from the aperture when the connecting element is installed in the aperture. Insert receiving structure is disposed at an opposite end of the connecting element and is disposed within the aperture when the connecting element is installed in the aperture. The insert receiving structure of the connecting element of the building block is constructed and arranged to receive and releasably retain the insert structure of the connecting element of the adjacent building block when the insert structure of the adjacent building block is inserted into the insert receiving structure of the building block. Further, the insert structure and the insert receiving structure are constructed and arranged such that when the insert structure of the connecting element of the adjacent building block is inserted into the insert receiving structure of the connecting element of the building block, the insert receiving structure of the connecting element of the building block resists extraction in the first direction of the insert structure of the connecting element of the adjacent building block from the insert receiving structure of the connecting element of the building block. The insert structure and the insert receiving structure are further constructed and arranged to permit limited movement in the second direction of the insert structure of the connecting element of the adjacent building block within the insert receiving structure of the connecting element of the building block.
These and other features of the present invention will become more apparent during the course of the following detailed description and appended claims. The invention may best be understood with the reference to the accompanying drawings wherein an illustrative embodiment is shown.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1A is a perspective view from above of one embodiment of a building block according to the present invention;
FIG. 1B is a perspective view from below of the building block shown in FIG. 1A;
FIG. 2A is a front-view elevation of a preferred embodiment of a male-female building block connecting element according to the present invention;
FIG. 2B is an end-view elevation of the preferred embodiment of a male-female building block connecting element according to the present invention;
FIG. 3A is a front-view elevation of a preferred embodiment of a female only building block connecting element according to the present invention;
FIG. 3B is an end-view elevation of the preferred embodiment of a female only building block connecting element according to the present invention;
FIG. 4A is a front-view elevation of one embodiment of a building block according to the present invention;
FIG. 4B is an end-view elevation of one embodiment of a building block according to the present invention;
FIG. 5 is cross-section taken along the line V--V in FIG. 4A;
FIG. 6 is a cross-section showing a female only building block connecting element taken in a direction corresponding to the direction of the cross-section of FIG. 5;
FIG. 7A is a perspective view from above of a second embodiment of a building block according to the present invention;
FIG. 7B is a perspective view from below of the building block shown in FIG. 7A;
FIG. 8 is an end-view cross section of two building blocks interconnected to each other in accordance with the present invention;
FIG. 9A is a top view of one row of a plurality of building blocks according to the present invention oriented in a straight wall configuration; and
FIG. 9B is a top view of the one row of building blocks of FIG. 9A manipulated in accordance with the present invention into a curved wall configuration.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
A building block according to the present invention is shown in FIGS. 1A, 1B, 4A, and 4B and is indicated generally by reference number 20. The block 20 shown is substantially rectangular, although it is presently contemplated that the present invention may be incorporated into blocks of substantially any shape as will be described below. The body of the block is preferably formed of wood (hard maple being preferred) but may be formed of other materials, such as plastic. Block 20 is provided with two connecting elements, such as, male-female locking inserts 22 inserted into the hole 24 formed in the bottom surface 28 and extending through hole 25 above top surface 26. Although block 20 is shown having two locking inserts 22, it will be appreciated that a building block according to the present invention could be provided with any number of locking inserts, i.e., more or less than two. In addition, although locking inserts 22 are shown projecting from surface 26, which, in the views depicted in FIGS. 1A and 1B, is the top of the block, locking inserts could project from any of the surfaces 30, 32, 34, or 28 in addition or alternatively to the locking inserts projecting from surface 26.
The details of the male-female locking insert 22 are shown in FIGS. 2A and 2B. Each male-female locking insert, preferably, but not exclusively, formed of molded plastic, includes a male end 40 and female end 48. In the preferred embodiment of the present invention, male end 40 comprises a spherical ball and female end 48 comprises a clip having two prongs 50. Each locking insert 22 includes an axially extending central shaft 46 and preferably further includes a circular rim 42 disposed along the central shaft 46 below the spherical ball 40 and centered on and extending radially from the central shaft 46. Rim 42 preferably has a diameter that is greater than that of the spherical ball of male end 40. Rim 42 preferably has a chamfer section 43 formed about the outer periphery of the upper surface of the rim 42 to facilitate installation of the insert into a block as will be described below. Rim 42 further preferably includes an indication mark 45 extending about the outer periphery of the rim 42. The purpose of indication mark 45 will be described below.
Located below the rim 42 is a plurality of radially extending circumferential fins 44. As can be appreciated from FIGS. 2A and 2B, each individual fin has a thickness that preferably varies linearly from a maximum thickness adjacent central shaft 46 to a minimum thickness at the radial extent of the fin. The fins 44 are preferably elastically deflectable and preferably deflect more readily toward the female end 48 of the locking insert than toward the male end 40. Although the locking inserts 22 shown in FIGS. 2A and 2B include five radial fins, a locking insert may have any number of radially extending fins, although a minimum of three fins is preferred.
In the preferred embodiment of the present invention, the plurality of radial fins is preferably divided into an upper group of fins and a lower group of fins separated from one another by gap 47. The purpose of gap 47 will be described below.
Located below the plurality of radially extending fins 44, is shoulder 54 centered on and extending radially from central shaft 46. Shoulder 54 is preferably circular and preferably has a diameter greater than that of the plurality of radially extending fins 44.
Located below shoulder 54 is the female end 48 which preferably comprises a clip structure composed of two diametrically opposed prongs 50. Each prong 50 includes a bevelled section 52 at the inner surface of the lower axial end of the prong 50, a retaining flange 56, and a ball holding area 58. The operation and function of the male-female locking insert 22 will be described below.
The installation of each locking insert into a block is shown in FIG. 5. As shown in FIG. 5, each locking insert 22 is installed into a through hole formed through the block which comprises a first portion 24 and a second portion 25. Portion 24 has a greater diameter than that of portion 25, and a radially extending, annular shoulder 23 is defined at the junction of portion 24 with portion 25. The locking insert 22 is inserted into the through hole in the direction indicated by arrow A shown in FIG. 5. As can be appreciated from FIG. 5, the diameter of portion 24 is preferably slightly larger than the diameter of shoulder 54 of the locking insert 22 so that shoulder 54 readily fits within hole portion 24, and the diameter of the radially extending fins 44 is preferably slightly larger than that of portion 25 of the through hole so that fins 44 deflect slightly and fit snugly within hole portion 25. Locking insert 22 is inserted into the through hole until shoulder 54 engages the annular shoulder 23. Chamfer section 43 eases the insertion of the insert into the hole portion 25. As can be appreciated from FIG. 5, the length of portion 24 of the through hole should be such that when insert 22 is installed in the through hole with shoulder 54 abutting annular shoulder 23, the bottom end of female end 48 is recessed within the hole 24. Also, the length of the locking insert between shoulder 54 and rim 42 (and the length of hole portion 25) should be such that indication mark 45 is disposed at the upper edge of hole portion 25 and a portion of the thickness of rim 42 extends above surface 26. Accordingly, indication mark 45 is preferably provided as a system control measure to ensure that hole portion 24 is drilled to a proper depth.
With shoulder 54 abutting the annular shoulder 23, locking insert 22 can move no further in the direction indicated by arrow A. In addition, because the radially extending fins 44 deflect more easily toward the female end 48 of insert 22 than toward the male end 40 and are slightly deflected toward female end 48 from the insertion of insert 22 into hole portion 25, the radially extending fins 44 resist movement of the locking insert in a direction opposite to that indicated by arrow A. Accordingly, locking insert 22 is substantially fixed into the installed position shown in FIG. 5.
Interconnection of building blocks according to the present invention to one another will be described with reference to FIG. 8. Shown in FIG. 8 are two blocks 20 and 80 interconnected to one another. Because the locking inserts of both blocks are preferably identical to one another in structure, common reference numbers will be employed for common structural features of the inserts of both blocks 20 and 80. As shown in FIG. 8, a first block 20 is interconnected to a second block 80 by inserting the male end 40 of insert 22 protruding above block 20 into the female end 48 of the locking insert 22 of the block 80. Prongs 50 are preferably shaped so as to facilitate insertion of the male end ball 40 into the female end clip 48. Specifically, bevelled sections 52 formed in the lower end of prongs 50 cause the prongs 50 to deflect away from each other as the ball 40 is forced into clip 48. As mentioned above, the inserts 22 are preferably formed from plastic. Therefore, deflection of the prongs 50 is elastic deflection. Once ball 40 is inserted all the way into the ball holding area 58, the prongs 50 return to their normal positions and withdrawal of the ball 40 from the clip 48 is resisted by retaining flanges 56.
With the blocks interlocked as shown in FIG. 8, separation of the blocks in an axial direction with respect to the locking inserts 22 is resisted by the female end clip 48 holding the male end ball 40. In addition, the prongs 50 of the clip 48 resist movement of the ball 40 of block 20 in a lateral direction with respect to block 80 (i.e., left or right as shown in FIG. 8). However, limited movement or play of block 20 with respect to block 80 is available in a direction into and out of the page of FIG. 8. The amount of linear play is limited by the portion of rim 42 extending above the top surface 26 of block 20. This portion of rim 42 extending above block 20 engages with the outer periphery of portion 24 of the through hole of 80 so as to limit movement of blocks 20 and 80 with respect to one another. As can be appreciated from FIG. 8, the diameter of rim 42 is less than that of portion 24 of the through hole. It is preferred that the diameter of rim 42 be approximately 1/8 inch less than the diameter of hole portion 24 so as to permit approximately 1/16 inch of play in either direction.
The manner in which the above-described interblock play permits a plurality of blocks interconnected in accordance with the present invention to be manipulated is shown in FIGS. 9A and 9B. A top view of at least a portion 70 of one row of building blocks 20 is shown. For simplicity, the row of blocks below row 70 with which the blocks of row 70 would be interconnected is not shown. As shown in FIG. 9A, when initially interconnected, row 70 may assume a straight configuration, the end of each block 20 being substantially parallel to the end of the adjacent block and there being little or no space between the ends of adjacent building blocks. Row 70 can be manipulated, however, by merely moving desired portions of row 70 in different transverse directions to create a curved row 70' as shown in FIG. 9B. The interblock play permits the ends of adjacent blocks to become partially separated and to allow some degree of rotation of the blocks so that the ends may assume non-parallel orientations with respect to each other. Accordingly straight walls can be manipulated into curved walls and vice versa.
It is not necessary, however, that a wall first be constructed in a straight-walled orientation and then manipulated into a desired curved orientation. A wall may be constructed in a curved orientation, limited only by the amount of play permitted by the connecting elements.
It can also be appreciated from FIG. 8 that if only one insert from block 20 is engaged with one insert of block 80, blocks 80 and 20 will be rotatable with respect to each other about the aligned longitudinal axes of their respective inserts.
When the locking insert 22 is installed into a block, the insert should be oriented such that the prongs 50 are disposed perpendicularly with respect to the direction in which the linear play is desired. In other words, the open area extending between the prongs 50 must be aligned with the desired direction of linear play. In addition, when more than one locking insert is provided in a block, each of the inserts should be oriented consistently with the desired direction of play.
To disengage blocks from one another, interconnected blocks are merely pulled apart in a direction roughly parallel to the axial direction of the connecting elements, or inserts. Prongs 50 will be caused to bend elastically outwardly by ball 40 so as to release ball 40 from the female end of the insert.
The block and locking insert configurations described thus far comprise a block having a locking insert with both a male end 40 and female end 48. When a wall structure is constructed of blocks according the present invention, the aesthetics of the structure will be enhanced if there are no locking inserts protruding from the top surface of the top row of blocks of the wall. Accordingly, a set of blocks according to the present invention will preferably include a plurality of blocks having a truncated, or female only, connecting element, or locking insert 22' as shown in FIGS. 3A, 3B and 6. Inserts 22' include a female end 48' which preferably comprises a clip having two diametrically opposed prongs 50' as with the male-female locking insert 22. In addition, inserts 22' include a shoulder 54', a central shaft 46' and a plurality of radially extending fins 44'. As opposed to the male-female locking inserts 22 shown in FIGS. 2A and 2B, however, the female locking insert 22' as shown in FIGS. 3A and 3B does not include a rim 42 or a male end ball 40.
Female only inserts 22' are preferably formed by cutting a male-female insert 22 at gap 47 into two portions. The upper, male end, portion may be discarded and the lower, female end, portion becomes a female only insert. Accordingly, both male-female and female only inserts can be produced using a single injection mold. It is, of course, possible to form each type of insert in specifically designed mold, in which case there is no need for gap 47 formed in the male-female insert. As shown in FIG. 6, the female locking insert 22' is installed into a block much as a male-female locking insert 22 is installed. Specifically, the insert 22' is inserted into a blind hole which comprises a first portion 24' and a second portion 25' having a diameter less than that of first portion 24'. Again, the diameter of first portion 24' is preferably such that shoulder 54' readily fits into first portion 24' and the diameter of second portion 25' is preferably such that radial fins 44' fit snugly within second portion 25'. Insert 22' is inserted into the blind hole until shoulder 54' engages the annular shoulder 23' defined at the junction of first portion 24' and second portion 25'.
As mentioned above, interlocking blocks according to the present invention can take on a practically limitless variety of shapes and sizes. One example of an alternate shape is shown in FIGS. 7A and 7B. Block 60 has an arcuate shape and has three locking inserts 22a, 22b, and 22c. Each of the locking inserts 22a-22c is preferably oriented such that the female clip portions thereof are aligned in the arcuate direction defining the block 60.
Other block shapes which can incorporate an interlocking mechanism of the present invention may include arches and a variety of other shapes.
A set of building blocks incorporating the present invention need not include only building blocks having interblock lateral play in accordance with the present invention, but may also include, for example, blocks that are not interconnectable at all with neighboring blocks and blocks that are rigidly interconnectable to neighboring blocks, that is to say, blocks without interblock play capability.
Any number of model structures can be built with a set of building blocks according to the present invention; the user's imagination being the limit.
Such model structures may include anything from simple four-sided houses to elaborate castles, bridges, and towers. To that end, a set of building blocks may include any number of specialty blocks having unique shapes, or add-on sets having specialty blocks for specific types of structures could be sold as accessories to basic building block sets. For example, a castle set may include numerous arches of different spans and radii of curvatures for constructing gates and windows, arcuate blocks for constructing towers, special blocks for constructing spiral staircases in one or more towers, and assorted crowning pieces for constructing wall and tower crowns.
It will be realized that the foregoing preferred specific embodiment of the present invention has been shown and described for the purposes of illustrating the functional and instructional principles of this invention and are subject to change without departure from such principles. Therefore, this invention includes all modifications encompassed within the spirit and scope of the following claims.
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A set of building blocks useful for constructing model structures includes a plurality of building blocks comprising block bodies and block interconnecting structure. The block interconnecting structure releasably locks each block to one or more adjacent blocks by resisting the blocks being pulled apart from each other. The interconnecting structure does provide, however, a limited amount of lateral play between the blocks so that the interconnected blocks may be moved laterally with respect to each other. The interconnecting structure preferably comprises one or more connecting elements installed into respective apertures in the block bodies. Some blocks have connecting elements with both an inserting end that projects above an outer surface of the block body and a receiving end disposed within the aperture. Other blocks have connecting elements having only a receiving end. The inserting end of the connecting element of a block is inserted into the receiving end of an adjacent block to which it is to be interconnected. The receiving end of a connecting element resists extraction of the inserting end inserted therein but permits the inserting end to move laterally a limited amount within the receiving end.
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BACKGROUND OF THE INVENTION
In fuel burners such as furnaces where the main burner is lit by a pilot burner, it is necessary for obvious reasons to assure that the pilot burner is lit before the main burner fuel valve is opened. This is true whether a standing pilot or intermittent pilot is involved. While there are many different types of sensing operations which can reliably detect presence of a pilot flame, one which is preferred senses the flicker frequency of typical pilot flames. This flicker is a periodic variation of the intensity or amplitude of the infrared, visible, or ultraviolet radiation produced by the burning of the fuel sustaining the pilot flame. The flicker frequency of this radiation in most cases has a component in the range of 13-17 hz. This characteristic is fairly independent of the fuel and the size of the pilot flame.
In the past an analog circuit has been used to sense for presence of this flicker in the intensity of the radiation emanating from the location of the pilot flame. However, the relatively large size of components for an analog-based flame sensing system for the low frequencies involved here, cannot be easily included on a single circuit board with the smaller digital and logic-based circuits which are now more and more often being used to implement other functions of typical fuel burners. This necessitates a separate flame sensor board or a larger single board with a larger power supply, resulting in turn in undesirable expense and inconvenience.
BRIEF DESCRIPTION OF THE INVENTION
The so-called fast Fourier transform (FFT) is a mathematical algorithm which has been used for signal frequency analysis for some time. When one desires to sense the presence of frequencies in a neighborhood of a particular single frequency, one can use a variation of the FFT called the discrete Fourier transform (DFT). A circuit for detecting presence of a radiation source such as a pilot flame having a significant flicker in its energy within a predetermined frequency range may use a particular variation of the DFT for the purpose of pilot flame detection. Such a circuit receives from a photocell a flame signal instantaneously representative of the intensity of the energy emanating from the flame. A simple analog low pass filter receives the flame signal and providing a filtered flame signal from which a substantial percentage of the amplitude of frequencies above the predetermined frequency range has been removed. This prevents the higher frequencies from simulating the flicker frequency of interest, a condition known as "aliasing", which is possible when using a DFT.
A clock circuit provides a clock signal having individual pulses at four times the frequency of the midpoint of the predetermined frequency range. For a common flicker frequency of 15 hz., it is convenient to use the normal 60 hz. power as the source of the clock signal. An analog to digital converter receives the filtered flame signal and the clock signal, samples the filtered flame signal responsive to each clock signal pulse, and provides a digital flame signal having a plurality of successive discrete, ordinally designated, digital values each encoding the amplitude of the filtered flame signal at successive sampling instants over a predetermined sampling interval. A first accumulator register receives the digital flame signal and forms from the plurality of digital values comprising the flame signal, the sum of the difference of successive pairs of even numbered ordinal digital values and provides at the end of each sampling interval a first intermediate digital transform signal encoding the current contents of the first accumulator register. A second accumulator register receives the digital flame signal and forms the sum of the difference of successive pairs of odd numbered ordinal digital values for the predetermined sampling interval, and provides at the end of each sampling interval a second intermediate digital transform signal encoding the current contents of the second accumulator register.
A calculator means receives the first and second intermediate digital transform signals from their respective accumulator registers and provides a transform signal digitally encoding a value at least approximately equal to the square root of the sum of the square of the digital values encoded in each of the first and second intermediate digital transform signals. That is, the actual computed value encoded in the transform signal to be used in the next phase of the operation of this apparatus should have at least the accuracy of an approximation of the precise value. A comparator means receives the transform signal from the calculator means and compares the value encoded in the transform signal with a predetermined transform constant value, and if greater than the transform constant value, issues a flame sense signal signifying presence of flame.
All of these elements except for the photocell analog low pass filter, and clock means can be formed by the proper programming of a microprocessor, and in fact this is the preferred embodiment for the invention.
Accordingly, one purpose of the invention is to reduce the size and power requirements of the flame sensing system in a burner control system.
A second purpose of the invention is to allow the flame sensing system to be included in the micro electronics package containing the control circuitry for the burner.
Yet another purpose of the invention is to allow changes in the sensitivity and response of the flame detector by software means only.
A further purpose is to increase the accuracy and reliability in detecting presence of a flame in a burner.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of electrical circuit employing discrete components to implement the invention.
FIG. 2 is a block diagram of a system implementing the invention using a microprocessor to perform the functions of the digital and logical blocks of FIG. 1.
FIGS. 3A and 3B flow diagram of instructions which may be loaded into the microprocessor of FIG. 2 to implement the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
This invention is for detecting a flame which has in its energy output intensity a flicker whose frequency is within a predetermined frequency range. The detection process used involves the so-called discrete Fourier transform (DFT) calculation to sense the presence of a component of the flicker frequency in the flame. In FIG. 1, a conventional burner 11, which may be a pilot burner such as is used in a conventional furnace or heater, produces a flame sensed by a photocell 12. The photocell 12 provides a flame signal on path 17 which is instantaneously representative of the intensity of the energy emanating from the flame. For the typical pilot flame, there is a frequency component in this flame signal within the 13-17 hz. range whose presence is a sufficient condition for the presence of a pilot flame, even though there are invariably many other frequencies present in the composite signal as well. This frequency component arises from the flow velocity, pressure, and combustion characteristics of the gaseous fuel supplying the typical pilot burner 11, and is independent of the size or design of the pilot burner itself. However, the overall signal energy of this frequency component is substantially less than the signal energy of other frequencies present These other frequencies typically are radiated by the hot surfaces of the furnace interior after the pilot flame goes out, and thus of course provide no indication of the presence of any pilot flame. Accordingly, it is necessary to carefully tune a detector intended to sense presence of this frequency component, to detect frequencies within this 13-17 hz. range.
The flame signal on path 17 is filtered by a low pass filter 14 which comprises a series resistor 15 and a shunt capacitor 16 as shown. Preferably filter 14 has a cutoff frequency of approximately 20 hz., so that the amplitude of frequencies above 20 hz. is substantially attenuated. The output of filter 14 is a filtered flame signal on path 18 which is supplied to an analog to digital (A/D) converter 20. In response to an enable sample signal on path 22, A/D converter 20 provides a digital flame signal on path 21 which digitally encodes the digital value of the amplitude of the filtered flame signal at the instant that the enable sample signal on path 22 occurred. The range of converter 20 must be great enough to assure that there is no clipping of the input voltage level of the filtered flame signal reflected in the digital output. The enable sample signal is provided at fixed intervals by other circuitry of FIG. 1, and it is strongly preferred that the enable sample signal occur at four times the rat of the flame signal frequency to be detected. Other sampling rates are possible, but any other rate involves substantially more complicated calculations to determine the DFT value of interest. When the invention is implemented within a simple and low powered microprocessor, complicated calculations are not easy to make, and such an implementation is the most likely. For the remainder of this description, the sampling rate of four times the DFT frequency will be assumed.
One can consider the output of A/D converter 20 as comprising a series of successive discrete, ordinally designated, digital values each encoding the magnitude of the filtered flame signal on path 18 at successive sampling instants occurring at the fixed enable sample rate. If a specific digital value is chosen as the first for a detection calculation, then it and the succeeding values may also be ordinally designated as well, as x 0 , x 1 , etc., with the subscripts forming the successive ordinal designations of the digital sample values.
The elements of FIG. 1 which will now be discussed will typically form parts of a microprocessor which is programmed to at the appropriate instants of time, perform the functions which the elements involved provide. In fact, many such microprocessors also include an A/D converter 20 as part of the package containing the microprocessor.
The digital flame signal on path 21 is supplied to the input of an output multiplexer 24. Such a multiplexer has a number of output paths 26-29, each of which has a unique address. The multiplexer 24 provides the binary digits encoded on its digital data input path 21 to the one of the output paths 26-29 whose address is specified by the address encoded in the signal on an address path 23. All of the output paths 26-29 except for the one designated by the two bit address path 23 carry a digital value of zero. That is, the digital data on the input path 21 is carried by the output path 26, 27, 28 or 29 of multiplexer 24 accordingly as the input on the two bit address path 23 encodes a zero, one, two, or three. Output paths 26-29 which are not designated by the two bit address on path 23 encode a digital value of zero.
To understand the processing which is performed using the digital flame signal provided on path 21 it is useful to examine the mathematical expression of the discrete Fourier transform (DFT) which is employed here. A flicker signal generated when flame is present will almost always have a detectable frequency component at 15 hz. using the system being described, and will essentially never have such a component when no flame is present. As mentioned earlier, one can consider the A/D converter 20 as providing a plurality of successive discrete, ordinally designated, digital values each encoding the magnitude of the filtered flame signal on path 18 at successive sampling instants. The general theory for calculating a DFT for a waveform can be considerably simplified when the values of the waveform are sampled at a rate four times that of the DFT target frequency. In this simplified case, calculating the DFT involves forming two related summations to be explained shortly. For the purpose of reliably detecting presence of a pilot flame, it has been found to be sufficient to continue the summation over eight successive cycles of the 15 hz. frequency component. In the first summation, the sum of the difference of successive pairs o digital values having even ordinal designations must be formed. For the second summation, the sum of the difference of successive pairs of digital values having odd ordinal designations must be formed. If the first series value is designated A, and the ordinal designation of the successive digital values is represented by a subscript of from 0 to 31, then A=x 0 -x 2 +x 4 -x 6 +. . . +x 28 -x 30 . (Equation 1) Similarly, the equation for the second series summation of the digital values can be written as B=x 1 -x 3 +x 5 -x 7 + . . . +x 29 -x 31 . (Equation 2) The DFT for this wave form as sampled by converter 22 at these precise intervals is then given by D=(A 2 +B 2 ) 1/2 . (equation 3) It is possible to use other than precisely 32 samples for a single calculation, but I have found 32 to be adequate for accurate and reliable flame detection without excessive calculations or time required. At any rate, with this detection algorithm, the number of samples involved in a single evaluation should be a multiple of four.
To allow sampling to occur at exactly four times the rate of the target frequency of 15 hz., the enable sample signal must occur at 60 times per second. It is extremely convenient to use the standard 60 hz. power wave form as the clock which generates the enable sample signal on path 22 which controls the sampling of the filtered flame signal on path 18. Accordingly, a 60 hz. AC signal on paths 50 and 51 is placed across a voltage divider comprising resistors 52 and 53. The common point 54 of these resistors provides a low voltage 60 hz. sine wave input to a square wave generator 58 which produces a 60 hz. square wave output on path 22. As mentioned earlier of course, the individual square wave pulses on path 22 enable successive samples of the filtered flame signal on path 18. The square wave signal on path 22 is also provided to a two bit counter 56 and a five bit counter 57 to increment the contents of each of these counters by one each time a pulse is provided to the input on path 22. It can be seen that two bit counter 56 counts from 0 to 3 decimal (0 to 11 binary) and then returns to 0 and continues cycling in that manner. Similarly, five bit counter 57 advances by one in response to each pulse on path 22 and after reaching 31 (11111 binary) returns to 0 and continues to advance with each additional pulse. It may well be more convenient to use the two least significant bits of five bit counter 57 as two bit counter 56, and this is completely acceptable.
For sequencing purposes, it is necessary to employ a start signal provided by some external controller on path 30. With respect to counters 56 and 57, this signal is applied to clear (CLR) inputs which cause the counter 56 or 57 to be reset to 0. In addition, counter 57 provides a carry from its high order bit, bit 4 (the low order bit being bit 0), to indicate that 32 pulses have been applied to it since the counter 57 was last cleared. This bit 4 carry signal is applied to a one shot 60 which provides an output pulse whose duration is set by the internal characteristics of one shot 60.
Multiplexer 24 along with an A accumulator 33 and a B accumulator 34 are the circuit elements directly involved with forming the two series summations of equations 1 and 2. While these two accumulators are shown here as discrete hardware elements, it is very likely that in a preferred embodiment using a microprocessor, these accumulators will be individual registers within the microprocessor memory. In such a case, the arithmetic unit of the microprocessor alternately cooperating with each of the registers to function as a part of one or the other of the accumulators. Each accumulator 33 or 34 has an add input and a subtract input, as the labeling indicates. Data on add input path 26 or 28 is added to the value stored in an accumulator 33 or 34 respectively responsive to a strobe signal on path 22. Similarly, the data on subtract path 27 or 29 is subtracted from the value in the respective accumulator 33 or 34 responsive to a strobe signal on path 22. It can thus be seen that individual digital values comprising the digital flame signal on path 21 are gated to one of the four output paths 26-29 of multiplexer 24 according to the value contained in two bit counter 56, and each is then added to or subtracted from the respective accumulator contents. The start signal on path 30 clears the accumulators 33 and 34 prior to forming these two series. It can be seen that as two bit counter 56 continuously increments from 0 through 3, resets back to 0 and counts up again through 3, each digital value from A/D converter 20 which is presented on path 21 when the two bit counter 56 is 0 is provided on path 26 to accumulator A 33 to be added to its contents. When the contents of two bit counter 56 equals 1 the digital value on path 21 is provided to accumulator B 34 to be added to its contents. When the contents of two bit counter 56 equals 2 then the digital value on path 21 is provided on path 28 to be subtracted from the contents of accumulator A 33. And lastly when the contents of two bit counter 56 equals 3 then the digital value on path 21 is gated to path 29 or subtraction from the contents of accumulator B 34.
This sequence of cycling incrementally through two bit counter 56 occurs precisely eight times at which time five bit counter 57 crosses from a decimal value of 31 to 0 and a carry is provided on the bit four carry output of counter 57. In this way exactly 32 sequential digital values are made available to compute the A and B summation series. The bit four carry signal is used to set one shot 60 which provides an enable signal on path 61 to a first arithmetic element 40 which receives the series summations in the A accumulator 33 and the B accumulator 34 on path A 37 and path B 38 respectively. Arithmetic module 40 computes the value (A 2 +B 2 ) 1/2 and provides a digital representation D of this value encoded in a signal on path 42. It is possible to employ an approximation for computing the value of D, and one possible formula for an acceptable approximation is explained in connection with the software implementation of FIGS. 3A and 3B. Thus, it may be said that if D is calculated by such an approximation, it is at least approximately equal to the precise value of D, and such precision is typically acceptable.
The value D is the actual DFT value for the flame signal on path 17 at 15 hz. To determine whether the 15 hz. frequency amplitude component in the flame signal on path 17 is sufficiently strong to indicate the presence of a flame, the value D is tested to be greater than a constant value Z provided on path 41, and this test is performed by a digital comparator shown as test element 45. As with the accumulators 33 and 34, this test element will usually comprise circuitry within a microprocessor. If the inequality is true then a flame sense signal is provided on path 47. This flame sense signal may be used for example as a precondition for opening the main valve of a burner, since this inequality assures that a pilot flame is present. The value Z should normally be equal to approximately four to five times the peak voltage of the filtered flame signal applied to the input of the A/D converter 20, taking into account any scale factor which the A/D converter uses in determining the individual digital values indicative of the instantaneous flame signal voltage.
While FIG. 1 is a block diagram of a dedicated discrete component system for performing the operations of this invention, FIG. 2 shows a system having identical functions but implemented with a microprocessor 62 which performs all of the functions shown in FIG. 1 except for the square wave generation and initial signal acquisition and filtering. Such a microprocessor is currently available on the market with input channels such as shown connected to input paths 21 and 22 and a memory 62a in Which instructions for accomplishing the computations of a DFT may be stored. Such a microprocessor 62 also includes computational and arithmetic capabilities in circuitry 62b, data storage in registers 62c which typically comprise a random access memory, and overall control and decision making capabilities in the circuitry shown generally as 62d. In particular, the instructions stored in memory 62a are selected so as to cause microprocessor 62 to function as the individual elements shown in FIG. 1 as directed by the instructions in memory 62a.
FIGS. 3A and 3B together form a flow chart of instructions which will direct microprocessor 62 to function as the individual elements shown in FIG. 1. In FIGS. 3A and 3B, rectangular boxes are activity elements which denote instructions performing arithmetic and data transfer operations. Diamond-shaped boxes denote decision making elements. Within individual activity elements, a horizontal arrow denotes transfer of data identified o the left side of the arrow to the location specified on the right side of the arrow. Parentheses conventionally indicate the numeric or logical contents or value of whatever register or element is contained within the parentheses. It should be understood that microprocessor 62 will typically have many other functions to perform besides those related to this invention. In particular, there will typically be a control or executive software module which directs individual operating modules of the software to execute their functions as appropriate. Typically, some signal will be provided within microprocessor 62 which will eventually culminate in what is shown in FIG. 1 as the start signal encoded in the signal on path 30.
It is desirable to test for flame at many times during a complete burner operating sequence, and each of these individual test times will typically be selected by microprocessor 6 operations. Each time that such a test time occurs, a short preset routine comprising instructions forming activity element 64 are executed. These presetting instructions clear five bit counter which may be a register forming one of the registers 62c, and also clear the A and B accumulators which will typically comprise two other registers of the registers 62c. The internal signals of microprocessor 62 which initiate this presetting operation correspond to the start signal carried on path 30 of the circuit of FIG. 1.
The 60 hz. square wave signal is applied to an input 22 of microprocessor 62 which causes an internal interrupt within microprocessor 62 transferring execution of instructions to the A connector element 69 shown in FIG. 3A, meaning that instructions commencing with decision element 70 and those following will be executed. The execution of instructions by microprocessor 62 is so fast compared with the 60 hz. sampling rate of A/D converter 20 that in every case the entire calculation plus whatever other functions which it may be necessary for microprocessor 62 to perform, have occurred before the next interrupt to connector element 69 occurs. The internal interrupt signal is simply one form of the enable sample signal on path 22 of FIG. 1. As shown in FIGS. 1 and 2, the signal on path 22 is also provided to an A/D converter 20 which provides a digital flame signal on path 21 to an input channel of microprocessor 62.
The flow chart elements starting with connector 69 perform the actual update on a digital value to a digital value basis for computing the A and B summation series discussed earlier. After the last of the 32 values for a single DFT computation has been received and processed, the actual DFT value D is computed and compared with the constant shown on path 41 in FIG. 1, to determine presence of a flame. In this embodiment, it is likely that this constant is internally stored by microprocessor 62. Decision elements 70-72 and activity elements 75-78 compute the actual values of the A and B summation series. It is convenient to use the two least significant bits (LSB) of the five bit counter which counts the total number of digital data values provided by the A/D converter 20 to determine the position in the ordinal designation of each digital value and hence what series and what sign is required when the value is summed with the accumulator A or B value.
As indicated by decision element 70, if the two least significant bits (LSB) of the five bit counter equal 00 (binary) then execution passes to the instructions represented by activity element 75. These instructions read up the input from A/D converter 20 currently available on the associated input channel and read up the contents of the register functioning as accumulator A, add these two values together and store the value back into the register functioning as accumulator A.
If the two least significant bits of the five bit counter equal 01 binary, then the instructions of decision element 71 cause the instructions of activity element 76 to be executed. These instructions represented by element 76 take the input from the A/D converter 20, add that digital value to the contents of the register functioning as accumulator B, and stores this sum back into accumulator B.
If the two least significant bits of the five bit counter are unequal to 01, then execution of instructions instead passe to the instructions represented by decision element 72. If the instructions of decision element 72 find the two least significant bits of the five bit digital value counter to be equal to 10 (binary), then execution passes to the instructions represented by activity element 77. Instructions of this element 77 cause the contents of the register serving as accumulator A to be read up, and then the input from the A/D converter 20 to be read up and subtracted from the contents of accumulator A. This difference is then stored back into accumulator A.
If the two least significant bits of the five bit counter are unequal to 00, 01, and 10 as sensed by the instructions of decision elements 70-72, then control is transferred to the instructions comprising activity element 78 as symbolized by the B connector 80. The instructions of element 78 cause the contents of the register functioning as accumulator B to be read up and from this value the input from the A/D converter 20 is subtracted. This difference value is then stored back into the register serving as accumulator B. It can be seen that the instructions symbolized by the activity and decision elements discussed above for computing the values in accumulators A and B in essence cause the microprocessor 62 to momentarily comprise multiplexer 24 and the A and B accumulators 33 and 34 of FIG. 1.
After one of the instruction groups for elements 75, 76, 77, or 78 have been executed during a pass through the program and the digital flame signal value has been added to or subtracted from the appropriate accumulator, control then passes to C element connector 81 and the instructions symbolized by activity element 82. The instructions of this element 82 simply increment the contents of the five bit counter by 1 and store that value back into the five bit counter. Then the contents of the five bit counter are tested, and if equal to 0 this implies that the contents of the counter has advanced to 32 (decimal) on the previous pass through this sequence of instructions because this last increment by the instructions of element 82 changed the value from 31 to 0. If the counter value is unequal to 0 then control is returned to the executive portion of the software module for further processing of other functions of the burner control system. If however, the five bit counter is equal to 0 then the A and B summation series of equations 1 and 2 has been computed, and the value D=(A 2 +B 2 ) 1/2 can be computed.
Because the small microprocessors likely to be used in these applications typically perform multiplications and extract square roots very slowly, it is frequently preferable to use an approximation so as to save instruction execution time for other functions. An appropriate approximation here is given by (A 2 +B w ) 1/2 ˜ A +B/4, where A>B. The division by 4 can be accomplished easily with a right shift of the value of B two binary places. This approximation is accurate to within 5% for the values which will typically occur for A and B, and 5% is more than adequate accuracy. Of course, the reader understands that where B>A, that B +A/4 must be calculated.
To implement this approximation algorithm, the instructions represented by decision element 84 compares the magnitude A of the contents of accumulator A with the magnitude B of the contents of the register containing accumulator B, and if A>B, then the instructions represented by activity element 85 are executed. These instructions cause the contents of accumulator B to be right shifted two places, which is the same as a divide by 4 without rounding, and then store this right shifted value back into the register functioning as accumulator B. If B>A, then the result of activity element 87 is that value A is divided by 4 by a right shift of two and this result stored back into the register functioning a accumulator A. Then regardless of whether the instructions of activity elements 85 or 87 were executed, instruction execution proceeds with those represented by decision element 90. The sum of the contents of the registers functioning as accumulators A and B are compared with a constant value and if the sum is greater than the constant value then the instructions represented by activity element 92 are executed. These instructions set a flame sense flag equal to 1, which symbolizes that flame has been detected. The flame sense flag value may be made available externally on path 47 if desired, or may be used as the criteria for further operations in a burner operation sequence If the sum of the contents of the registers functioning as accumulators A and B is equal to or less than the constant value, then the flame sense flag is cleared by the instructions which activity element 91 represents. In either case, then operation returns to the executive portion of the program for further operation in the burner control sequence.
The preceding describes my invention.
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A circuit for detecting presence of a flame receives a flame signal from a standard photocell positioned to receive radiation from the flame and digitally processes the amplitude variations in the photocell's output to sense for the presence of frequencies near a frequency which is characteristic of a flame. The frequencies substantially higher than the characteristic frequency are filtered from the signal, and the remaining signal is sampled at a frequency which is preferably four times the characteristic frequency. The samples are converted to digital values and processed using a discrete Fourier transform. If the value resulting from the transform operation exceeds a preselected value, presence of a flame is essentially certain. Such digital processing allows use of a dedicated microcircuit or a microprocessor for the flame sensing function and avoids the need for many large discrete components.
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BACKGROUND OF THE INVENTION
The present invention relates generally to pinball games and more particularly to a drop target assembly for a pinball game.
In a pinball game, a pinball is propelled into play on a playfield and strikes various elements with each strike typically registering a score. Among these elements are drop targets which are strip-like members mounted for vertical movement between an upper position in which the target member is located above the surface of the playfield and a lower position in which the target member is located below the playfield. The drop target member is normally maintained in its raised position by a latch which permits the target member to drop to its lower position in response to impact, from a pre-determined direction, by a pinball in play on the playfield. When the target member drops from its raised to its lowered position, a score is registered.
Normally, drop target members are arranged in banks or groups, e.g., with four or five drop target members in a group. Conventionally, all target members in a group are elevated simultaneously to their raised positions and initially maintained there, and then each target member is dropped to its lowered position individually in response to the impact of a pinball on that particular drop target member. When all the target members in a group have been dropped to their lowered position, a switch is closed which actuates a mechanism to elevate all of the drop target members in the group simultaneously back to their raised positions, and the entire sequence is then repeated.
The procedure described in the preceding paragraph is conventional for operating a group of drop target members. However, the conventional procedure offers little variation in play and, after awhile, may become dull or boring to the pinball player who typically seeks a variation in challenges to his skill.
SUMMARY OF THE INVENTION
In accordance with the present invention, a mechanism is provided for varying the number and arrangement of drop target members which are exposed to impact by a pinball at various times during a given pinball game. For example, assume that, in the initial stages of the game, all five drop target members in a group have been elevated to and maintained in their raised positions, at least initially, and then, one by one, the members are dropped to their lowered positions in response to the impact of a pinball on individual members of the group. However, when this occurs in a pinball game of the present invention, all five members of the group are not both elevated to and then maintained in their raised positions. Instead, although the entire group is elevated, less than the entire group is maintained in the raised position.
For example, elevated members 1, 3 and 5 may be maintained in their raised position while elevated members 2 and 4 drop to their lowered position before a pinball is put into play. Then, when the three raised members (1, 3 and 5) have been dropped to their lowered position in response to individual impacts by a pinball, a third and different arrangement of drop target members is maintained in the raised position, e.g., members 2 and 4, for example, with members 1, 3, and 5 being dropped to their lowered position. This type of variation continues for essentially the length of the game, with a different number and arrangement of target members being maintained in the raised position each time a group is elevated.
The particular number and arrangement of target members and the sequence in which the different arrangements of target members are raised during a game is governed by a controller unit comprising a microprocessor connected to the drop target assembly. Each time all target members in a group attain the lowered position, the controller actuates mechanism which changes the number or arrangement, or both, of drop target members which are maintained in the raised position in accordance with a sequence which has been programmed into the microprocessor.
Appropriate mechanical and electromechanical structure is provided to inform, and respond to the orders of, the controller.
Other features and advantages are inherent in the structure claimed and disclosed or will become apparent to those skilled in the art from the following detailed description in conjunction with the accompanying diagramatic drawing.
BRIEF DESCRIPTION OF DRAWING
FIG. 1 is a front view of a drop target assembly in accordance with an embodiment of the present invention;
FIG. 2 is a vertical sectional view taken along line 2--2 in FIG. 1, showing a drop target member in a raised position;
FIG. 3 is a side view of the assembly, viewed from the left in FIG. 1;
FIG. 4 is a bottom view of the assembly;
FIG. 5 is a perspective, partially cut away, of the assembly;
FIG. 6 is a sectional view, similar to FIG. 2, showing a drop target member in a lowered position;
FIG. 7 is a schematic diagram illustrating some of the electrical components in the assembly; and
FIG. 8 (sheet 2) is an enlarged, fragmentary vertical, sectional view of a portion of the assembly.
DETAILED DESCRIPTION
Referring initially to FIGS. 1-6 there is shown a drop target assembly constructed in accordance with an embodiment of the present invention. The drop target assembly includes a sheet metal frame comprising a base member 10 having front and rear flanges 11, 12, respectively. The sheet metal frame also includes first and second side frame members 13, 14, respectively and front and back frame members 15, 16, respectively. The various members of the sheet metal frame 10-16 are connected together by conventional fastening means such as screws 17.
Extending between first and second side frame members 13 and 14 and freely, pivotally mounted thereon is a shaft 20 on which are freely pivotally mounted a plurality of link members 21 extending rearwardly from their mounting on shaft 20 toward back frame member 16. Opposite ends of shaft 20 extend outwardly beyond side frame members 13, 14, and shaft 20 is held against axial movement relative to side frame members 13, 14, by spacer members 23, 24 attached by screws 25, 26 to respective opposite ends of shaft 20.
Mounted on each opposite end of shaft 20 is one end of a respective connecting element 27, 28 extending rearwardly from shaft 20 and terminating at another end pivotally connected to a respective opposite flange 29, 30 of an elevating bar 31. Connecting element 27 is also pivotally connected at 39 (FIGS. 1 and 3) to the bottom end of a vertical link element 32 extending upwardly and terminating at another end located within a slot 36 in a reciprocating arm 34 of a solenoid 35. Vertical link element 32 is pivotally connected at 33 to solenoid arm 34.
Solenoid 35 is mounted to side frame member 13 by upper and lower attachment brackets 37, 38, respectively. Actuation of solenoid 35 raises solenoid arm 34 and vertical link element 32 upwardly, in turn causing connecting elements 27, 28 to pivot upwardly about the axis of shaft 20. This raises elevating bar 29, in turn causing link members 21 to pivot upwardly about the axis of shaft 20.
The rearward end of each link member 21 is pivotally connected at 40 to the bottom end of a shank 41 of a drop target member 42. Drop target member 42 and its shank 41 move up and down with the rearward end of its corresponding link member 21, and shank member 41 is guided, during its vertical movement, by a slot 43 in the flange 44 of a guide member 45 attached to back frame member 16.
As noted above, the actuation of solenoid 35 raises elevating bar 29 which in turn pivots link members 21 upwardly. This elevates each of the drop target members 42 from the lowered position of FIG. 6 to the raised position of FIG. 2.
When a target member 42 is elevated to its raised position, it is normally maintained there by the engagement of a latch finger 50 of a latch 51 beneath a protrusion 52 on target member 42. The cooperation of latch finger 50 and target member protrusion 52 maintain the target member in its raised position until either target member 42 is pushed off latch finger 50 or the latch finger is withdrawn from under protrusion 52 on the target member.
Also cooperating to maintain target member 42 in a latching relationship with latch finger 50 is a spring 46 having a lower end connected at 47 to a middle part of link member 21 and an upper end connected at 48 to an upper part of shank 41 of the drop target member. Spring 46 normally urges drop target member 42 to pivot about the axis of pivotal connection 40, in a frontward direction, and this pivotal action is limited by the engagement of protrusion 52 with a stop bar 49 extending between first and second side frame members 13, 14.
Latch finger 50 is normally maintained in an operative position for engaging beneath the bottom of target member protrusion 52 by structure shown in FIGS. 2, 4, 6 and 8.
Latch 51 is mounted, on a latch bracket 56, for rocking movement between a rearward, operative or latching position illustrated in FIGS. 2 and 6 and a forward, inoperative position in which latch 51 engages against a solenoid electromagnet 57 mounted on a front flange 58 of latch bracket 56. Flange 58 is in turn mounted on front frame member 15.
Located along opposite vertical margins of latch 51, near the bottom thereof, are a pair of slots 60, 60 (FIGS. 4 and 8) through which extend a pair of fingers 61, 61 at the rear of latch bracket 56. Latch 51 also includes, near its bottom end, an opening 62 through which extends a tongue 63 at the rear end of latch bracket 56. Tongue 63 curves upwardly to help maintain latch 51 on latch bracket 56. The bottom of latch 51 is connected, below latch bracket 56, at an ear 64 to one end of a coil spring 65 having another end connected at 66 to the forward end of latch bracket 56. Coil spring 65 rocks latch 51 on latch bracket 56, rearwardly to the operative position illustrated in FIG. 2. A stop bar 67 limits rearward movement of latch 51. Stop bar 67 is composed of non-magnetic material such as brass and extends between side frame members 13, 14.
When target member 42 is in its raised position (FIG. 2), it normally projects above the top surface 55 of the playfield on a pinball game, through a slot 68. When target member 42 is struck by a ball, moving in a direction from the front to the rear of the drop target assembly (to the right in FIG. 2), the drop target member is caused to pivot to the rear about the axis of pivotal connection 40 located at the lower end of drop target shank 41. This is pivotal movement in a clockwise sense as viewed in FIG. 2. When this occurs, the protrusion 52 on drop target member 42 is pushed off the rearward end of latch finger 50, and the drop target member falls from the raised position of FIG. 2 to the lowered position of FIG. 6.
Each of the drop target members 42 is mounted for movement, independent of the other drop target members, between its raised position (FIG. 2) and its lowered position (FIG. 6) in which the drop target member is located below the playfield. When a drop target member 42 is located below the playfield, it is no longer visible to a player and is no longer a target for a pinball.
As a target member 42 drops, the link member 21 connected thereto also drops, pivoting about the axis of shaft 20, from the position illustrated in FIG. 2 to the position illustrated in FIG. 6. Link member 21 includes, at its rearward end, a terminal portion 70. During pivotal movement of the link member, terminal portion 70 is received in and guided by a slot 71 in back frame member 16 and a slot 72 in rear flange 12 of base member 10. Also, the front end 53 of each link member is received and guided within a guide slot 54 in front flange 11 of base member 10 (FIG. 5).
As link member 21 drops from the position of FIG. 2 to the position of FIG. 6, terminal portion 70 engages a cam member 75 on a switch 76 and closes or engages the terminals 77, 78 of switch 76. Switch 76 is mounted by a bracket 74 on back frame member 16. There is a switch 76 for each drop target member 42 and its corresponding link member 21. When all of the switches 76 for each of the drop target members in the assembly have been closed, solenoid 35 is actuated to raise elevating bar 31, in turn elevating all of the drop target members 42 back to the raised positions of FIG. 2.
When the drop target members 42 are elevated to their raised positions by the elevating bar 31, normally all of the drop target members in the assembly are engaged by their respective latches, and, absent the actuation of some additional mechanism, all of the drop target members in the assembly will be maintained in the raised position each time they are elevated to that position by elevating bar 31. Now to be described is a mechanism which is actuable to cause selective drop target members in the assembly to be dropped to their lowered positions, out of play, after all the drop target members in the assembly have been elevated to their raised positions.
As noted above, located adjacent each rockable latch 51 is a solenoid electromagnet 57, one for each latch. An electromagnet 57 and its corresponding rockable latch 51 together constitute a form of solenoid. When the electromagnet 57 for a given latch 51 is energized or actuated, the corresponding latch is urged frontwardly toward electromagnet 57 until a contact element 80 on latch 51 engages a contact element 81 on electromagnet 57. When latch 51 is thus retracted, it is no longer in a position in which latch finger 50 will engage beneath protrusion 52 on the corresponding drop target member 42 when the latter is in its raised position. Accordingly, when elevating bar 31 is dropped to its normal, lowered position, all those drop target members 42 which are unsupported by a latch finger 50, will also drop to their lowered positions.
In a normal sequence of operation, elevating solenoid 35 is actuated only long enough to cause elevating bar 31 to elevate all of the drop target members 42 to their raised position and to allow latch fingers 50 to engage beneath protrusions 52. Then, elevating solenoid 35 is deactuated, causing elevating bar 31 to drop by gravity to its lowered position. Next, predetermined latch-retracting electromagnets 57 are actuated, but only long enough to permit the corresponding drop target members to drop to their lowered positions, following which these latch-retracting electromagnets 57 are deactuated, allowing the corresponding latches 51 to return to their normal position, illustrated in FIG. 2, in response to the urging of coil springs 65.
The drop target assembly includes a mechanism operable to actuate individual latch-retracting electromagnets 57 in accordance with a predetermined program, and this mechanism will now be described, with reference to FIG. 7. Each of the switches 76 is connected to a controller 82 in turn conncted to an individual target solenoid driving unit (S.D.U.) 83 as well as a reset solenoid driving unit (S.D.U.) 84. Controller 82 comprises a microprocessor which includes a read only memory unit, input and output coupling circuits, and the like. It is of conventional construction and may be programmed to perform the functions described below.
Reset solenoid driving unit 84 is connected to a coil 135 of elevating solenoid 35. When all of the switches 76 have been closed, this is noted by controller 82 which, in turn, sends a signal to reset solenoid driving unit 84 which energizes coil 135 in elevating solenoid 35 to actuate solenoid 35 and raise elevating bar 31.
Individual target solenoid driving unit 83 is connected to a plurality of coils 157-557 each for actuating a respective electromagnet 57. Each time all of the switches 76 are closed, various combinations of the coils 157-557 are actuated in accordance with a predetermined program which has been set into unit 82. For example, the first time controller 82 senses that all of switches 76 have been closed, it will instruct unit 83 to actuate only coils 157 and 557. This would cause the target members corresponding to coils 157 and 557 to drop, closing their corresponding switches 76, while leaving in their raised positions the target members corresponding to coils 257, 357 and 457. Subsequently, when the switches 76 for the target members corresponding to coils 257, 357 and 457 have been closed, by the dropping of their corresponding target members in response to impact by a pinball, controller 82 will send another instruction to unit 83, this time to actuate coils 257 and 457, for example. The next time all of the switches 76 have been closed, controller 82 will send a still different instruction to unit 83, and so on, for each of the times controller 82 senses that all the switches 76 are closed.
The result is that only those drop target members whose particular coil among the coils 157-557 has been energized, will initially drop before a pinball is put into play, while the remainder of the target members will remain in the raised position. This causes a different combination of targets to remain for presentation to the pinball on the playfield each time the elevating bar is raised and lowered.
The particular number, arrangement and sequence in which target members remain in the raised position depends upon the particular program initially entered into controller 82, and this may vary from one controller 82 to another.
The actuation of a given electromagnet coil within the group of coils 157-557 depends not only upon the dropping to its lowered position of the target member corresponding to that given coil, but, also, it depends upon the dropping to their lowered positions of target members corresponding to other coils in the group 157-557, in response to impact by a pinball.
The foregoing detailed description has been given for clearness of understanding only, and no unnecessary limitations should be understood therefrom, as modifications will be obvious to those skilled in the art.
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A pinball game contains a plurality of drop target members each mounted for vertical movement between a raised position, above the playfield of the pinball game, and a lowered position below the playfield. Each target member is maintained in its raised position by a latch, and the target member may be knocked off its latch by impact from a pinball, causing the target member to drop to its lowered position. A latch may be withdrawn from a supportive position for its target member, causing the target member to drop without having undergone impact by a pinball. Structure is provided to elevate the target members to their raised positions, and there is a controller programmed to withdraw selected latches following the elevation of the target members.
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FIELD OF THE INVENTION
The present invention is directed to the field of storing and displaying print images, for identifying the source from which the images originated, and for storing the source of the original image.
BACKGROUND OF THE INVENTION
Typically, consumers receive individual photographic prints from photofinishers and the film negative from which the prints were made. The film negatives may be provided in cut strips loosely with the prints, or may be provided in a film cassette having a cartridge ID if the prints were obtained from APS film (Advanced Photographic System, recently introduced). The loosely provided prints tend to make it difficult for the owners to store or view the prints. When prints provided from APS film are returned to the customer, index prints are also provided. The index print allows the identifying and locating of particular images returned in the APS film cartridge. This, of course, provides an added print at added cost to the photofinisher.
In U.S. Ser. No. 08/455,770, filed May 31, 1995, entitled “Dual Sides Photographic Album Leaf and Method of Making,” there is disclosed providing to the customer one or more album leaves containing the images on the roll of film. These leaves may be used to provide all of the service prints present on the negative filmstrip. However, it is difficult to relate the images on the album page to the individual negatives from the roll of film from which it originated. The customer must first sort through the separate index prints returned to the customer, which may not be conveniently located.
Applicants have invented an improved album page and system for displaying, storing and retrieving of images which overcomes many of the storing, displaying and retrieving problems of the prior art.
SUMMARY OF THE INVENTION
The present invention is directed to overcoming one or more of the problems set forth above. According to one aspect of the present invention, there is provided an album leaf having a first side having a first image retaining section and a second side having a second image retaining section, the first image retaining section on the first side having a plurality of images, and a first icon formed thereon, the first icon individually identifying the source from which the plurality of images originated.
In accordance with another aspect of the present invention there is provided a system for displaying, storing and retrieving images, comprising:
an album leaf having a first side having a first image retaining section and a second side having a second image retaining section, the first image retaining section on the first side having a plurality of images, and a first icon formed thereon, the first icon individually identifying the source from which each of the plurality of images originated; and
a binder for containing a plurality of the album leaves, the album having a plurality of retaining means for holding items containing the original source of the images contained in the album leaf.
In accordance with another aspect of the present invention there is provided a system for displaying, storing and retrieving images, comprising:
an album leaf having a first side and a second side, the first side having a plurality of images and an icon formed thereon, the icon for individually identifying the first source from which the at least each of the plurality of images originated;
a binder for containing a plurality of the album leaves; and
a retaining album leaf having a plurality of retaining means for holding items containing the original source of the images contained in the album leaf.
In accordance with yet another aspect of the present invention there is provided a source retaining album leaf for placement in a binder having at least one album leaf placed therein, the album leaf having a first side having a first image retaining section and a second side having a second image retaining section, the first image retaining section on the first side having a plurality of images and a first icon formed thereon, the first icon individually identifying the first source from which each of the plurality of images on the first side originated, the source retaining album leaf having a plurality of retaining means for holding items containing the original source of the images contained in the album leaf.
In another aspect of the present invention there is provided an image-bearing media having a first side having a first image retaining section the first image retaining section of the first side having a plurality of images and a fist icon formed thereon, said first icon individually identifying the source from which each of the plurality of images originated.
In still another aspect of the present invention there is provided a system for displaying, storing and retrieving images, comprising:
an image-bearing media having a first side having a first image retaining section and a second side having a second image retaining section, the image retaining section on the first side having a plurality of images formed on the first side originating from a first source and an icon also formed on the first side for individually identifying the source from which each of the plurality of images originated; and
a binder for containing the album leaf, the album having a plurality of retaining means for holding items containing the first source of the images contained in the album leaf.
The above, and other objects, advantages and novel features of the present invention will become more apparent from the accompanying detailed description thereof when considered in conjunction with the following drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
In the detailed description of the preferred embodiments of the invention presented below, reference is made to the accompanying drawings in which:
FIG 1 is a front elevational view of an album leaf made in accordance with the present invention;
FIG. 2 is a back elevational view of the album leaf of FIG. 1 ;
FIG. 3 is a perspective view of a sheet of photographic material illustrating how the album leaf of FIGS. 1 and 2 may be formed;
FIG. 4 is a perspective view of a photographic album containing a plurality of album leaves made in accordance with the present invention; and
FIG. 5 is a perspective view of an album leaf for holding a plurality of film cartridges, each containing a strip of photographic film.
DETAILED DESCRIPTION OF THE INVENTION
The present description will be directed in particular to elements forming part of, or in cooperation more directly with, the apparatus in accordance with the present invention. It is understood that elements not specifically shown or described may take various forms well known to those skilled in the art.
Referring to FIGS. 1-4 , there is illustrated an album leaf 10 made in accordance with the present invention. The leaf 10 includes a first side 12 and a second side 14 . The first side 12 includes a plurality of images 15 , 16 , 17 , 18 , 19 and the second side includes a plurality of images 21 , 22 , 23 , 23 , 25 . Also provided in the preferred embodiment is a plurality of holes 28 in a margin area 29 , which can be used for mounting of the leaf in an album. The width d of margin area 29 may be of any desired size. In the particular embodiment illustrated, the width d is about one inch (2.54 cm).
As can be seen by FIGS. 1 and 2 , the various size images are composed so as to substantially fill the space on each side 12 , 14 . Also, as illustrated, various combinations and sizes of prints may be placed together. For example, as illustrated in FIG. 1 , the images 15 , 16 , 18 , 19 are similar in size and whereas image 17 is of a substantially different size format, such as the C, H, and P formats of the Advanced Photo System. It is to be understood that any desired size images and/or number of images may be provided on either of sides 12 , 14 . The images have been either automatically composed by the printing device, or printed in accordance with customer instructions. This can be done by optical printers such as the Kodak S-Series Printer, which prints multiple images on a single web of photosensitive paper. Alternatively, digital printers, such as the Kodak PCD 600 CRT Printer and the Kodak HLT-7720 Continuous Tone Digital Printer, can be used which allows for free form formatting of the images. It is, of course, understood that other type printers, such as laser, thermal, ink jet, or electrophotographic printers, may be used as desired. In the embodiment illustrated, images 15 , 16 , 18 , 19 each have a size of about 3-½ inches×4-⅞ inches, and image 17 is equivalent to a panoramic-type image, which have a size of approximately 3-½ inches×9-¾ inches. Likewise, on the second side 14 , images 21 , 22 , 23 , 24 are substantially equal size, whereas image 25 is of a substantially greater size.
Referring to FIG. 3 , there is illustrated a sheet 30 made of an image-bearing media. In the embodiment illustrated, sheet 30 is a photosensitive material. In particular, the photosensitive material is photographic paper, which has an image forming side 32 and a backside 34 . As is typical with photosensitive material, the image forming side 32 includes an emulsion layer 33 upon which an image can be formed. The backside of the material merely provides the supporting substrate for holding of the emulsion layer. The sheet 30 has a thickness t. The thickness t may be any thickness desired. Preferably, the thickness t is minimal so that the album page will not be too thick, yet provide the desired rigidity. Generally the thickness t will be in the range of 0.05 mm to 0.5 mm. In the particular embodiment illustrated, the thickness t is approximately 0.2 mm.
As illustrated in FIG. 3 , images 15 , 16 , 17 , 18 , 19 , 21 , 22 , 23 , 24 , 25 have been formed on the image forming side 32 of sheet 30 by an appropriate printer, such as previously described. The images 15 , 16 , 17 , 18 , 19 have been composed into a first image retaining section 36 , whereas images 21 , 22 , 23 , 23 , 25 have been composed onto a second image retaining section 38 . These image retaining sections 36 , 38 may be sized and configured as desired. Preferably, the image retaining sections 36 , 38 are designed so as to correspond to the first and second sides 12 , 14 of leaf 10 , respectively. In the preferred embodiment illustrated, a space 43 having a width d 1 is provided between first and second image retaining sections 36 , 38 . Also, as preferably illustrated, a fold line 40 about which the sheet 30 is folded is provided in space 43 . The width d 1 may be any desired size. In the embodiment illustrated, width d 1 is about 1.0 inches (2.54 cm). The fold line 40 is preferably located such that the first image section 36 and second image section 38 are substantially co-extensive with each other. As illustrated, lateral edge portions 42 , 44 are disposed adjacent first and second image sections 36 , 38 , respectively, and placed adjacent each other so as to form the margin area 29 when sheet 30 is folded.
The images sent to the digital printer may be obtained by any desired manner. In the preferred embodiment of the present invention, a digital printer such as the Kodak PCD-600 CRT Printer, is used so that free form formatting can be easily obtained in accordance with instructions provided by the consumer. The digital data information is representative of the images and can be obtained by scanning original images, either in the form of prints or negatives as is customarily done in the prior art. However, the digital data information may not be limited to images. The digital data information may also contain other information such as text, or the logos, images, etc., which can be added to the scanned data. Also the digital data may be obtained in any desired manner, for example, by computers or other devices which contains digital files such as CDs or from data contained in the magnetics on film. A digital record is formed from the scanned information and any other digital information provided. This digital record is then composed into first and second digital sub-records. The first and second digital sub-records are used to print images in the first and second image retaining sections 36 , 38 , which will correspond to the sides 12 , 14 of the leaf 10 . It is, of course, understood that the images may be composed in any desired manner. Additionally, any text or other information provided, or manipulation of the data, may be conducted as desired. For example, but not by way of limitation, text, logos, or other images, could be added to the scanned images. Once the appropriate digital records have been formed, printing by the printer can then be performed whereby the images and other text/images present in the digital records are appropriately printed on the photosensitive material. The developed photosensitive material is then taken from the printer where thereafter it is formed into the leaf 10 .
Developed photographic material is folded in a manner such that the backsides are brought back against each other and an appropriate adhesive is applied therebetween for securely holding the folded sections together. It is to be understood that the formation of the album leaf may take place in any appropriate manner. U.S. Ser. No. 08/455,770, filed May 31, 1995, entitled “Dual Sides Photographic Album Leaf and Method of Making,” provides further details by which the leaf may be formed and which hereby is incorporated by reference in its entirety.
As illustrated in FIGS. 1 and 2 , icons (reference indicia) 50 , 52 , 54 are provided for identifying each of the images ( 15 - 25 ) and the source from which the images originate. In particular, referring to icon 50 , it comprises a plurality of silhouettes (an outline representation of the edges) of the actual images 15 , 16 , 17 , 18 , 19 provided on the first side 12 . Additionally, the icons may be composed of thumbnail (miniature) image representations of the actual images. In particular, there are provided silhouettes 55 , 56 , 57 , 58 , 59 , each of which refer to the location of its respective images 15 , 16 , 17 , 18 , 19 . In the embodiment illustrated, the source of the images is a filmstrip contained in a film cartridge having a cartridge ID number. The icon 50 includes an origination (source) identification 60 (ID) for identifying the source of the images. In the embodiment illustrated, the origination ID 60 is the film cartridge ID, which contains the film negative from which the images have been made. This information can be obtained by a variety of sources as previously discussed. For example, when a customer order is received by a photofinisher for printing by the photofinisher, the cartridge ID (which represents the origination ID in this case) may be manually entered into the computer controlling scanning and printing, or can be machine read by any appropriate device for reading such number. Thus, the information relating to the origination of the images may be obtained in any manner desired.
In each of the silhouettes 55 , 56 , 57 , 58 , 59 there is provided an image ID 61 . In the embodiment illustrated, the image ID 61 identifies the location of the image on the source, which in the present embodiment is a filmstrip provided within the film cartridge. In the embodiment illustrated, the numeral represents the frame number on the filmstrip and the letters represent the format of the image; PAN represents a Panoramic format, CLS represents a classic format, and HD represents a portrait format. Thus, each of the images can be quickly related to a location on the filmstrip contained within a particular film cartridge from which the images originated and its current format. It is, of course, to be understood that any other identification location system may be provided as desired having any desired number of formats.
Referring to FIG. 2 , there is illustrated the second side 14 , which has two icons 64 , 65 , each having silhouettes of the images provided on the page. However, since some of the images originated from different sources, each of the icons are associated with a different source. Thus, icon 64 provides a cartridge ID 68 from which the images 21 , 24 originated, whereas icon 66 includes a cartridge ID 70 from which images 22 , 23 , 25 originated. In the particular embodiment illustrated, it can be seen that different icons are provided for identifying different sources. It is, of course, to be understood that various other systems may be utilized for identifying different sources for each of the images. For example, the cartridge ID could be somehow provided in each of the image silhouettes, which correspond to the images on that side of the album leaf.
As previously noted, there are provided a plurality of holes 28 in the margin area 29 , which can allow the placement of the album leaf in a loose-leaf binder allowing the individual album leaves to be inserted or removed as desired. It is understood that any other type binder or holder may be used for holding the leaves through the holes 28 or any other binding system may be utilized for holding the leaves.
Referring to FIG. 4 , there is illustrated a loose-leaf notebook 72 containing a front cover 74 and a back cover 76 having a plurality of rings 87 for holding of the album containing a plurality of album leaves 10 . The rings pass through holes 28 provided in the leaves 10 . The back cover 76 contains means for holding a plurality of film cartridges 79 , each containing a filmstrip of the images provided in the leaves. In the particular embodiment illustrated, the back cover 76 is provided with a plurality of pockets 84 , each designed to hold an individual film cartridge such that the cartridge ID provided on the cartridge will be visible when that portion of the loose-leaf binder is revealed. Thus, if an individual is viewing the images on the album leaves and is interested in finding the original source reproduction, or for any other purpose, the individual simply opens up to the back and quickly locates the cartridge containing the image of interest.
It is, of course, understood that the cartridges are not required to be held in the magazine, but may be provided in a separate container wherein the cartridge IDs may be exposed or somehow otherwise written on a label placed on the back of the container.
Referring to FIG. 5 , there is illustrated a leaf 80 in notebook 72 , identical numerals representing like parts previously discussed, for holding a plurality of film cartridges 79 that may be placed within the notebook 72 . The leaf 80 includes a plurality of holes 28 , which align with the appropriate rings 78 in the binder 72 and is further provided with a plurality of pockets, each designed to receive a film cartridge. Preferably, the pockets 88 are designed such that the film cartridges 79 may be snapped in and snapped out as desired. This allows the owner of the album to either place the cartridges directly with the images, or if so desired, place them in a separate or different location from the images. Preferably, as illustrated, the pockets 88 are designed so that the cartridge ID 90 would be visible.
It is to be understood that the retaining means for holding the cartridges may be in any appropriate manner in the leaf or binder, for example, but not by way of limitation, snaps, use of Velcro™, or any other securing means that allows securing and removing of the film cartridge that is currently available, or may become available.
While the image-bearing media in the preferred embodiment illustrated is photographic media, the present invention is not so limited, for example, but not by way of limitation, images formed by laser printers and digital thermal printers can be used to print the images on the image-bearing media.
In the particular embodiment illustrated, the source of the image was a filmstrip contained in a film cartridge, however, the present invention is not so limited. For example, but not by way of limitation, the source of the image may be a photo CD, computer disc, or transmitted from a digital memory source such as PC or other digital memory device. Appropriate source ID may be provided for each of the foregoing sources.
The invention has been described in detail with particular reference to certain preferred embodiments thereof, but it will be understood that variations and modifications can be effected within the scope of the invention.
PARTS LIST
10 Album leaf
12 First side
14 Second side
15 Image
16 Image
17 Image
18 Image
19 Image
21 Image
22 Image
23 Image
24 Image
25 Image
28 Holes
29 Margin area
30 Sheet
32 Image forming side
33 Emulsion layer
34 Backside
36 First image retaining section
38 Second image retaining section
40 Fold line
42 Lateral edge portion
43 Space
44 Lateral edge portion
50 Icon
52 Icon
54 Icon
55 Silhouettes
56 Silhouettes
57 Silhouettes
58 Silhouettes
59 Silhouettes
60 Origination identification
61 Image ID
64 Icon
65 Icon
66 Icon
68 Cartridge ID
70 Cartridge ID
72 Loose-leaf notebook
74 Front cover
76 Back cover
78 Rings
79 Film cartridges
80 Leaf
84 Pockets
87 Rings
88 Pockets
90 Cartridge ID
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An improved album leaf and system for displaying, storing and retrieving images. The album leaf comprises a first side and a second side, the first side having a plurality of images formed thereon, and an icon for identifying the images on the first side and the source from which the images originated. A binder may include a plurality of the album leaves having a plurality of retaining means, for example, pockets for holding items containing the original source from which the images displayed in the album leaf originated. A separate source retaining leaf may be provided having holding means for retaining the original source from which the images displayed on the album leaf originated.
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RELATED APPLICATION DATA
This application is a continuation of U.S. patent application Ser. No. 12/198,682, filed Aug. 26, 2008 (U.S. Pat. No. 7,720,255), which is a continuation of U.S. patent application Ser. No. 11/552,436, filed Oct. 24, 2006 (U.S. Pat. No. 7,418,111), which is a continuation of application Ser. No. 10/869,320, filed Jun. 15, 2004 (U.S. Pat. No. 7,130,087), which is a continuation of application Ser. No. 09/975,739, filed Oct. 10, 2001 (U.S. Pat. No. 6,750,985), which is a division of application Ser. No. 09/127,502, filed Jul. 31, 1998 (U.S. Pat. No. 6,345,104), which claims the benefit of provisional application No. 60/082,228, filed Apr. 16, 1998 (the specification of which is attached as Appendix A).
application Ser. No. 09/127,502 is also related to application Ser. No. 08/649,419, filed May 16, 1996 (now U.S. Pat. No. 5,862,260). application Ser. No. 09/127,502 is also related to application Ser. No. 08/967,693, filed Nov. 12, 1997 (now U.S. Pat. No. 6,122,392), which is a continuation of application Ser. No. 08/614,521, filed Mar. 15, 1996 (now U.S. Pat. No. 5,745,604), which is a continuation of application Ser. No. 08/215,289, filed Mar. 17, 1994 (now abandoned).
The subject matter of this application is also related to that of the present assignee's other issued U.S. Pat. Nos. 5,636,292, 5,710,834, 5,721,788, 5,748,763, 5,748,783, 5,768,426, 5,850,481, 5,841,978, 5,832,119, 5,822,436, 5,841,886, 5,809,160, 6,122,403 and 6,026,193.
FIELD OF THE INVENTION
The present invention relates to methods and systems for inconspicuously embedding binary data in security documents, and associated methods/systems for detecting/decoding such data. (“Security document” is used herein to refer to negotiable financial instruments (e.g. banknotes, travelers checks, bearer bonds), passports, visas, other immigration documents, stock certificates, postal stamps, lottery tickets, sports/concert tickets, etc.) One application of this the invention is in discouraging counterfeiting of security documents. Another is in transferring machine-readable information through such documents, without alerting human viewers to the presence of such information.
BACKGROUND AND SUMMARY OF THE INVENTION
Digital watermarking (sometimes termed “data hiding” or “data embedding”) is a growing field of endeavor, with several different approaches. The present assignee's work is reflected in the patents and applications detailed above, together with laid-open PCT application WO97/43736. Other work is illustrated by U.S. Pat. Nos. 5,734,752, 5,646,997, 5,659,726, 5,664,018, 5,671,277, 5,687,191, 5,687,236, 5,689,587, 5,568,570, 5,572,247, 5,574,962, 5,579,124, 5,581,500, 5,613,004, 5,629,770, 5,461,426, 5,743,631, 5,488,664, 5,530,759, 5,539,735, 4,943,973, 5,337,361, 5,404,160, 5,404,377, 5,315,098, 5,319,735, 5,337,362, 4,972,471, 5,161,210, 5,243,423, 5,091,966, 5,113,437, 4,939,515, 5,374,976, 4,855,827, 4,876,617, 4,939,515, 4,963,998, 4,969,041, and published foreign applications WO 98/02864, EP 822,550, WO 97/39410, WO 96/36163, GB 2,196,167, EP 777,197, EP 736,860, EP 705,025, EP 766,468, EP 782,322, WO 95/20291, WO 96/26494, WO 96/36935, WO 96/42151, WO 97/22206, WO 97/26733. Some of the foregoing patents relate to visible watermarking techniques. Other visible watermarking techniques (e.g. data glyphs) are described in U.S. Pat. Nos. 5,706,364, 5,689,620, 5,684,885, 5,680,223, 5,668,636, 5,640,647, 5,594,809.
Much of the work in data embedding is not in the patent literature but rather is published in technical articles. In addition to the patentees of the foregoing patents, some of the other workers in this field (whose watermark-related writings can by found by an author search in the INSPEC or NEXIS databases, among others) include I. Pitas, Eckhard Koch, Jian Zhao, Norishige Morimoto, Laurence Boney, Kineo Matsui, A. Z. Tirkel, Fred Mintzer, B. Macq, Ahmed H. Tewfik, Frederic Jordan, Naohisa Komatsu, Joseph O'Ruanaidh, Neil Johnson, Ingemar Cox, Minerva Yeung, and Lawrence O'Gorman.
The artisan is assumed to be familiar with the foregoing prior art.
In the following disclosure it should be understood that references to watermarking encompass not only the assignee's watermarking technology, but can likewise be practiced with any other watermarking technology, such as those indicated above.
Watermarking can be applied to myriad forms of information. The present disclosure focuses on its applications to security documents. However, it should be recognized that the principles discussed below can also be applied outside this area.
Most of the prior art in image watermarking has focused on pixelated imagery (e.g. bit-mapped images, JPEG/MPEG imagery, VGA/SVGA display devices, etc.). In most watermarking techniques, the luminance or color values of component pixels are slightly changed to effect subliminal encoding of binary data through the image. (This encoding can be done directly in the pixel domain, or after the signal has been processed and represented differently—e.g. as DCT or wavelet coefficients, or as compressed data, etc.)
While pixelated imagery is a relatively recent development, security documents—commonly employing line art—go back centuries. One familiar example is U.S. paper currency. On the one dollar banknote, for example, line art is used in several different ways. One is to form intricate webbing patterns (sometimes termed “guilloche patterns”) around the margin of the note (generally comprised of light lines on dark background). Another is to form gray scale imagery, such as the portrait of George Washington (generally comprised of dark lines on a light background).
There are two basic ways to simulate grey-scales in security document line art. One is to change the relative spacings of the lines to effect a lightening or darkening of an image region. FIG. 1A shows such an arrangement; area B looks darker than area A due to the closer spacings of the component lines. The other technique is to change the widths of the component lines—wider lines resulting in darker areas and narrower lines resulting in lighter areas. FIG. 1B shows such an arrangement. Again, area B looks darker than area A, this time due to the greater widths of the component lines. These techniques are often used together. Ultimately, a given region simply has more or less ink.
In my U.S. Pat. No. 5,850,481 I introduced, and in my U.S. Pat. No. 6,449,377 I elaborated on, techniques for watermarking line art by making slight changes to the widths, or positions, of the component lines. Such techniques are further expanded in the present disclosure.
In several of my cited applications, I discussed various “calibration signals” that can be used to facilitate the decoding of watermark data despite corruption of the encoded image, such as by scaling or rotation. Common counterfeiting techniques—e.g. color photocopying, or scanning/inkjet printing—often introduce such corruption, whether deliberately or accidentally. Accordingly, it is important that watermarks embedded in security documents be detectable notwithstanding such effects. Calibration signals particularly suited for use with security documents are detailed in this disclosure.
In accordance with embodiments of the present invention, security documents are encoded to convey machine-readable multi-bit binary information (e.g. digital watermarks), usually in a manner not alerting human viewers that such information is present. The documents can be provided with overt or subliminal calibration patterns. When a document incorporating such a pattern is scanned (e.g. by a photocopier), the pattern facilitates detection of the encoded information notwithstanding possible scaling or rotation of the scan data. The calibration pattern can serve as a carrier for the watermark information, or the watermark can be encoded independently. In one embodiment, the watermark and the calibration pattern are formed on the document by an intaglio process, with or without ink. A photocopier responsive to such markings can take predetermined action if reproduction of a security document is attempted. A passport processing station responsive to such markings can use the decoded binary data to access a database having information concerning the passport holder. Some such apparatuses detect both the watermark data and the presence of a visible structure characteristic of a security document (e.g., the seal of the issuing central bank).
The foregoing and other features and advantages of the present technology will be more readily apparent from the following detailed description, which proceeds with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A and 1B show prior art techniques for achieving grey-scale effects using line art.
FIG. 2 shows a virtual array of grid points that can be imposed on a security document image according to an embodiment of the present invention.
FIG. 3 shows a virtual array of regions that can be imposed on a security document image according to the FIG. 2 embodiment.
FIG. 4 shows an excerpt of FIG. 3 with a line from a line art image passing therethrough.
FIG. 5 shows changes to the width of the line of FIG. 3 to effect watermark encoding.
FIG. 6 shows changes to the position of the line of FIG. 3 to effect watermark encoding.
FIGS. 7A and 7B show aspects of watermark and calibration blocks according to an embodiment of the invention.
FIG. 8 shows an illustrative reference grey-scale calibration tile.
FIGS. 9A-9C show steps in the design of a weave calibration pattern according to an embodiment of the invention.
FIG. 10 shows the generation of error data used in designing a weave calibration pattern according to an embodiment of the invention.
FIG. 11 is a block diagram of a passport processing station according to another embodiment of the invention.
FIG. 12 is a block diagram of a photocopier according to another embodiment of the invention.
FIG. 13 is a flow diagram of a method according to one embodiment of the invention.
DETAILED DESCRIPTION
By way of introduction, the present specification begins with review of techniques for embedding watermark data in line art, as disclosed in my U.S. Pat. No. 6,449,377.
Referring to FIG. 2 , the earlier-described technique employs a grid 10 of imaginary reference points arrayed over a line art image. The spacing between points is 250 microns in the illustrated arrangement, but greater or lesser spacings can of course be used.
Associated with each grid point is a surrounding region 12 , shown in FIG. 3 . As described below, the luminosity (or reflectance) of each of these regions 12 is slightly changed to effect subliminal encoding of binary data.
Region 12 can take various shapes; the illustrated rounded-rectangular shape is representative only. (The illustrated shape has the advantage of encompassing a fairly large area while introducing fewer visual artifacts than, e.g., square regions.) In other embodiments, squares, rectangles, circles, ellipses, etc., can alternatively be employed.
FIG. 4 is a magnified view of an excerpt of FIG. 3 , showing a line 14 passing through the grid of points. The width of the line, of course, depends on the particular image of which it is a part. The illustrated line is about 40 microns in width; greater or lesser widths can naturally be used.
In one encoding technique, shown in FIG. 5 , the width of the line is controllably varied so as to change the luminosity of the regions through which it passes. To increase the luminosity (or reflectance), the line is made narrower (i.e. less ink in the region). To decrease the luminosity, the line is made wider (i.e. more ink).
Whether the luminance in a given region should be increased or decreased depends on the particular watermarking algorithm used. Any algorithm can be used, by changing the luminosity of regions 12 as the algorithm would otherwise change the luminance or colors of pixels in a pixelated image. (Some watermarking algorithms effect their changes in a transformed domain, such as DCT, wavelet, or Fourier. However, such changes are ultimately manifested as changes in luminance or color.)
In an exemplary algorithm, the binary data is represented as a sequence of −1s and 1s, instead of 0s and 1s. (The binary data can comprise a single datum, but more typically comprises several. In an illustrative embodiment, the data comprises 128 bits, some of which are error-correcting or -detecting bits.)
Each element of the binary data sequence is then multiplied by a corresponding element of a pseudo-random number sequence, comprised of −1s and 1s, to yield an intermediate data signal. Each element of this intermediate data signal is mapped to a corresponding sub-part of the image, such as a region 12 . (Commonly, each element is mapped to several such sub-parts.) The image in (and optionally around) this region is analyzed to determine its relative capability to conceal embedded data, and a corresponding scale factor is produced. Exemplary scale factors may range from 0 to 3. The scale factor for the region is then multiplied by the element of the intermediate data signal mapped to the region in order to yield a “tweak” or “bias” value for the region. In the illustrated case, the resulting tweaks can range from −3 to 3. The luminosity of the region is then adjusted in accordance with the tweak value. A tweak value of −3 may correspond to a −5% change in luminosity; −2 may correspond to −2% change; −1 may correspond to −1% change; 0 may correspond to no change; 1 may correspond to +1% change; 2 may correspond to +2% change, and 3 may correspond to +5% change. (This example follows the basic techniques described in the Real Time Encoder embodiment disclosed in U.S. Pat. No. 5,710,834.)
In FIG. 5 , the watermarking algorithm determined that the luminance of region A should be reduced by a certain percentage, while the luminance of regions C and D should be increased by certain percentages.
In region A, the luminance is reduced by increasing the line width. In region D, the luminance is increased by reducing the line width; similarly in region C (but to a lesser extent).
No line passes through region B, so there is no opportunity to change the region's luminance. This is not fatal to the method, however, since the exemplary watermarking algorithm redundantly encodes each bit of data in sub-parts spaced throughout the line art image.
The changes to line widths in regions A and D of FIG. 5 are exaggerated for purposes of illustration. While the illustrated variance is possible, most implementations will typically modulate the line width 3-50% (increase or decrease).
(Many watermarking algorithms routinely operate within a signal margin of about +/−1% changes in luminosity to effect encoding. That is, the “noise” added by the encoding amounts to just 1% or so of the underlying signal. Lines typically don't occupy the full area of a region, so a 10% change to line width may only effect a 1% change to region luminosity, etc. Security documents are different from photographs in that the artwork generally need not convey photorealism. Thus, security documents can be encoded with higher energy than is used in watermarking photographs, provided the result is still aesthetically satisfactory. To illustrate, localized luminance changes on the order of 10% are possible in security documents, while such a level of watermark energy in photographs would generally be considered unacceptable. In some contexts, localized luminance changes of 20, 30, 50 or even 100% are acceptable.)
In the illustrated technique, the change to line width is a function solely of the watermark tweak (or watermark/calibration pattern tweak, as discussed below) to be applied to a single region. Thus, if a line passes through any part of a region to which a tweak of 2% is to be applied, the line width in that region is changed to effect the 2% luminance difference. In variant techniques, the change in line width is a function of the line's position in the region. In particular, the change in line width is a function of the distance between the region's center grid point and the line's closest approach to that point. If the line passes through the grid point, the full 2% change is effected. At successively greater distances, successively smaller changes are applied. The manner in which the magnitude of the tweak changes as a function of line position within the region can be determined by applying one of various interpolation algorithms, such as the bi-linear, bi-cubic, cubic splines, custom curve, etc.
In other variant techniques, the change in line width in a given region is a weighted function of the tweaks for adjoining or surrounding regions. Thus, the line width in one region may be increased or decreased in accordance with a tweak value corresponding to one or more adjoining regions.
Combinations of the foregoing techniques can also be employed.
In the foregoing techniques, it is sometimes necessary to trade-off the tweak values of adjoining regions. For example, a line may pass along a border between regions, or pass through the point equidistant from four grid points (“equidistant zones”). In such cases, the line may be subject to conflicting tweak values—one region may want to increase the line width, while another may want to decrease the line width. (Or both may want to increase the line width, but differing amounts.) Similarly in cases where the line does not pass through an equidistant zone, but the change in line width is a function of a neighborhood of regions whose tweaks are of different values. Again, known interpolation functions can be employed to determine the weight to be given the tweak from each region in determining what change is to be made to the line width in any given region.
In the exemplary watermarking algorithm, the average change in luminosity across the security document image is zero, so no generalized lightening or darkening of the image is apparent. The localized changes in luminosity are so minute in magnitude, and localized in position, that they are essentially invisible (e.g. inconspicuous/subliminal) to human viewers.
An alternative technique is shown in FIG. 6 , in which line position is changed rather than line width.
In FIG. 6 the original position of the line is shown in dashed form, and the changed position of the line is shown in solid form. To decrease a region's luminosity, the line is moved slightly closer to the center of the grid point; to increase a region's luminosity, the line is moved slightly away. Thus, in region A, the line is moved towards the center grid point, while in region D it is moved away.
It will be noted that the line on the left edge of region A does not return to its nominal (dashed) position as it exits the region. This is because the region to the left of region A also is to have decreased luminosity. Where possible, it is generally preferable not to return a line to its nominal position, but instead to permit shifted lines to remain shifted as they enter adjoining regions. So doing permits a greater net line movement within a region, increasing the embedded signal level.
Again, the line shifts in FIG. 6 are somewhat exaggerated. More typical line shifts are on the order of 3-50 microns.
One way to think of the FIG. 6 technique is to employ a magnetism analogy. The grid point in the center of each region can be thought of as a magnet. It either attracts or repels lines. A tweak value of −3, for example, may correspond to a strong-valued attraction force; a tweak value of +2 may correspond to a middle-valued repulsion force, etc. In FIG. 6 , the grid point in region A exhibits an attraction force (i.e. a negative tweak value), and the grid point in region D exhibits a repulsion force (e.g. a positive tweak value).
The magnetic analogy is useful because the magnetic effect exerted on a line depends on the distance between the line and the grid point. Thus, a line passing near a grid point is shifted more in position than a line near the periphery of the region.
(Actually, the magnetism analogy can serve as more than a conceptual tool. Instead, magnetic effects can be modeled in a computer program and serve to synthesize a desired placement of the lines relative to the grid points. Arbitrarily customized magnetic fields can be used.)
Each of the variants applicable to FIG. 5 is likewise applicable to FIG. 6 .
Combinations of the embodiments of FIGS. 5 and 6 can of course be used, resulting in increased watermark energy, better signal-to-noise ratio and, in many cases, less noticeable changes.
In still a further technique, the luminance in each region is changed while leaving the line unchanged. This can be effected by sprinkling tiny dots of ink in the otherwise-vacant parts of the region. In high quality printing, of the type used with security documents, droplets on the order of 3 microns in diameter can be deposited. (Still larger droplets are still beyond the perception threshold for most viewers.) Speckling a region with such droplets (either in a regular array, or random, or according to a desired profile such as Gaussian), can readily effect a 1% or so change in luminosity. (Usually dark droplets are added to a region, effecting a decrease in luminosity. Increases in luminosity can be effected by speckling with a light colored ink, or by forming light voids in line art otherwise present in a region.) (Actually, production realities often mean that many such microdots will not print, but statistically some will.)
In a variant of the speckling technique, very thin mesh lines can be inserted in the artwork—again to slightly change the luminance of one or more regions (so-called “background tinting”).
The following portion of the specification reviews a calibration, or synchronization pattern used in an illustrative security document to facilitate proper registration of the watermark data for decoding. It may be helpful to begin by reviewing further details about the illustrative watermarking method.
Referring to FIG. 7A , an exemplary watermark is divided into “cells” that are 250 microns on a side, each conveying a single bit of information. The cells are grouped into a “block” having 128 cells on a side (i.e. 16,384 cells per block). The blocks are tiled across the region being watermarked (e.g. across the face of a security document).
As noted, the watermark payload consists of 128 bits of data. Each bit is represented by 128 different cells within each block. (The mapping of bits to cells can be pseudo-random, sequential, or otherwise.) The 128“0”s and “1”s of the watermark data are randomized into substantially equal-probability “1”s and “−1”s by a pseudo-random function to reduce watermark visibility. Where a cell has a value of “1,” the luminance of the corresponding area of the image is slightly increased; where a cell has a value of “−1,” the luminance of the corresponding area of the image is slightly decreased (or vice versa). In some embodiments, the localized changes to image luminance due to the +1/−1 watermark cell values are scaled in accordance with data-hiding attributes of the local area (e.g. to a range of +/−4 digital numbers) to increase the robustness of the watermark without compromising its imperceptibility.
It should be noted that a single watermark “cell” commonly encompasses a large number of ink droplets. In high resolution printing, as is commonly used in security documents (e.g. 5000 microdroplets per inch), a single watermark cell may encompass a region of 50 droplets by 50 droplets. In other embodiments, a cell may encompass greater or lesser numbers of droplets.
Decoding a watermark requires precise re-registration of the scanned document image, so the watermark cells are located where expected. To facilitate such registration, a calibration signal can be employed.
An exemplary calibration signal is a geometrical pattern having a known Fourier-Mellin transform. As described in U.S. Pat. No. 5,862,260, when a known pattern is transformed into the Fourier domain, and then further transformed into the Fourier-Mellin domain, the transformed data indicates the scale and rotation of the pattern. If this pattern is replicated on a security document that is thereafter scanned (as noted, scanning commonly introduces rotation, and sometimes scaling), the F-M transform data indicates the scale and rotation of the scanned data, facilitating virtual re-registration of the security document image for watermark detection.
As shown in FIG. 7B , an illustrative geometrical calibration pattern is a block, 3.2 cm on a side. The block comprises a 16×16 array of substantially identical tiles, each 2 mm on a side. Each tile, in term, comprises an 8×8 array of component cells.
As described below, the geometrical calibration pattern in the illustrated embodiment is a visible design feature on the security document. Accordingly, unlike the watermark data, the calibration pattern does not have to be limited to a small range of digital numbers in order to keep it substantially hidden among other features of the document. Also unlike the watermark data, the illustrated calibration pattern is not locally scaled in accordance with data hiding attributes of the security document image.
It is possible to print rectangular grids of grey-scaled ink on a document to serve as a calibration pattern. However, aesthetic considerations usually discourage doing so. Preferable is to realize the calibration pattern in a more traditional art form, such as a seemingly random series of intertwining lines, forming a weave-like pattern that is printed across part or all of the document.
To create this weave-like calibration pattern, a designer first defines an 8×8 cell reference calibration tile. Each cell in the tile is assigned a grey-scale value. In the illustrated embodiment, values within 2-10 percent of each other are used, although this is not essential. An exemplary reference calibration tile is shown in FIG. 8 (assuming 8-bit quantization).
The Fourier-Mellin transform of a block derived from this reference calibration tile will serve as the key by which the scale and rotation of a scanned security document image are determined.
There is some optimization that may be done in selecting/designing the pattern of grey-scale values that define the reference calibration tile. The pattern should have a F-M transform that is readily distinguished from those of other design and watermark elements on the security document. One design procedure effects a trial F-M transform of the rest of the security document design, and works backwards from this data to select a reference calibration tile that is readily distinguishable.
Once a reference tile pattern is selected, the next steps iteratively define a tile having a weave-like pattern whose local luminance values approximately match the reference tile's grey-scale pattern.
Referring to FIG. 9A , the first such step is to select points on the bottom and left side edges of the tile where lines are to cross the tile boundaries. The angles at which the lines cross these boundaries are also selected. (In the illustrated embodiment, these points and angles are selected arbitrarily, although in other embodiments, the choices can be made in conformance with an optimizing design procedure.)
The selected points and angles are then replicated on the corresponding right and top edges of the tile. By this arrangement, lines exiting the top of one tile seamlessly enter the bottom of the adjoining tile at the same angle. Likewise, lines exiting either side of a tile seamlessly join with lines in the laterally adjoining blocks.
The designer next establishes trial line paths snaking through the tile ( FIGS. 9B , 9 C), linking arbitrarily matched pairs of points on the tile's edges. (These snaking paths are sometimes termed “worms.”) Desirably, these paths pass through each of the 64 component cells forming the tile, with the total path length through each cell being within +/−30% of the average path length through all cells. (This trial routing can be performed with pencil and paper, but more commonly is done on a computer graphics station, with a mouse, light pen, or other input device being manipulated by the designer to establish the routing.) In the illustrated embodiment, the lines have a width of about 30-100 microns, and an average spacing between lines of about 100-400 microns, although these parameters are not critical.
Turning next to FIG. 10 , the trial tile is assembled with like tiles to form a 16×16 trial block (3.2 cm on a side), with a repetitive weave pattern formed by replication of the line pattern defined on the 8×8 cell trial tile. This trial block is then converted into grey-scale values. The conversion can be done by scanning a printed representation of the trial block, or by computer analysis of the line lengths and positions. The output is a 128×128 array of grey-scale values, each value corresponding to the luminance of a 250 micron cell within the trial block.
This grey-scale data is compared with grey-scale data provided by assembling 256 of the reference calibration tiles (each an 8×8 array of cells) into a 16×16 calibration pattern block. In particular, the grey-scale array resulting from the trial block is subtracted from the grey-scale array resulting from the reference block, generating a 128×128 array of error values. This error data is used to tweak the arrangement of lines in the trial block.
In cells of the trial calibration block where the error value is positive, the line is too long. That is, the pattern is too dark in those cells (i.e. it has a low luminance grey-scale value), due to a surplus of line length (i.e. too much ink). By shortening the line length in those cells, their luminance is increased (i.e. the cell is lightened). Shortening can be effected by straightening curved arcs, or by relocating a line's entrance and exit points in a cell so less distance is traversed through the cell.
Conversely, in cells where the error value is negative, the line is too short. By increasing the line length in such cells, their luminance is decreased (i.e. the cell is darkened). Increasing the line length through a cell can be accomplished by increasing the curvature of the line in the cell, or by relocating a line's entrance and exit points along the boundary of the cell, so more distance is traversed through the cell.
A computer program is desirably employed to effect the foregoing changes in line routing to achieve the desired darkening or lightening of each cell.
After line positions in the trial calibration block have been tweaked in this fashion, the trial block is again converted to grey-scale values, and again subtracted from the reference block. Again, an array of error values is produced. The positions of the lines are then further tweaked in accordance with the error values.
The foregoing steps of tweaking line routes in accordance with error signals, converting anew into grey-scale, and computing new error values, is repeated until the luminance of the resulting weave pattern in the trial block is arbitrarily close to the luminance of the reference block. Four of five iterations of this procedure commonly suffice to converge on a final calibration block.
(It will be noted that the initial tile pattern created by the designer is done at the tile level—8×8 cells. After the initial trial tile is created, subsequent processing proceeds at the block level (128×128 cells). A common result of the iterative design procedure is that the component tiles lose their uniformity. That is, the pattern of lines in a tile at a corner of the final calibration block will generally be slightly different than the pattern of lines in a tile near the center of the block.)
After the final calibration block pattern has been established as above, the blocks are tiled repetitively over some or all of the security document, and can serve either as a background design element, or as a more apparent element of the design. By printing this weave pattern in an ink color close to the paper substrate color, the patterning is highly unobtrusive. (If a highly contrasting ink color is used, and if the pattern extends over most or all of the security document, it may be desirable to employ a brighter luminance paper than otherwise, since the weave pattern effectively darkens the substrate.)
As noted in my U.S. Pat. No. 5,862,260, the Fourier-Mellin transform has the property that the same output pattern is produced, regardless of rotation or scaling of the input image. The invariant output pattern is shifted in one dimension proportional to image rotation, and shifted in another dimension proportional to image scaling. When an image whose F-M transform is known, is thereafter rotated and/or scaled, the degree of rotation and scaling can be determined by observing the degree of shift of the transformed F-M pattern in the two dimensions. Once the rotation and scale are known, reciprocal processing of the image can be performed to restore the image to its original orientation and scale.
In the above-described embodiment, the calibration block pattern has a known F-M transform. When a security document incorporating such a pattern is scanned (e.g. by a photocopier, a flatbed scanner, a facsimile machine, etc.), the resulting data can be F-M transformed. The known F-M pattern is then identified in the transformed data, and its two-dimensional shift indicates the scale and rotation corruption of the scanned security document data. With these parameters known, misregistration of the security document—including scale and rotation corruption—can be backed-off, and the security document data restored to proper alignment and scale. In this re-registered state, the watermark can be detected. (In alternative embodiments, the original scan data is not processed to remove the scale/rotation effects. Instead, subsequent processing proceeds with the data in its corrupted state, and takes into account the specific corruption factor(s) to nonetheless yield accurate decoding, etc.)
The just-described calibration pattern and design procedure, of course, are just exemplary, and are subject to numerous modifications. The dimensions can be varied at will. It is not essential that the cell size of the calibration tiles match that of the watermark. Nor do the cells sizes need to be integrally related to each other. Nor does the calibration pattern need to be implemented as lines; other ink patterns can alternatively be used to approximate the grey-scale reference pattern
There is no requirement that the lines snake continuously through the tiles. A line can connect to just a single edge point of a tile, resulting in a line that crosses that tile boundary, but no other. Or a line can both begin and end in a single tile, and not connect to any other.
While darker lines on a lighter background are illustrated, lighter lines on a darker background can alternatively be employed.
The iterative design procedure can employ the F-M transform (or other transform). For example, the trial block pattern can be transformed to the F-M domain, and there compared with the F-M transform of the reference block. An F-M domain error signal can thus be obtained, and the routing of the lines can be changed in accordance therewith.
Although the illustrated embodiment tweaked the cell-based grey-scales of the calibration block by changing line curvature and position, other luminance changing techniques can be employed. For example, the width of the weave lines can be locally changed, or small ink dots can be introduced into certain cell areas.
The foregoing (and following) discussions contemplate that the watermark and/or calibration pattern is printed at the same time as (indeed, sometimes as part of) the line art on the security document. In many applications it is desirable to provide the calibration pattern on the security document substrate prior to printing. The markings can be ink applied by the manufacturer, or can be embossings applied, e.g., by rollers in the paper-making process. (Such textural marking is discussed further below.) Or, the markings can be applied by the security document printer, as a preliminary printing operation, such as by offset printing. By using an ink color/density that is already closely matched to the underlying tint of the paper stock, the manufacturer of the paper can introduce less tinting during its manufacture. Such tinting will effectively be replaced by the preliminary printing of the watermark/calibration pattern on the blank paper.
Calibration signals entirely different than those detailed above can also be used. Calibration signals that are optimized to detect rotation, but not scaling, can be employed when scaling is not a serious concern. DCT and Fourier transforms provide data that is readily analyzed to determine rotation. A calibration signal can be tailored to stand out in a typically low-energy portion of the transformed spectrum (e.g. a series of fine lines at an inclined angle transforms to a usually vacant region in DCT space), and the scanned image can be transformed to the DCT/Fourier domains to examine any shift in the calibration signal (e.g. a shift in the spatial frequency representation of the inclined lines).
In some security documents, the just-described calibration weave is printed independently of the watermark encoding. In other embodiments, the weave serves as the lines whose widths, locations, etc., are modulated by the watermark data, as detailed herein and in U.S. Pat. No. 6,449,377.
In an illustrative embodiment, the printing of the security document is achieved by intaglio printing. Intaglio is a well known printing process employing a metal plate into which the security document pattern is etched or engraved. Ink is applied to the plate, filling the etched recesses/grooves. Paper is then pressed into the plate at a very high pressure (e.g. 10-20 tons), both raised-inking and slightly deforming (texturing) the paper.
Although ink is commonly used in the intaglio process, it need not be in certain embodiments of the present invention. Instead, the paper texturing provided by the intaglio pressing—alone—can suffice to convey watermark data. (Texturing of a medium to convey watermark information is disclosed in various of my prior applications, including U.S. Pat. No. 5,850,481.)
To illustrate, an intaglio plate was engraved (using a numerically controlled engraving apparatus), to a depth of slightly less than 1 mm, in accordance with a 3.2×3.2 cm. noise-like block of watermark data. The watermark data was generated as described above (e.g. 128 bits of data, randomly distributed in a 128×128 cell array), and summed with a correspondingly-sized block of calibration data (implemented as discrete grey-scaled cells, rather than the line/weave pattern detailed above). In this embodiment, the data was not kept within a small range of digital numbers, but instead was railed to a full 8-bit dynamic range.)
This textured paper was placed—textured extrema down—on the platen of an conventional flatbed scanner (of the sort commonly sold as an accessory for personal computers), and scanned. The resulting image data was input to Adobe's Photoshop image processing software, version 4.0, which includes Digimarc watermark reader software. The software readily detected the watermark from the textured paper, even when the paper was skewed on the scanner platen.
The optical detection process by which a seemingly blank piece of paper can reliably convey 128 bits of data through an inexpensive scanner has not been analyzed in detail; the degree of localized reflection from the paper may be a function of whether the illuminated region is concave or convex in shape. Regardless of the explanation, it is a remarkable phenomenon to witness.
Experiments have also been conducted using traditional opaque inks. Again, the watermark can reliably be read.
In addition to the just-described technique for “reading” intaglio markings by a conventional scanner, a variant technique is disclosed in Van Renesse, Optical Inspection Techniques for Security Instrumentation, SPIE Proc. Vol. 2659, pp. 159-167 (1996), and can alternatively be used in embodiments according to the present invention.
Although intaglio is a preferred technique for printing security documents, it is not the only such technique. Other familiar techniques by which watermarks and calibration patterns can be printed include offset litho and letterpress, as well as inkjet printing, xerographic printing, etc. And, as noted, textured watermarking can be effected as part of the paper-making process, e.g. by high pressure textured rollers.
In still other embodiments, the watermark and/or calibration (“information”) patterns are not printed on the security document substrate, but rather are formed on or in an auxiliary layer that is laminated with a base substrate. If a generally clear laminate is used, the information patterns can be realized with opaque inks, supplementing the design on the underlying substrate. Or the added information can be encoded in textural form. Combinations of the foregoing can similarly be used.
To retrofit existing security document designs with information patterns, the existing artwork must be modified to effect the necessary additions and/or tweaks to localized security document luminance and/or texture.
When designing new security documents, it would be advantageous to facilitate integration of information patterns into the basic design. One such arrangement is detailed in the following discussion.
Many security documents are still designed largely by hand. A designer works at a drafting table or computer workstation, and spends many hours laying-out minute (e.g. 5 mm×5 mm) excerpts of the design. To aid integration of watermark and/or calibration pattern data in this process, an accessory layout grid can be provided, identifying the watermark “bias” (e.g. −3 to +3) that is to be included in each 250 micron cell of the security document. If the accessory grid indicates that the luminance should be slightly increased in a cell (e.g. 1%), the designer can take this bias in mind when defining the composition of the cell and include a touch less ink than might otherwise be included. Similarly, if the accessory grid indicates that the luminance should be somewhat strongly increased in a cell (e.g. 5%), the designer can again bear this in mind and try to include more ink than might otherwise be included. Due to the substantial redundancy of most watermark encoding techniques, strict compliance by the designer to these guidelines is not required. Even loose compliance can result in artwork that requires little, if any, further modification to reliably convey watermark and/or calibration information.
Such “designing-in” of embedded information in security documents is facilitated by the number of arbitrary design choices made by security document designers. A few examples from U.S. banknotes include the curls in the presidents' hair, the drape of clothing, the clouds in the skies, the shrubbery in the landscaping, the bricks in the pyramid, the fill patterns in the lettering, and the great number of arbitrary guilloche patterns and other fanciful designs, etc. All include curves, folds, wrinkles, shadow effects, etc., about which the designer has wide discretion in selecting local luminance, etc. Instead of making such choices arbitrarily, the designer can make these choices deliberately so as to serve an informational—as well as an aesthetic—function.
To further aid the security document designer, data defining several different information-carrying patterns (both watermark and/or calibration pattern) can be stored on mass storage of a computer workstation and serve as a library of design elements for future designs. The same user-interface techniques that are employed to pick colors in image-editing software (e.g. Adobe Photoshop) and fill textures in presentation programs (e.g. Microsoft PowerPoint) can similarly be used to present a palette of information patterns to a security document designer. Clicking on a visual representation of the desired pattern makes the pattern available for inclusion in a security document being designed (e.g. filling a desired area).
In the embodiment earlier-described, the calibration pattern is printed as a visible artistic element of the security document. However, the same calibration effect can be provided subliminally if desired. That is, instead of generating artwork mimicking the grey-scale pattern of the reference calibration block, the reference calibration block can itself be encoded into the security document as small changes in local luminance. In many such embodiments, the bias to localized document luminance due to the calibration pattern is simply added to the bias due to the watermark data, and encoded like the watermark data (e.g. as localized changes to the width or position of component line-art lines, as inserted ink droplets, etc.).
The uses to which the 128 bits of watermark data can be put in security documents are myriad. Many are detailed in the materials cited above. Examples include postal stamps encoded with their value, or with the zip code of the destination to which they are addressed (or from which they were sent); banknotes encoded with their denomination, and their date and place of issuance; identification documents encoded with authentication information by which a person's identify can be verified; etc., etc.
The encoded data can be in a raw form—available to any reader having the requisite key data (in watermarking techniques where a key data is used), or can be encrypted, such as with public key encryption techniques, etc. The encoded data can embody information directly, or can be a pointer or an index to a further collection of data in which the ultimate information desired is stored.
For example, watermark data in a passport need not encode a complete dossier of information on the passport owner. Instead, the encoded data can include key data (e.g. a social security number) identifying a particular record in a remote database in which biographical data pertaining to the passport owner is stored. A passport processing station employing such an arrangement is shown in FIG. 11 .
To decode watermark data, the security document must be converted into electronic image data for analysis. This conversion is typically performed by a scanner.
Scanners are well known, so a detailed description is not provided here. Suffice it to say that scanners conventionally employ a line of closely spaced photodetector cells that produce signals related to the amount of the light reflected from successive swaths of the document. Most inexpensive consumer scanners have a resolution of 300 dots per inch (dpi), or a center to center spacing of component photodetectors of about 84 microns. Higher quality scanners of the sort found in most professional imaging equipment and photocopiers have resolutions of 600 dpi (42 microns), 1200 dpi (21 microns), or better.
Taking the example of a 300 dpi scanner (84 micron photodetector spacing), each 250 micron region 12 on the security document will correspond to about a 3×3 array of photodetector samples. Naturally, only in rare instances will a given region be physically registered with the scanner so that nine photodetector samples capture the luminance in that region, and nothing else. More commonly, the image is rotated with respect to the scanner photodetectors, or is longitudinally misaligned (i.e. some photodetectors image sub-parts of two adjoining regions). However, since the scanner oversamples the regions, the luminance of each region can unambiguously be determined.
In one embodiment, the scanned data from the document is collected in a two dimensional array of data and processed to detect the embedded calibration information. The scanner data is then processed to effect a virtual re-registration of the document image. A software program next analyzes the statistics of the re-registered data (using the techniques disclosed in my prior writings) to extract the bits of the embedded data.
(Again, the reference to my earlier watermark decoding techniques is exemplary only. Once scanning begins and the data is available in sampled form, it is straightforward to apply any other watermark decoding technique to extract a correspondingly-encoded watermark. Some of these other techniques employ domain transformations (e.g. to wavelet, DCT, or Fourier domains, as part of the decoding process).)
In a variant embodiment, the scanned data is not assembled in a complete array prior to processing. Instead, it is processed in real-time, as it is generated, in order to detect embedded watermark data without delay. (Depending on the parameters of the scanner, it may be necessary to scan a half-inch or so of the document before the statistics of the resulting data unambiguously indicate the presence of a watermark.)
In other embodiments, hardware devices are provided with the capability to recognize embedded watermark data in any document images they process, and to respond accordingly.
One example is a color photocopier. Such devices employ a color scanner to generate sampled (pixel) data corresponding to an input media (e.g. a dollar bill). If watermark data associated with a security document is detected, the photocopier can take one or more steps.
One option is simply to interrupt copying, and display a message reminding the operator that it is illegal to reproduce currency.
Another option is to dial a remote service and report the attempted banknote reproduction. Photocopiers with dial-out capabilities are known in the art (e.g. U.S. Pat. No. 5,305,199) and are readily adapted to this purpose. The remote service can be an independent service, or can be a government agency.
Yet another option is to permit the copying, but to insert forensic tracer data in the resultant copy. This tracer data can take various forms. Steganographically encoded binary data is one example. An example is shown in U.S. Pat. No. 5,568,268. The tracer data can memorialize the serial number of the machine that made the copy and/or the date and time the copy was made. To address privacy concerns, such tracer data is not normally inserted in all photocopied output, but is inserted only when the subject being photocopied is detected as being a security document. (An example of such an arrangement is shown in FIG. 12 .)
Desirably, the scan data is analyzed on a line-by-line basis in order to identify illicit photocopying with a minimum of delay. If a security document is scanned, one or more lines of scanner output data may be provided to the photocopier's reprographic unit before the recognition decision has been made. In this case the photocopy will have two regions: a first region that is not tracer-marked, and a second, subsequent region in which the tracer data has been inserted.
Photocopiers with other means to detect not-to-be-copied documents are known in the art, and employ various response strategies. Examples are detailed in U.S. Pat. Nos. 5,583,614, 4,723,149, 5,633,952, 5,640,467, and 5,424,807.
Another hardware device that can employ the foregoing principles is a standalone scanner. A programmed processor (or dedicated hardware) inside the scanner analyzes the data being generated by the device, and responds accordingly.
Yet another hardware device that can employ the foregoing principles is a printer. A processor inside the device analyzes graphical image data to be printed, looking for watermarks associated with security documents.
For both the scanner and printer devices, response strategies can include disabling operation, or inserting tracer information. (Such devices typically do not have dial-out capabilities.)
Again, it is desirable to process the scanner or printer data as it becomes available, so as to detect any security document processing with a minimum of delay. Again, there will be some lag time before a detection decision is made. Accordingly, the scanner or printer output will be comprised of two parts, one without the tracer data, and another with the tracer data.
Many security documents already include visible structures that can be used as aids in banknote detection (e.g. the seal of the issuer, and various geometrical markings on U.S. currency). In accordance with a further aspect of the present invention, a security document is analyzed by an integrated system that considers both the visible structures and watermark-embedded data.
Visible security document structures can be sensed using known pattern recognition techniques. Examples of such techniques are disclosed in U.S. Pat. Nos. 5,321,773, 5,390,259, 5,533,144, 5,539,841, 5,583,614, 5,633,952, 4,723,149, 5,692,073, and 5,424,807 and laid-open foreign applications EP 649,114 and EP 766,449.
In photocopiers (and the like) equipped to detect both visible structures and watermarks from security documents, the detection of either can cause one or more of the above-noted responses to be initiated ( FIG. 12 ).
Again, scanners and printers can be equipped with a similar capability—analyzing the data for either of these security document hallmarks. If either is detected, the software (or hardware) responds accordingly.
Identification of security documents by watermark data provides an important advantage over recognition by visible structures—it cannot so easily be defeated. A security document can be doctored (e.g. by white-out, scissors, or less crude techniques) to remove/obliterate the visible structures. Such a document can then be freely copied on either a visible structure-sensing photocopier or scanner/printer installation. The removed visible structure can then be added back in via a second printing/photocopying operation. If the printer is not equipped with security document-disabling capabilities, image-editing tools can be used to insert visible structures back into image data sets scanned from such doctored documents, and the complete document can then be freely printed. By additionally including embedded watermark data in the security document, and sensing same, such ruses will not succeed.
(A similar ruse is to scan a security document image on a non-security document-sensing scanner. The resulting image set can then be edited by conventional image editing tools to remove/obliterate the visible structures. Such a data set can then be printed—even on a printer/photocopier that examines such data for the presence of visible structures. Again, the missing visible structures can be inserted by a subsequent printing/photocopying operation.)
Desirably, the visible structure detector and the watermark detector are integrated together as a single hardware and/or software tool. This arrangement provides various economies, e.g., in interfacing with the scanner, manipulating pixel data sets for pattern recognition and watermark extraction, electronically re-registering the image to facilitate pattern recognition/watermark extraction, issuing control signals (e.g. disabling) signals to the photocopier/scanner, etc.
While the foregoing apparatuses are particularly concerned with counterfeit deterrence, the embedded markings can also serve other functions. Examples include banknote processing machines that perform denomination sorting, counterfeit detection, and circulation analysis functions. (I.e., banknotes with certain markings may be distributed through known sources, and their circulation/distribution can subsequently be monitored to assist in macro-economic analyses.)
From the foregoing, it will be recognized that various embodiments according to the present invention provide techniques for embedding multi-bit binary data in security documents, and provide for the reliable extraction of such data even in the presence of various forms of corruption (e.g. scale and rotation).
(To provide a comprehensive disclosure without unduly lengthening the following specification, applicant incorporates by reference the patents and applications cited above.)
Having described and illustrated the principles of my invention with reference to several illustrative embodiments, it will be recognized that these embodiments are exemplary only and should not be taken as limiting the scope of my invention. Guided by the foregoing teachings, it should be apparent that other watermarking, decoding, and anti-counterfeiting technologies can be substituted for, and/or combined with, the elements detailed above to yield advantageous effects. Other features disclosed in my earlier applications can similarly be employed in embodiments of the technology detailed herein. (Thus, I have not here belabored application of each of the techniques disclosed in my earlier applications—e.g. use of neural networks for watermark detectors—to the present subject matter since same is fairly taught by reading the present disclosure in the context of my earlier work.)
While the technology has been described with reference to embodiments employing regular rectangular arrays of cells, those skilled in the art will recognize that other arrays—neither rectangular nor regular—can alternatively be used.
While the embodiments have described the calibration patterns as adjuncts to digital watermarks—facilitating their detection, such patterns have utility apart from digital watermarks. One example is in re-registering scanned security document image data to facilitate detection of visible structures (e.g. detection of the seal of the issuer, using known pattern recognition techniques). Indeed, the use of such calibration patterns to register both watermark and visible structure image data for recognition is an important economy that can be gained by integration a visible structure detector and a watermark detector into a single system.
Although security documents have most commonly been printed on paper (e.g. cotton/linen), other substrates are gaining in popularity (e.g. synthetics, such as polymers) and are well (or better) suited for use with the above-described techniques.
The embodiments detailed above can be implemented in dedicated hardware (e.g. ASICs), programmable hardware, and/or software.
In view of the many possible embodiments to which the principles of the above-described technology may be put, it should be recognized that the detailed embodiments are illustrative only and should not be taken as limiting the scope of my invention. Rather, I claim as my invention all such embodiments as may come within the scope and spirit of the following claims and equivalents thereto.
APPENDIX A
Watermarking Methods, Apparatuses, and Applications
(To provide a comprehensive disclosure without unduly lengthening the following specification, applicants incorporate by reference the cited patent documents.)
Watermarking is a quickly growing field of endeavor, with several different approaches. The present assignee's work is reflected in U.S. Pat. Nos. 5,710,834, 5,636,292, 5,721,788, allowed U.S. application Ser. Nos. 08/327,426, 08/598,083, 08/436,134 (to issue as U.S. Pat. No. 5,748,763), Ser. No. 08/436,102 (to issue as U.S. Pat. No. 5,748,783), and 08/614,521 (to issue as U.S. Pat. No. 5,745,604), and laid-open PCT application WO97/43736. Other work is illustrated by U.S. Pat. Nos. 5,734,752, 5,646,997, 5,659,726, 5,664,018, 5,671,277, 5,687,191, 5,687,236, 5,689,587, 5,568,570, 5,572,247, 5,574,962, 5,579,124, 5,581,500, 5,613,004, 5,629,770, 5,461,426, 5,743,631, 5,488,664, 5,530,759, 5,539,735, 4,943,973, 5,337,361, 5,404,160, 5,404,377, 5,315,098, 5,319,735, 5,337,362, 4,972,471, 5,161,210, 5,243,423, 5,091,966, 5,113,437, 4,939,515, 5,374,976, 4,855,827, 4,876,617, 4,939,515, 4,963,998, 4,969,041, and published foreign applications WO 98/02864, EP 822,550, WO 97/39410, WO 96/36163, GB 2,196,167, EP 777,197, EP 736,860, EP 705,025, EP 766,468, EP 782,322, WO 95/20291, WO 96/26494, WO 96/36935, WO 96/42151, WO 97/22206, WO 97/26733. Some of the foregoing patents relate to visible watermarking techniques. Other visible watermarking techniques (e.g. data glyphs) are described in U.S. Pat. Nos. 5,706,364, 5,689,620, 5,684,885, 5,680,223, 5,668,636, 5,640,647, 5,594,809.
Most of the work in watermarking, however, is not in the patent literature but rather in published research. In addition to the patentees of the foregoing patents, some of the other workers in this field (whose watermark-related writings can by found by an author search in the INSPEC database) include I. Pitas, Eckhard Koch, Jian Zhao, Norishige Morimoto, Laurence Boney, Kineo Matsui, A. Z. Tirkel, Fred Mintzer, B. Macq, Ahmed H. Tewfik, Frederic Jordan, Naohisa Komatsu, and Lawrence O'Gorman.
The artisan is assumed to be familiar with the foregoing prior art.
In the following disclosure it should be understood that references to watermarking encompass not only the assignee's watermarking technology, but can likewise be practiced with any other watermarking technology, such as those indicated above.
Watermarking can be applied to myriad forms of information. These include imagery (including video) and audio—whether represented in digital form (e.g. an image comprised of pixels, digital video, etc.), or in an analog representation (e.g. non-sampled music, printed imagery, banknotes, etc.) Watermarking can be applied to digital content (e.g. imagery, audio) either before or after compression. Watermarking can also be used in various “description” or “synthesis” language representations of content, such as Structured Audio, Csound, NetSound, SNHC Audio and the like (c.f. http://sound.media.mit.edu/mpeg4/) by specifying synthesis commands that generate watermark data as well as the intended audio signal. Watermarking can also be applied to ordinary media, whether or not it conveys information. Examples include paper, plastics, laminates, paper/film emulsions, etc. A watermark can embed a single bit of information, or any number of bits.
The physical manifestation of watermarked information most commonly takes the form of altered signal values, such as slightly changed pixel values, picture luminance, picture colors, DCT coefficients, instantaneous audio amplitudes, etc. However, a watermark can also be manifested in other ways, such as changes in the surface microtopology of a medium, localized chemical changes (e.g. in photographic emulsions), localized variations in optical density, localized changes in luminescence, etc. Watermarks can also be optically implemented in holograms and conventional paper watermarks.
One improvement to existing technology is to employ established web crawler services (e.g. AltaVista, Excite, or Inktomi) to search for watermarked content (on the Web, in internet news groups, BBS systems, on-line systems, etc.) in addition to their usual data collecting/indexing operations. Such crawlers can download files that may have embedded watermarks (e.g. *.JPG, *.WAV, etc.) for later analysis. These files can be processed, as described below, in real time. More commonly, such files are queued and processed by a computer distinct from the crawler computer. Instead of performing watermark-read operations on each such file, a screening technique can be employed to identify those most likely to be conveying watermark data. One such technique is to perform a DCT operation on an image, and look for spectral coefficients associated with certain watermarking techniques (e.g. coefficients associated with an inclined embedded subliminal grid). To decode spread-spectrum based watermarks, the analyzing computer requires access to the noise signal used to spread the data signal. In one embodiment, interested parties submit their noise/key signals to the crawler service so as to enable their marked content to be located. The crawler service maintains such information in confidence, and uses different noise signals in decoding an image (image is used herein as a convenient shorthand for imagery, video, and audio) until watermarked data is found (if present). This allows the use of web crawlers to locate content with privately-coded watermarks, instead of just publicly-coded watermarks as is presently the case. The queueing of content data for analysis provides certain opportunities for computational shortcuts. For example, like-sized images (e.g. 256×256 pixels) can be tiled into a larger image, and examined as a unit for the presence of watermark data. If the decoding technique (or the optional pre-screening technique) employs a DCT transform or the like, the block size of the transform can be tailored to correspond to the tile size (or some integral fraction thereof). Blocks indicated as likely having watermarks can then be subjected to a full read operation. If the queued data is sorted by file name, file size, or checksum, duplicate files can be identified. Once such duplicates are identified, the analysis computer need consider only one instance of the file. If watermark data is decoded from such a file, the content provider can be informed of each URL at which copies of the file were found.
Some commentators have observed that web crawler-based searches for watermarked images can be defeated by breaking a watermarked image into sub-blocks (tiles). HTML instructions, or the like, cause the sub-blocks to be presented in tiled fashion, recreating the complete image. However, due to the small size of the component sub-blocks, watermark reading is not reliably accomplished.
This attack is overcome by instructing the web-crawler to collect the display instructions (e.g. HTML) by which image files are positioned for display on a web page, in addition to the image files themselves. Before files collected from a web page are scrutinized for watermarks, they can be concatenated in the arrangement specified by the display instructions. By this arrangement, the tiles are reassembled, and the watermark data can be reliably recovered.
Another such postulated attack against web crawler detection of image watermarks is to scramble the image (and thus the watermark) in a file, and employ a Java applet or the like to unscramble the image prior to viewing. Existing web crawlers inspect the file as they find it, so the watermark is not detected. However, just as the Java descrambling applet can be invoked when a user wishes access to a file, the same applet can similarly be employed in a web crawler to overcome such attempted circumvention of watermark detection.
Although “content” can be located and indexed by various web crawlers, the contents of the “content” are unknown. A *.JPG file, for example, may include pornography, a photo of a sunset, etc.
Watermarks can be used to indelibly associate meta-data within content (as opposed to stored in a data structure that forms another part of the object, as is conventionally done with meta-data). The watermark can include text saying “sunset” or the like. More compact information representations can alternatively be employed (e.g. coded references). Still further, the watermark can include (or consist entirely of) a Unique ID (UID) that serves as an index (key) into a network-connected remote database containing the meta data descriptors. By such arrangements, web crawlers and the like can extract and index the meta-data descriptor tags, allowing searches to be conducted based on semantic descriptions of the file contents, rather than just by file name.
Existing watermarks commonly embed information serving to communicate copyright information. Some systems embed text identifying the copyright holder. Others embed a UID which is used as an index into a database where the name of the copyright owner, and associated information, is stored.
Looking ahead, watermarks should serve more than as silent copyright notices. One option is to use watermarks to embed “intelligence” in content. One form of intelligence is knowing its “home.” “Home” can be the URL of a site with which the content is associated. A photograph of a car, for example, can be watermarked with data identifying the web site of an auto-dealer that published the image. Wherever the image goes, it serves as a link back to the original disseminator. The same technique can be applied to corporate logos. Wherever they are copied on the internet, a suitably-equipped browser or the like can decode the data and link back to the corporation's home page. (Decoding may be effected by positioning the cursor over the logo and pressing the right-mouse button, which opens a window of options—one of which is Decode Watermark.)
To reduce the data load of the watermark, the intelligence need not be wholly encoded in the content's watermark. Instead, the watermark can again provide a UID—this time identifying a remote database record where the URL of the car dealer, etc., can be retrieved. In this manner, images and the like become marketing agents—linking consumers with vendors (with some visual salesmanship thrown in). In contrast to the copyright paradigm, in which dissemination of imagery was an evil sought to be tracked and stopped, dissemination of the imagery can now be treated as a selling opportunity. A watermarked image becomes a portal to a commercial transaction.
(Using an intermediate database between a watermarked content file and its ultimate home (i.e. indirect linking) serves an important advantage: it allows the disseminator to change the “home” simply by updating a record in the database. Thus, for example, if one company is acquired by another, the former company's smart images can be made to point to the new company's home web page by updating a database record. In contrast, if the old company's home URL is hard-coded (i.e. watermarked) in the object, it may point to a URL that eventually is abandoned. In this sense, the intermediate database serves as a switchboard that couples the file to its current home.
The foregoing techniques are not limited to digital content files. The same approach is equally applicable with printed imagery, etc. A printed catalog, for example, can include a picture illustrating a jacket. Embedded in the picture is watermarked data. This data can be extracted by a simple hand-scanner/decoder device using straightforward scanning and decoding techniques (e.g. those known to artisans in those fields). In watermark-reading applications employing hand-scanners and the like, it is important that the watermark decoder be robust to rotation of the image, since the catalog photo will likely be scanned off-axis. One option is to encode subliminal graticules (e.g. visualization synchronization codes) in the catalog photo so that the set of image data can be post-processed to restore it to proper alignment prior to decoding.
The scanner/decoder device can be coupled to a modem-equipped computer, a telephone, or any other communications device. In the former instance, the device provides URL data to the computer's web browser, linking the browser to the catalog vendor's order page. (The device need not include its own watermark decoder; this task can be performed by the computer.) The vendor's order page can detail the size and color options of the jacket, inventory availability, and solicit ordering instructions (credit card number, delivery options, etc.)—as is conventionally done with on-line merchants. Such a device connected to a telephone can dial the catalog vendor's toll-free automated order-taking telephone number (known, e.g., from data encoded in the watermark), and identify the jacket to the order center. Voice prompts can then solicit the customer's choice of size, color, and delivery options, which are input by Touch Tone instructions, or by voiced words (using known voice recognition software at the vendor facility).
In such applications, the watermark may be conceptualized as an invisible bar code employed in a purchase transaction. Here, as elsewhere, the watermark can serve as a seamless interface bridging the print and digital worlds
Another way of providing content with intelligence is to use the watermark to provide Java or ActiveX code. The code can be embedded in the content, or can be stored remotely and linked to the content. When the watermarked object is activated, the code can be executed (either automatically, or at the option of the user). This code can perform virtually any function. One is to “phone home”—initiating a browser and linking to the object's home. The object can then relay any manner of data to its home. This data can specify some attribute of the data, or its use. The code can also prevent accessing the underlying content until permission is received. An example is a digital movie that, when double-clicked, automatically executes a watermark-embedded Java applet which links through a browser to the movie's distributor. The user is then prompted to input a credit card number. After the number has been verified and a charge made, the applet releases the content of the file to the computer's viewer for viewing of the movie. Support for these operations is desirably provided via the computer's operating system, or plug-in software.
Such arrangements can also be used to collect user-provided demographic information when smart image content is accessed by the consumer of the content. The demographic information can be written to a remote database and can be used for market research, customization of information about the content provided to the consumer, sales opportunities, advertising, etc.
In audio and video and the like, watermarks can serve to convey related information, such as links to WWW fan sites, actor biographies, advertising for marketing tie-ins (T-shirts, CDs, concert tickets). In such applications, it is desirable (but not necessary) to display on the user interface (e.g. screen) a small logo to signal the presence of additional information. When the consumer selects the logo via some selection device (mouse, remote control button, etc.), the information is revealed to the consumer, who can then interact with it.
Much has been written (and patented) on the topic of asset rights management. Sample patent documents include U.S. Pat. Nos. 5,715,403, 5,638,443, 5,634,012, 5,629,980. Again, much of the technical work is memorialized in journal articles, which can be identified by searching for relevant company names and trademarks such as IBM's Cryptolope system, Portland Software's ZipLock system, the Rights Exchange service by Softbank Net Solutions, and the DigiBox system from InterTrust Technologies.
An exemplary asset management system makes content available (e.g. from a web server, or on a new computer's hard disk) in encrypted form. Associated with the encrypted content is data identifying the content (e.g. a preview) and data specifying various rights associated with the content. If a user wants to make fuller use of the content, the user provides a charge authorization (e.g. a credit card) to the distributor, who then provides a decryption key, allowing access to the content. (Such systems are often realized using object-based technology. In such systems, the content is commonly said to be distributed in a “secure container.”)
Desirably, the content should be marked (personalized/serialized) so that any illicit use of the content (after decryption) can be tracked. This marking can be performed with watermarking, which assures that the mark travels with the content wherever—and in whatever form—it may go. The watermarking can be effected by the distributor—prior to dissemination of the encrypted object—such as by encoding a UID that is associated in a database with that particular container. When access rights are granted to that container, the database record can be updated to reflect the purchaser, the purchase date, the rights granted, etc. An alternative is to include a watermark encoder in the software tool used to access (e.g. decrypt) the content. Such an encoder can embed watermark data in the content as it is released from the secure container, before it is provided to the user. The embedded data can include a UID, as described above. This UID can be assigned by the distributor prior to disseminating the container. Alternatively, the UID can be a data string not known or created until access rights have been granted. In addition to the UID, the watermark can include other data not known to the distributor, e.g. information specific to the time(s) and manner(s) of accessing the content.
In other systems, access rights systems can be realized with watermarks without containers etc. Full resolution images, for example, can be freely available on the web. If a user wishes to incorporate the imagery into a web page or a magazine, the user can interrogate the imagery as to its terms and conditions of use. This may entail linking to a web site specified by the embedded watermark (directly, or through an intermediate database), which specifies the desired information. The user can then arrange the necessary payment, and use the image knowing that the necessary rights have been secured.
As noted, digital watermarks can also be realized using conventional (e.g. paper) watermarking technologies. Known techniques for watermarking media (e.g. paper, plastic, polymer) are disclosed in U.S. Pat. Nos. 5,536,468, 5,275,870, 4,760,239, 4,256,652, 4,370,200, and 3,985,927 and can be adapted to display of a visual watermark instead of a logo or the like. Note that some forms of traditional watermarks which are designed to be viewed with transmissive light can also show up as low level signals in reflective light, as is typically used in scanners. Transmissive illumination detection systems can also be employed to detect such watermarks, using optoelectronic traditional-watermark detection technologies known in the art.
As also noted, digital watermarks can be realized as part of optical holograms. Known techniques for producing and securely mounting holograms are disclosed in U.S. Pat. Nos. 5,319,475, 5,694,229, 5,492,370, 5,483,363, 5,658,411 and 5,310,222. To watermark a hologram, the watermark can be represented in the image or data model from which the holographic diffraction grating is produced. In one embodiment, the hologram is produced as before, and displays an object or symbol. The watermark markings appear in the background of the image so that they can be detected from all viewing angles. In this context, it is not critical that the watermark representation be essentially imperceptible to the viewer. If desired, a fairly visible noise-like pattern can be used without impairing the use to which the hologram is put.
Digital watermarks can also be employed in conjunction with labels and tags. In addition to conventional label/tag printing processes, other techniques—tailored to security—can also be employed. Known techniques useful in producing security labels/tags are disclosed in U.S. Pat. Nos. 5,665,194, 5,732,979, 5,651,615, and 4,268,983. The imperceptibility of watermarked data, and the ease of machine decoding, are some of the benefits associated with watermarked tags/labels. Additionally, the cost is far less than many related technologies (e.g. holograms). Watermarks in this application can be used to authenticate the originality of a product label, either to the merchant or to the consumer of the associated product, using a simple scanner device, thereby reducing the rate of counterfeit product sales.
Recent advances in color printing technology have greatly increased the level of casual counterfeiting. High quality scanners are now readily available to many computer users, with 300 dpi scanners available for under $100, and 600 dpi scanners available for marginally more. Similarly, photographic quality color ink-jet printers are commonly available from Hewlett-Packard Co., Epson, etc. for under $300.
Watermarks in banknotes and other security documents (passports, stock certificates, checks, etc.—all collectively referred to as banknotes herein) offer great promise to reduce such counterfeiting, as discussed more fully below. Additionally, watermarks provide a high-confidence technique for banknote authentication. One product enabled by this increased confidence is automatic teller machines that accept, as well as dispense, cash. The machine is provided with known optical scanning technology to produce digital data corresponding to the face(s) of the bill. This image set is then analyzed to extract the watermark data. In watermarking technologies that require knowledge of a code signal for decoding (e.g. noise modulation signal, crypto key, spreading signal, etc.), a bill may be watermarked in accordance with several such codes. Some of these codes are public—permitting their reading by conventional machines. Others are private, and are reserved for use by government agencies and the like. (C.f. public and private codes in the present assignee's issued patents.)
Banknotes presently include certain markings which can be used as an aid in note authentication. Well known visible structures are added to banknotes to facilitate visual authentication and machine detection. An example is the seal of the issuing bank. Others are geometrical markings. Desirably, a note is examined by an integrated detection system, for both such visible structures as well as the present watermark-embedded data, to determine authenticity.
The visible structures can be sensed using known pattern recognition techniques. Examples of such techniques are disclosed in U.S. Pat. Nos. 5,321,773, 5,390,259, 5,533,144, 5,539,841, 5,583,614, 5,633,952, 4,723,149 and 5,424,807 and laid-open foreign application EP 766,449. The embedded watermark data can be recovered using the scanning/analysis techniques disclosed in the cited patents and publications.
To reduce counterfeiting, it is desirable that document-reproducing technologies recognize banknotes and refuse to reproduce same. A photocopier, for example, can sense the presence of either a visible structure *or* embedded banknote watermark data, and disable copying if either is present. Scanners and printers can be equipped with a similar capability—analyzing the data scanned or to be printed for either of these banknote hallmarks. If either is detected, the software (or hardware) disables further operation.
The watermark detection criteria provides an important advantage not otherwise available. An original bill can be doctored (e.g. by white-out, scissors, or less crude techniques) to remove/obliterate the visible structures. Such a document can then be freely copied on either a visible structure-sensing photocopier or scanner/printer installation. The removed visible structure can then be added in via a second printing/photocopying operation. If the printer is not equipped with banknote-disabling capabilities, image-editing tools can be used to insert visible structures back into image data sets scanned from such doctored bills, and the complete bill freely printed. By additionally including embedded watermark data in the banknote, and sensing same, such ruses will not succeed.
(A similar ruse is to scan a banknote image on a non-banknote-sensing scanner. The resulting image set can then be edited by conventional image editing tools to remove/obliterate the visible structures. Such a data set can then be printed—even on a printer/photocopier that examines such data for the presence of visible structures. Again, the missing visible structures can be inserted by a subsequent printing/photocopying operation.)
Desirably, the visible structure detector and the watermark detector are integrated together as a single hardware and/or software tool. This arrangement provides various economies, e.g., in interfacing with the scanner, manipulating pixel data sets for pattern recognition and watermark extraction, electronically re-registering the image to facilitate pattern recognition/watermark extraction, issuing control signals (e.g. disabling) signals to the photocopier/scanner, etc.
A related principle is to insert an imperceptible watermark having a UID into all documents printed with a printer, scanned with a scanner, or reproduced by a photocopier. The UID is associated with the particular printer/photocopier/scanner in a registry database maintained by the products' manufacturers. The manufacturer can also enter in this database the name of the distributor to whom the product was initially shipped. Still further, the owner's name and address can be added to the database when the machine is registered for warranty service. While not preventing use of such machines in counterfeiting, the embedded UID facilitates identifying the machine that generated a counterfeit banknote. (This is an application in which a private watermark might best be used.)
While the foregoing applications disabled potential counterfeiting operations upon the detection of *either* a visible structure or watermarked data, in other applications, both criteria must be met before a banknote is recognized as genuine. Such applications typically involve the receipt or acceptance of banknotes, e.g. by ATMs as discussed above.
The foregoing principles (employing just watermark data, or in conjunction with visible indicia) can likewise be used to prevent counterfeiting of tags and labels (e.g. the fake labels and tags commonly used in pirating Levis brand jeans, Microsoft software, etc.)
The reader may first assume that banknote watermarking is effected by slight alterations to the ink color/density/distribution, etc. on the paper. This is one approach. Another is to watermark the underlying medium (whether paper, polymer, etc.) with a watermark. This can be done by changing the microtopology of the medium (a la mini-Braille) to manifest the watermark data. Another option is to employ a laminate on or within the banknote, where the laminate has the watermarking manifested thereon/therein. The laminate can be textured (as above), or its optical transmissivity can vary in accordance with a noise-like pattern that is the watermark, or a chemical property can similarly vary.
Another option is to print at least part of a watermark using photoluminescent ink. This allows, e.g., a merchant presented with a banknote, to quickly verify the presence of *some* watermark-like indicia in/on the bill even without resort to a scanner and computer analysis (e.g. by examining under a black light). Such photoluminescent ink can also print human-readable indicia on the bill, such as the denomination of a banknote. (Since ink-jet printers and other common mass-printing technologies employ cyan/magenta/yellow/black to form colors, they can produce only a limited spectrum of colors. Photoluminescent colors are outside their capabilities. Fluorescent colors—such as the yellow, pink and green dyes used in highlighting markers—can similarly be used and have the advantage of being visible without a black light.)
An improvement to existing encoding techniques is to add an iterative assessment of the robustness of the mark, with a corresponding adjustment in a re-watermarking operation. Especially when encoding multiple bit watermarks, the characteristics of the underlying content may result in some bits being more robustly (e.g. strongly) encoded than others. In an illustrative technique employing this improvement, a watermark is first embedded in an object. Next, a trial decoding operation is performed. A confidence measure (e.g. signal-to-noise ratio) associated with each bit detected in the decoding operation is then assessed. The bits that appear weakly encoded are identified, and corresponding changes are made to the watermarking parameters to bring up the relative strengths of these bits. The object is then watermarked anew, with the changed parameters. This process can be repeated, as needed, until all of the bits comprising the encoded data are approximately equally detectable from the encoded object, or meet some predetermined signal-to-noise ratio threshold.
The foregoing applications, and others, can generally benefit by multiple watermarks. For example, an object (physical or data) can be marked once in the spatial domain, and a second time in the spatial frequency domain. (It should be understood that any change in one domain has repercussions in the other. Here we reference the domain in which the change is directly effected.)
Another option is to mark an object with watermarks of two different levels of robustness, or strength. The more robust watermark withstands various types of corruption, and is detectable in the object even after multiple generations of intervening distortion. The less robust watermark can be made frail enough to fail with the first distortion of the object. In a banknote, for example, the less robust watermark serves as an authentication mark. Any scanning and reprinting operation will cause it to become unreadable. Both the robust and the frail watermarks should be present in an authentic banknote; only the former watermark will be present in a counterfeit.
Still another form of multiple-watermarking is with content that is compressed. The content can be watermarked once (or more) in an uncompressed state. Then, after compression, a further watermark (or watermarks) can be applied.
Still another advantage from multiple watermarks is protection against sleuthing. If one of the watermarks is found and cracked, the other watermark(s) will still be present and serve to identify the object.
The foregoing discussion has addressed various technological fixes to many different problems. Exemplary solutions have been detailed above. Others will be apparent to the artisan by applying common knowledge to extrapolate from the solutions provided above.
For example, the technology and solutions disclosed herein have made use of elements and techniques known from the cited references. Other elements and techniques from the cited references can similarly be combined to yield further implementations within the scope of the present invention. Thus, for example, holograms with watermark data can be employed in banknotes, single-bit watermarking can commonly be substituted for multi-bit watermarking, technology described as using imperceptible watermarks can alternatively be practiced using visible watermarks (glyphs, etc.), techniques described as applied to images can likewise be applied to video and audio, local scaling of watermark energy can be provided to enhance watermark signal-to-noise ratio without increasing human perceptibility, various filtering operations can be employed to serve the functions explained in the prior art, watermarks can include subliminal graticules to aid in image re-registration, encoding may proceed at the granularity of a single pixel (or DCT coefficient), or may similarly treat adjoining groups of pixels (or DCT coefficients), the encoding can be optimized to withstand expected forms of content corruption. Etc., etc., etc. Thus, the exemplary embodiments are only selected samples of the solutions available by combining the teachings referenced above. The other solutions necessarily are not exhaustively described herein, but are fairly within the understanding of an artisan given the foregoing disclosure and familiarity with the cited art.
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The presently claimed invention relates generally to digital watermarking, and processing imagery (e.g., including video) or audio content. One claim recites a method including: obtaining first media comprising imagery or audio; obtaining second media comprising imagery or audio; aggregating the first media and the second media to yield a unit; and using a programmed electronic processor, examining the unit for the presence of a digital watermark. Another claim recites a method comprising: upon encountering imagery or audio content, performing a screening operation on the imagery or audio content; based at least in part on the result of the screening operation, determining whether to derive or extract identifying data from the imagery or audio content, said act of determining uses a programmed electronic processor; providing the identifying data for storage in an electronic data record. Still another claim recites a method comprising: using a programmed electronic processor, extracting identifying data from data representing imagery or from data representing audio; automatically dialing a telephone number; providing the identifying data for telephonic communication to a device hosting the telephone number; receiving signals representing a human voice command; and providing signals for telephonic communication to a device hosting the telephone number. Of course, other claims and combinations are provided too.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. application Ser. No. 13/099,017 filed May 2, 2011, which is a continuation of U.S. application Ser. No. 11/337,163 filed Jan. 20, 2006, which is a non-provisional of U.S. Provisional Patent App. Ser. No. 60/647,464 filed Jan. 28, 2005, the entire disclosures of which are hereby incorporated by reference.
BACKGROUND OF INVENTION 1. Field of Invention
[0002] This invention relates to cleaning compositions for body, food, and food contact surfaces which reduce the risk of illness caused by harmful chemical residues, infectious agents and other disease causing and spoilage microbial agents. More particularly, the present invention provides chemical disinfecting compositions which reduce injury or inflammation to the skin. Even more particularly the present invention concerns disinfecting compositions which use safe and non-toxic chemical agents selected from alcohol esters of ethyl lactate and its homologs for preparing products with cleaning, solubilizing, antimicrobial and microbicidal properties.
[0003] 2. Prior Art
[0004] Most common antimicrobial products such as chlorine, chlorine dioxide peracetic acid, ozone, hydrogen peroxide, UV- and other radiations, used to reduce microbial population on food and other contact surfaces possess highly oxidizing and sometimes destructive properties. These oxidizing chemicals and physical agents inactivate microorganisms by reacting with their organic material. However, these chemicals also react with organic food material and produce unknown chemical residues often harmful to human and animal health. Hypochlorite (chlorine) produces carcinogenic residues on food. These antimicrobial products do not have detergent action or cleaning properties. Some other cleaning preparations that are allowed on food either do not have antimicrobial and microbicidal properties or are not safe enough as the ingredients are not considered by the FDA as GRAS or food additive safe. Some other preparations have disinfecting properties without the solubilizing properties to remove harmful pesticide residues. Still some other cleaning products need to incorporate antibacterial compounds in these preparations to inhibit or kill microorganisms.
[0005] Thus, there is a need for cleaning compositions containing antimicrobial and disinfecting properties which do not exhibit the deleterious properties identified above.
[0006] The antimicrobial cleaning compositions of this invention, as described below, employ all GRAS and/or food grade additive ingredients with cleaning, solubilizing, detergent and antimicrobial properties.
SUMMARY OF INVENTION
[0007] In accordance herewith, there is provided a class of chemical compositions predicated on chemical agents that can be used to prepare antimicrobial, microbicidal and disinfecting compositions for cleaning fresh fruits, vegetables, seeds, sprouts, meats, poultry, eggs, carcasses, other food surfaces and surgical instruments as well as body parts in order to prevent, to reduce or to eliminate the risk of infection and illness arising from both chemical residues and microorganisms spread by or carried on the food, food contact and body surfaces.
[0008] The antimicrobial cleaning and disinfecting composition hereof comprises:
[0009] (a) at least one alcohol ester of an organic acid, alone, or in admixture with one or more of,
[0010] (1) an antimicrobial surface active agent selected from chemicals classified as GRAS or food grade additive by the US FDA;
[0011] (2) an emulsifying surface active agents classified as GRAS or food grade additive by the USFDA;
[0012] (3) an organic acidifying agent selected from chemicals classified as GRAS or food grade additive by the USFDA which adjust the pH of the composition between 2 to 12;
[0013] (4) a chelant, either organic or inorganic, selected from chemicals classified as GRAS or food grade additive by the USFDA;
[0014] (5) a reducing agent or an antioxidant selected from chemicals classified as GRAS or food grade additive by the USFDA, and
[0015] (6) a diluent to dissolve, disperse or suspend the ester and any one of the above ingredients.
[0016] The composition hereof may include other compatible ingredients, which do not reduce or interfere with the antimicrobial and cleaning properties such as for example, urea, to enhance the cleaning properties of the composition.
[0017] The composition may, additionally, include a coloring agent, fragrances, vitamins, nutritive agents and/or a thixotropic agent or other agents, which alter physical and functional properties of the composition as, desired.
[0018] The present cleaning compositions can be prepared in either concentrated liquid or powder forms as well as in gel form, or as in a foam, thus, giving operational flexibility for use. The concentrate can be further diluted to form a use composition.
[0019] For a more complete understanding of the present invention reference is made to the following detailed description and accompanying illustrative examples.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0020] As noted hereinabove, the present invention provides a cleaning and disinfecting compound using GRAS or food grade additives and which comprises an alcohol ester of an organic acid used alone or in admixture with any one of: (a) surface active agents, (b) emulsifying agents, (c) acidifying agents, (d) sequestrants or chelants, (e) reducing agents or antioxidants, and/or (f) a diluent.
[0021] Other adjuvants such as fragrances, coloring agents and the like may, also be incorporated into the composition.
[0022] With more particularity, the alcohol ester contemplated for use herein is the reaction product of a C to C.sub.12 fatty alcohol and a C.sub.1 to C.sub.8 fatty acid.
[0023] The ester hereof may be represented by the formula:
[0000] R—COO—R. sub.1
where R is an acid moiety and is either C.sub.nH.sub.2n+1 or C.sub.nH.sub.2n+1O where n is an integer ranging from about 1 to about 8 and R.sub.1 is an alcohol moiety corresponding to the formula C.sub.mH.sub.m+1 here m is an integer ranging from about 1 to about 12.
[0026] Respective useful esters include, for example, methyl lactate, ethyl lactate, propyl lactate, butyl lactate, etc., and the like, as well as mixtures thereof.
[0027] Among the surface active agents classified by the US FDA as generally regarded as safe (GRAS) and or classified as food additive, and having antimicrobial properties that impart additional cleaning microbicidal properties that may be incorporated into the composition hereof, include, for example lactylic esters of C.sub.6 to C.sub.16 fatty acid and the corresponding alkali salts. Other useful compounds include, for example, dioctyl sodium sulfosuccinate, sodium lauryl sulfate, salts of fatty acids and sodium mono and dimethyl naphthalene sulfonate. Mixtures of such surfactants may be used herein.
[0028] Representative of useful emulsifying agents include, for example, food grade or GRAS lecithin, polysorbate 60, polysorbate 65, polysorbate 80, sucrose fatty acid esters, salts of stearyol 2-lactylate and the like, as well as mixtures thereof.
[0029] The acidifying agent, where used, may be selected from acetic acid, adipic acid, ascorbic acid, benzoic acid, citric acid, dehydroacetic acid, erythorbic acid, fumaric acid, glutaric acid, gluconic acid, hyaluronic acid, hydroxyacetic acid, lactic acid, malic acid, sorbic acid, succinic acid, tannic acid, tartaric acid, sulfuric acid, phosphoric acid, nitric acid, hydrochloric acid, sulfamic acid, carboxylic acid polymers, homo- or hetero-polymerized carboxylic acid such as poly lactic acid or poly lactic-glycollic acid, and the like, as well as mixtures thereof Where used, the acidifying agent is, preferably, lactic acid.
[0030] Either an organic or inorganic sequestrating or chelating agent selected from chemicals classified as GRAS or food grade additive by the US FDA such as gluconic acid and citric acid esters such as isopropyl citrate, monoisopropyl citrate, and stearyl citrate may, also, be used herein.
[0031] Also, a reducing agent or an antioxidant selected from chemicals classified as GRAS or food additive by the US FDA such as BHT, propyl gallate, and L-cysteine, and the like, may be used herein.
[0032] The composition may be admixed with a suitable diluent be it liquid, powder, gel or foam form to dissolve or disperse or suspend the component(s). The dilutent is selected from chemicals classified as GRAS or food additive by the US FDA, and include, for example, ethyl alcohol, propylene glycol, isopropyl alcohol, water, fatty acid esters of carbohydrates including sucrose, sorbitol and the like, other useful diluents include, for example, triglycerides of fatty acids, derivatives or simple compounds of silica, cellulose, starch and natural products or synthetic polymers, and the like, as well as mixtures thereof Preferred diluents include water, ethanol as well as propylene glycol and mixtures thereof
[0033] Where the composition is the ester itself it is dispersed in a suitable diluent to form a concentrate containing from about 0.001% to about 99.999%, by weight, of the ester and, preferably, from about 0.01% to about 99.999%, by weight, of ester.
[0034] Where the ester is used in conjunction with any of the aforementioned additional components, generally, the ester will be present in the composition, in an amount ranging from about 0.001% to about 99.99%, by weight, based on the total weight of the concentrate.
[0035] Generally, where the additional component is a surface active agent, the concentrate will contain from about 0.01% to about 40.00%, by weight, of the surfactant based on the weight of the concentrate.
[0036] Where the ester is used with an emulsifier, the concentrate will comprise from about 0.01% to about 40.00% by weight of the emulsifier based on the weight of the concentrate.
[0037] Where the adjuvant is an acidifying agent, it will be present in an amount ranging from about 0.01% to about 40% by weight of the acidifying agent based on the weight of the acidifying concentration.
[0038] The chelant, where used, will be present in the concentrate in an amount ranging from about 0.01% to about 10% by weight, based upon the total weight of the concentrate.
[0039] With respect to the reducing agent or antioxidant, where used, in forming the concentrate it will be present in an amount ranging from about 0.01% to about 40.00% by weight, based on the weight of the concentrate.
[0040] Where the concentrate is an admixture of each of the adjuvants, the resulting composition will contain from about 0.01% to about 99.99%, by weight, of the ester; from about 0.01% to about 40.00% by weight, of the surfactant; from about 0.01% to about 40.00% by weight, of the emulsifier; from about 0.01% to about 10.00% by weight, of the chelant; from about 0.01% to about 40.00% by weight, of the reducing agent, all based upon the total weight of the concentrate.
[0041] In preparing the concentrate, it is prepared at room temperature, by admixing the components together.
[0042] In forming the use solution, the use solution will contain from about 0.01% to about 99.99% by weight, of the ester and from about 0.01% to about 99.99% by weight, of the additional component, be it any one component or a mixture thereof.
[0043] The use solution is prepared at room temperature by mixing or admixing together the concentrate with the diluent.
[0044] Where the diluent is a powder, the powder is brought into a solution or suspension with the concentrate, the powder being mixed therewithin.
[0045] Generally, the final form of the use composition will contain from about 0.01% to about 99.99%, by weight, of ester; from about 0% to about 99.99%, by weight of adjuvant or additional component and from about 0.01% to about 99.99%, by weight, based on the final form of the use composition of diluent.
[0046] The composition hereof is storage stable and exhibits antimicrobial cleaning and disinfecting properties.
[0047] For a more complete understanding of the present invention, reference is made to the following examples, which are to be constructed as illustrative not limitations of the present invention, all parts are by volume.
Example I
[0048] This example illustrates the sporicidal activity of lactic esters against Bacillus coagulans spores.
[0049] One ml each of a mixture of ethyl lactate and butyl lactate (1:1) was mixed, at room temperature, with 0.1 ml of B. coagulans spore suspension containing 1.5.times.10.sup.6 spores per ml and incubated at room temperature for five minutes. B. coagulans exhibit very high heat resistance and is used as an indicator for bacteria in a heat sterilization process.
[0050] After five minutes 1 ml of the test mixture was mixed with 10 mls of Butterfield's buffer, at pH 7.0. Then, 0.1 ml of the buffered test mixture was plated on a plate count in agar. The colonies were counted after 48 hrs of incubation at room temperature.
[0051] The following table, Table I, shows the results of the colony counting.
[0000]
TABLE 1
Sporicidal Activity of Lactic Esters
Starting Number of Spores in the inoculum:
1.5 × 10 6 /ml
Number of spores in the test (diluted 1:10):
1.5 × 10 5 /ml
Number of spores in the buffer (diluted 1:11):
1.4 × 10 4 /ml
Number of spores plated (0.1 ml):
1.4 × 10 3 /ml
Surviving number colony forming units:
150/plate
Percentage killed (1.4 × 10 3 − 150) × 100:
89.28%
[0052] Example 1 shows that the mixture of ethyl lactate and butyl lactate displays sporicidal activity.
Example II
[0053] This example illustrates the microbicidal activity of ethyl lactate and butyl lactate against vegetative bacteria. Example II, also, shows the minimum lethal activity (MLC) of these lactic esters against both gram positive and gram-negative bacteria.
[0054] The microbicidal activity was further investigated by determining the minimum inhibitory concentration (MIC) and minimum lethal concentrations (MLC) of these esters.
[0055] The tests were carried out in 10 ml of brain heart infusion broth. The esters were serially diluted in brain heart infusion broth of samples of, 0.1, 0.2, 0.3, 0.4 and 0.5/10 ml and challenged with 0.1 ml of 1/100 dilution of 24 hr old brain heart infusion bacterial culture. The lowest concentration determined the minimum inhibitory concentration (MIC). The samples were observed after 48 hrs at 37.degree. C. A loopful from tubes without growth were plated on BHI agar plates and observed for growth for 24 to 48 hrs at 37.degree. C. The samples with the lowest concentration of the ester without bacterial growth on the plates represented the minimum lethal concentration (MLC).
[0056] Tables 2 and 3, below, show the results of the tests.
[0000]
TABLE 2
Antimicrobial Properties of Ethyl Lactate
Concentration of Ethyl lactate
Test Organism
0.5%
1%
2%
3%
4%
5%
E. coli 0157;H7
MLC
+
+
−
−
−
−
MLC
+
+
+
−
−
−
Listeria monocytogenes
MLC
+
+
+
+
+
+
MLC
+
+
+
+
+
+
Pseudomonas aeruginosa
MLC
+
+
−
−
−
−
MLC
+
+
+
+
−
−
Staphylococcus aureus
MLC
+
+
+
+
+
−
MLC
+
+
+
+
+
+
Salmonella typhimurium
MLC
+
+
+
+
−
−
MLC
+
+
+
+
+
+
MIC = Minimum Inhibitory Concentration,
MLC = Minimum Lethal Concentration;
+ = growth (inactive);
− = no growth (active)
[0000]
TABLE 3
Antimicrobial Properties (MLC) of Butyl Lactate
Concentration of Butyl lactate
Test Organism
0.5%
1%
2%
3%
4%
5%
Pseudomonas aeruginosa
MLC
+
+
+
−
−
−
Listeria monocytogenes
MLC
+
+
−
−
−
−
MIC = Minimum Inhibitory Concentration,
MLC = Minimum Lethal Concentration;
+ = growth (inactive);
− = no growth (active)
Example III
[0057] This example illustrates the enhancement of antimicrobial activity of lactic esters by the incorporation of additional components therewith.
[0058] A series of samples of (a) methyl lactate, (b) ethyl lactate and (c) butyl lactate, alone, and in admixture with varying amounts of decyl lactate and sodium dodecyl sulfates were used to test minimum inhibitory activity (MIC) by the method described in Example II, against the cultures of E. coli 0157 H7, Listeria monocytogenes, Staphylococcus aureus, Salmonella typhi , and Pseudomonas aeruginosa . Tables 4 and 5 show that decyl lactate and sodium dodecyl sulfate enhanced inhibitory activities against the test bacteria.
[0000] TABLE 4 Enhancement of Antimicrobial Properties (MIC) of Ethyl lactate by Decyl lactylate Test Organism Test Compound 1% 2% 3% 4% 5% E. coli 0157;H7 EL + + + − − EL + DL + + − − − Listeria monocytogenes EL + + + + + EL + DL − − − − Staphylococcus aureus EL + + + + + EL + DL − − − − − Salmonella typhi EL + + + − − EL + DL + + − − MIC = Minimum Inhibitory Concentration, + = growth (inactive); − = no growth (active)
In undiluted form these esters were found to kill all vegetative bacteria on contact.
[0000]
TABLE 5
Enhancement of Antimicrobial Properties (MIC) of Lactic esters by
Sodium dodecyl sulfate against Pseudomonas aeruginosa
SDS
Concentration of Lactic Esters
Test Organism
DL
ppm
0.5%
1%
2%
3%
4%
5%
Methyl lactate
MIC
0.0
+
+
−
−
−
−
50
−
−
−
−
−
−
100
−
−
−
−
−
−
200
−
−
−
−
−
−
Ethyl lactate
MIC
0.0
+
+
−
−
−
−
50
−
−
−
−
−
−
100
−
−
−
−
−
−
200
−
−
−
−
−
−
Butyl lactate
MIC
0.0
+
+
−
−
−
−
50
−
−
−
−
−
−
100
−
−
−
−
−
−
200
−
−
−
−
−
−
MIC = Minimum Inhibitory Concentration,
MLC = Minimum Lethal Concentration;
+ = growth (inactive);
− = no growth (active)
[0059] These results show that the microbicidal activity of lactic esters can be enhanced to include a broad spectrum activity against both bacterial spores as well as vegetative bacterial pathogens.
Example IV
[0060] This example illustrates the MIC and MLC of esters of lactic acid against yeast: Saccaromyces cerevisiae.
[0061] A 0.1 ml of 1/100 dilution of 48 hr old culture of S. cerevisiae was used as inoculum. The test was performed using Sab. broth. The tubes were incubated at room temperature 25.degree. C. The test was read after 48 hrs. The results are shown in Tables 6 and 7 below.
[0000]
TABLE 6
Antimicrobial activity against Saccharomyces cerevisiae
Inhibitory (MIC)/Lethal (MLC)
Test
Concentration
Test Ester
Type
1%
1.5%
2%
3%
4%
Methyl lactate
MIC
+
+
+
−
−
MLC
+
+
+
−
−
Ethyl lactate
MIC
+
−
−
−
−
MLC
+
+
−
−
−
Butyl lactate
MIC
−
−
−
−
−
MLC
−
−
−
−
−
[0000]
TABLE 7
Enhancement of Antimicrobial Properties (MIC) of Lactic esters by
Sodium dodecyl sulfate against saccharomyces cerevisiae
Inhibitory (MIC)/Lethal (MLC)
Sodium lauryl
Concentration
Ester Tested
sulfate (ppm)
1%
1.5%
2%
3%
4%
Methyl lactate
200
MIC
+
+
+
−
−
MLC
+
+
+
−
−
Ethyl lactate
200
MIC
+
−
−
−
−
MLC
+
+
−
−
−
Butyl lactate
200
MIC
−
−
−
−
−
MLC
−
−
−
−
−
Example V
[0062] This example shows that ethyl lactate can be used to solubilize other antimicrobial agents or ingredients that have low solubility in aqueous solutions. In this example ethyl lactate was used to prepare aqueous antifungal preparations of dehydroacetic acid.
[0063] Into a suitable reaction vessel dehydroacetic was mixed together at room temperature 5.0 parts of dehydroacetic acid in 100 ml of ethyl lactate.
[0064] A clear solution was formed. A 0.1 ml sample was added to 2 ml a wax coating sample. The mixture was homogeneous and did not show precipitate. The final concentration of dehydroacetic acid in the coating solution was 2,500 ppm. Thus, in parting antifungal properties to wax coating.
[0065] By reducing the spoilage microbial population the present esters, alone, or in combination with any of the above additives helps to increase the shelf life and/or keeping qualities of food. Thus the invention offers to prevent economic loss due to food spoilage and improves public health and curtails medical costs arising from food-borne and other infectious agents.
[0066] The alcohol esters of fatty acids hereof also display lethal activity against difficult to kill bacterial spores. These microbicidal agents can also be incorporated into household, personal care, health care and homeland security-related products. By incorporating other non-toxic, and generally regarded as safe (GRAS) or other ingredients considered as food additive by the United States Food and Drug Administration (US FDA), the technology provides the potential to replace products with toxic manifestation. In addition to microbicidal properties these agents can be used to solubilize and to remove certain water insoluble harmful residues from food.
[0067] The compositions can also be used to clean and disinfect inanimate surfaces. The composition can also used to prepare personal care and healthcare products used for preventing and reducing skin infections, either by direct application or by incorporating in ointments, bandages or other carriers. Further the chemicals can also be used to destroy harmful bacterial spores that are very resistant to known disinfecting agents.
[0068] These esters can also be formulated with other ingredients to prepare highly effective microbicidal products for cosmetic personal care, healthcare, pharmaceutical and other industries. Powerful microbicidal and cleaning products can be developed incorporating these esters in product formulations.
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Broad spectrum disinfecting and microbicidal compositions of biodegradable and environmentally friendly compositions containing esters formed from fatty organic alcohols and fatty carboxylic acids. These compositions display activities against the most resistant microbial forms including bacterial spores. The preparations can be used in health care, food processing, personal care and other industries where the use of harsh oxidizing chemicals is undesirable.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to systems for removably sealing a closure member to an opening, such as a window shade to a frame using magnetic attractive forces.
2. Description of the Prior Art
It has long been appreciated that magnetic forces could be desirably utilized to secure various types of coverings to a window frame. For example, U.S. Pat. No. 3,679,505 (Hinderaker and Nelson) discloses a method of sandwiching a flexible insect screen between parallel strips of a flexible rubber based magnet such as Plastiform®, manufactured by Minnesota Mining and Manufacturing Company, St. Paul, Minn., such that when the screen is magnetically attracted to a vehicle window frame substantially no gaps between the screen and frame are present, thus facilitating the use of the vehicle for sleeping accommodations during camping trips.
Flexible window coverings are also disclosed in U.S. Pat. Nos. 2,321,078 and 2,514,316. While not there suggested, such coverings could also be held in place via magnets disposed about the periphery of the covering. U.S. Pat. No. 3,133,324 discloses the use of magnetic fasteners when using conventional rigid window constructions.
All known window systems using magnetic attraction provide a magnet construction on the closure element and a magnetizable element providing a magnetic flux return path in the frame. In some systems, the flux path is present as a result of the intrinsic ferromagnetic nature of the frames such as a vehicle body, while in other systems a separate ferromagnetic strip is inserted into the frame. Even when "flexible" rubber based magnets such as employed in U.S. Pat. No. 3,679,505 are so used, a relatively thick and stiff member is present which precludes using the closure member in roll-up form ala a conventional window shade.
SUMMARY OF THE INVENTION
The recent, greatly intensified, importance placed on conservation of energy has resulted in a greater concern for reducing heat loss through architectural windows. Typical constructions which have found increasing acceptance in effecting such a reduction are solar control films adhered to windows such that internally generated heat is reflected back into the room. While such permanently adhered films are satisfactory for certain applications, they are not desirable in other installations, such as on south facing windows which may realize a net gain in energy be maximizing the influx of solar energy during the day, while minimizing the loss of internal heat during cloudy days and at night. The desire to minimize the heat loss in such installations has emphasized the need for a flexible heat shield, i.e., shade, which can be removably sealed to existing frames while yet allowing the shield to be rolled up during periods when influx of solar radiation is desired.
In the present invention, such a capability is provided by a sealing strip adapted for use in a window shade and frame combination in which a magnetized strip is disposed along a major portion of the periphery of the frame and the sealing strip is secured to the shade such that when the shade is in juxtaposition with the frame the sealing strip is attracted to the magnetized strip, thereby forming a reclosable seal between the shade and the frame to inhibit convection currents. In this invention, the sealing strip comprises a layer of magnetically soft particles, such as a ferromagnetic stainless steel powder, in a flexible polymeric binder, which particles have a saturation induction in excess of 4000 gauss, have a particle size ranging between 50 and 1000 micrometers, and are present in the layer in an amount ranging between 0.01 and 0.2 grams/cm 2 , and an adhesive, preferably a layer of pressure sensitive adhesive, for securing the sealing strip to the window shade. The layer of magnetically soft particles is conveniently characterized in terms of the shear force required to slide a section of the sealing strip having a defined area from a standard magnet prepared from a section of the permanent magnetized strip having a further defined area and magnetic attractive force. In such a test, the standard magnet is fabricated to have a substantially planar surface of one cm square and to have a magnetic attraction force such that it will stay in surface contact with a one cm square section of low carbon steel against a force applied normal to the surface of the sections of 70 grams. A one square cm of the sealing strip is then placed in surface contact with the standard magnet. Under such conditions, the sealing strip of the present invention will stay in position against a shear force of 1 gram.
In a further embodiment of the present invention, such a sealing strip is permanently affixed to a window shade and forms a part of a system including a frame having the permanent magnetized strip disposed along a major portion of the periphery of the frame.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a partially cut-away perspective view of a window frame and shade sealing system according to the present invention; and
FIG. 2 is a cross-section of the shade sealing system of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 discloses a window frame 10 having mounted thereon in a conventional manner double hung sashes 12 and 14 respectively. Mounted at the top of the frame are brackets 16 and 18 for supporting a roll-up type roller shade 20. A flat narrow strip of a flexible rubber based magnet 22 such as Plastiform®, type M.G.O. 1017 manufactured by Minnesota Mining and Manufacturing Company and disclosed in U.S. Pat. No. 2,999,275 is secured along the vertical sides 24 and 26 of the frame 10 and along the bottom horizontal side 28. Such a magnetized strip has a layer of pressure sensitive adhesive secured to one surface of the strip, which adhesive layer is protected prior to installation by a release liner. The strip is magnetized with alternating magnetic poles extending across its breadth, 8 poles per in (3.2 poles/cm). A 60 mil (0.15 cm) thick section typically exhibits an external magnetic field such that a 1 cm square section of the magnetized strip will stay in surface contact with a 1 cm square section of low carbon steel against a force applied normal to the surface of the sections of 70 grams. I.e., that it will withstand a normal force of at least one pound/square inch (70 grams/cm 2 ). A preferred installation utilizes a 1/2 inch (1.2 cm) wide section of such a strip, 60 mils (0.15 cm) thick. Upon installation, the release liner is stripped off the magnetized strip and the adhesive layer is pressed against the frame. Other magnetized strips without the adhesive layer may be secured by a variety of mechanical fasteners. Similarly, magnetized strips of a nonflexible construction such as a length of ceramic magnet could also be used.
In order to minimize air convection currents which increase the heat transfer through the windows 30 and 32, it is preferred that the magnetized strip 22 extend substantially continuously along the three sides 24, 26 and 28 of the frame, without an appreciable gap therebetween. In the event the bottom horizontal section 28 of the frame is not in the same plane as the vertical sections 24 and 26, the magnetized strip along the horizontal section may be eliminated or positioned in another plane.
In order to maximize the magnetic attractive force provided by the magnetized strip 22, it is preferably magnetized with an alternating pole configuration extending across the breadth of the strip such as having 2-6 alternating poles per centimeter, however, other magnetization configurations may likewise be used. Furthermore, if the magnetizable material in the sealing strip is not saturated by the field of the magnetized strip, the attractive force may be improved by providing a flux return path in back of the magnetized strip. Such a path is intrinsically present if the frame 10 is of a ferromagnetic construction. Likewise, an additional ferromagnetic strip may be inserted between the frame 10 and the magnetized strip 22.
The shade 20 may be constructed of any of a variety of conventional sheet materials such as fabrics or flexible polymeric sheeting. In a preferred embodiment, the shade 20 comprises a polymeric sheet having an infrared-reflecting coating on at least one surface. A magnetizable sealing strip 34 is secured to the bottom edge 36 and to the sides 38 and 40 of the shade 20 such that when the shade 20 is in juxtaposition with the frame 10, the sealing strip 34 is attracted to the magnetized strip 22, thereby forming a reclosable seal.
The various elements of the present invention are more clearly shown in the cross-sectional view of FIG. 2. In that figure, it may be seen that the magnetized strip 22 is secured to the frame 10 via a layer of pressure sensitive adhesive 42. The shade 20 and sealing strip 34 are further shown to comprise a number of layers. The sealing strip 34 includes a layer of magnetizable particles 44 in a flexible polymeric binder 46, which binder adheres the particles 44 to a polymeric substrate 48. The adhesive layer 50 is further provided to adhere the strip 34 to the shade 20. In a preferred embodiment, the sealing strip 34 is made by coating a conventional double coated pressure sensitive adhesive tape, such as Type 444 manufactured by Minnesota Mining and Manufacturing Company, with ferromagnetic particles, after which the particles are pressed into the tape surface to maximize the adherence thereto. Particularly desirable constructions may be formed from 40-140 mesh particles having an average particle size ranging between 100-400 micrometers of ASM type 410 ferromagnetic stainless steel. Similarly, any ferromagnetic particle having a saturation induction in excess of 4000 gauss is suitable for use in the present invention. Such particles may be formed of materials selected from the ferromagnetic elements (iron, cobalt and nickel, which have a saturation induction of approximately 21,000, 18,000 and 6,000, respectively) as well as alloys including such materials as ferromagnetic oxides and ferrites. In a preferred embodiment, magnetically soft ferromagnetic particles of Fe and ferromagnetic stainless steel are utilized. Such particles are preferably applied to the adhesive tape in an amount ranging between 0.01 and 0.2 grams/cm 2 .
It has been found that if extremely small particles are dry coated onto a previously prepared adhesive surface, the small particles rapidly detackify the adhesive surface and result in a mono layer in which the coating weight is insufficient to provide adequate attractive force for many applications. Conversely, if large particles are provided, insufficient contact of the particles with the adhesive may occur such that the particles are readily removed from the adhesive layer. Typically, such a construction is further provided with a release liner adjacent the exposed surface of the adhesive layer 50. Such a liner is advantageous in that the sealing strip 34 may be separately marketed and applied to pre-cut shade materials as a separate processing step. Where the shade material and the sealing strip are to be manufactured as an integral unit, an adhesive/binder material may be applied directly to the edges of the shade material and the magnetizable particles applied directly to the binder without the use of an intermediate substrate such as the polymeric sheet 48.
In order to provide an adequate seal between the frame 10 and shade 20, it has been found desirable that the magnetic attractive force between the frame and the shade exceed a certain force. This force can be varied both by modifying the magnetic field provided by magnetized strip 22 or by modifying the saturation induction of ferromagnetic particles in the sealing strip 34. It has been found that an attractive force as expressed hereinabove in terms of the shear force in excess of approximately 1 gram/cm 2 is sufficient to provide a seal in applications where the windows 30 and 32 are allowed to be opened, such that air currents may be directed against the shade 20.
In two examples where 40 mesh particles of iron and 50 mesh particles of type 410 stainless steel were coated onto type 444 double coated tape in the manner discussed hereinabove, resulting in a coating weight of 0.082 and 0.050 grams/cm 2 respectively, which tapes were than applied to a smooth polyester sheet, a shear force of 9.0 and 6.0 grams respectively was observed for 1 cm 2 sections when the smooth surface of the polyester sheets were adjacent the magnet. The holding force is, of course, appreciably greater when the magnet and magnetizable layer are in direct contact, resulting in enhanced magnetic coupling and greater friction between the members.
In a particularly preferred construction, the shade 20 comprises a polymeric sheet 52 such as polyester or similar materials onto which is coated an infrared-reflecting layer 54. The layer 54 typically consists of an evaporated thin film such as gold, silver, copper or aluminum, which layer may also be sandwiched between dielectric layers in order to provide enhanced antireflection of visible light. When a conventional opaque vinyl shade was sealed to a typical architectural window frame fitted with single pane windows via the described sealing strips and flexible magnetized strips applied substantially continuously along the sides and bottom of the frame, a 44% reduction in the heat loss over that of the same, but unsealed, shade was observed.
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A system for controlling the transmission of heat through architectural windows is disclosed in which a magnetized strip is disposed along a major periphery of a frame supporting the window and a flexible window shade is supported adjacent to the frame and is magnetically attracted to the magnetized strip on the frame by a flexible sealing strip secured to the shade. The sealing strip contains a layer of magnetizable particles in a flexible polymeric binder.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is the U.S. national stage of International Application No. PCT/EP2012/058499, filed, May 9, 2012 and claims the benefit thereof. The International Application claims the benefits of Austrian Application No. A723/2011 filed on May 19, 2011, both applications are incorporated by reference herein in their entirety.
BACKGROUND
[0002] 1. Technical Field
[0003] Described below is a method for charging material, including lumped carbonaceous (coal-containing) material and (e.g., hot) iron carrier material, into a melter gasifier of a smelting reduction plant.
[0004] 2. Related Art
[0005] In the context of smelting reduction processes for producing pig iron in a melter gasifier, e.g. COREX® or FINEX®, material including carbonaceous material, iron carrier material and fluxes is charged into the melter gasifier. The carbonaceous material is gasified with oxygen to produce a reduction gas, the heat required to melt the iron carrier material being released in the process.
[0006] Carbonaceous material includes e.g. coal in lump form or carbonaceous briquettes. It is stored at ambient temperature in a charging bin for carbonaceous material, from which it is loaded into the melter gasifier. In the case of FINEX®, for example, the iron carrier material is hot-briquetted iron (HBI) or hot-compacted iron (HCI). HBI is hot-compacted iron having a very high proportion of metallic iron (often more than 90% metallization) and a density of approximately 5 g/cm 3 , allowing transport by ship, for example. The material takes the form of individual briquettes, generally >25 mm, and is therefore present in lump form. HCI is hot-compacted iron with fluxes and has a lower proportion of metallic iron than HBI. Its density is slightly less than 4 g/cm 3 . As part of the manufacturing process for pig iron, HCI is further processed immediately after production, being granulated by crushers and used in a form that is advantageous for a melter gasifier. HCI has a temperature of approximately 550-650° C. in this case. In the case of COREX®, the iron carrier material is e.g. hot direct reduced iron (DRI).
[0007] Pyrolysis of coal or carbonaceous briquettes at high temperatures results in the development and release of volatile hydrocarbons and tar. Therefore the carbonaceous material cannot be stored together with hot iron carrier material in a charging bin, since the development and release of volatile hydrocarbons and tar, triggered by the contact with the hot iron carrier material, would result in conglutination and blockages in the charging bin and in the lines transporting the material to the melter gasifier.
[0008] The charging of carbonaceous material and iron carrier material into a melter gasifier usually takes place separately in existing related art installations.
[0009] Carbonaceous material is transported from e.g. a charging bin for carbonaceous material via screw feeders to a distributing device which is disposed centrally in the dome of the melter gasifier and from which the carbonaceous material is distributed over the cross-section of the melter gasifier as it is introduced into the melter gasifier. Iron carrier material is introduced into the melter gasifier e.g. via a plurality of drop shafts which are arranged around the circumference of the dome of the melter gasifier.
[0010] The separate addition of carbonaceous material and iron carrier material into the melter gasifier involves considerable expense in terms of the construction and maintenance of those plant parts required for the separate addition. Moreover, in the case of separate addition, the carbonaceous material and iron carrier material are not distributed with an adequate degree of control on the material bed in the melter gasifier, and e.g. the formation of vertical islands of iron carrier material can occur, thereby adversely affecting the melting and gasification process.
[0011] It is known from EP0299231A1 to charge the carbonaceous material and the iron carrier material into the melter gasifier centrally via the same opening. Central charging as described in EP0299231A1 is disadvantageous in that fresh material is supplied to precisely that region of the material bed which is known as the “dead man” region in the melting and gasification process, wherein preheating and reduction processes take place less effectively than in the peripheral region of the melter gasifier. Moreover, fine and heavy material remains concentrated in the central region of the material bed due to segregation processes, while coarser and lighter material migrates toward the peripheral region. Accordingly, the mixture which is charged onto the material bed is again segregated to some extent and in an uncontrolled manner.
SUMMARY
[0012] The method and device are for charging material which includes carbonaceous material and (e.g., hot) iron carrier material, the method and device, in comparison with the related art, not only being associated with less construction and maintenance overhead but also enabling controlled distribution.
Technical Solution
[0013] This is achieved by a method for charging material, including lumped carbonaceous material and (e.g., hot) iron carrier material, into a melter gasifier of a smelting reduction plant, wherein the lumped carbonaceous material and the (e.g., hot) iron carrier material are combined before and/or during entry into the melter gasifier, and the ratio of the combined quantities of (e.g., hot) iron carrier material and lumped carbonaceous material can be varied, wherein the combined quantities of (e.g., hot) iron carrier material and lumped carbonaceous material are distributed over the cross-section of the melter gasifier by a dynamic distributing device, and the ratio of the combined quantities of (e.g., hot) iron carrier material and lumped carbonaceous material is set as a function of the position of the dynamic distributing device.
Advantageous Effects
[0014] Using such a method, the melter gasifier requires fewer plant parts and openings for charging than when lumped carbonaceous material and iron carrier material enter the melter gasifier separately.
[0015] Hot iron carrier material is understood to mean iron carrier material having a temperature higher than 100° C., e.g., higher than 200° C., such as higher than 300° C. The iron carrier material contains elementary iron and/or iron oxide. The iron carrier material is present in lump form, in lump form with a proportion of fines, or as fine grain (such as less than 10 mm).
[0016] The carbonaceous material is present in lump form. The proportion of coal in the lumped carbonaceous material represents at least 50% by weight, e.g., at least 70% by weight, such as 90% by weight. In this case the proportion by weight relates to the weight of the constituents of the lumped carbonaceous material at the time when the constituents are loaded into the charging bin. In addition to coal, the lumped carbonaceous material may also contain coke, for example.
[0017] No further details of the fluxes such as limestone and/or dolomite and/or quartz, for example, which are also charged into the melter gasifier (which may be via the iron carrier route) in the context of a method, are included within the scope of the present application.
[0018] The lumped carbonaceous material and the (e.g., hot) iron carrier material may be combined shortly before and/or during entry of the mixture, which is obtained by the combination, into the melter gasifier. In this case, lumped carbonaceous material and the (e.g., hot) iron carrier material are merged during transport to the melter gasifier, e.g. in a chute, without previously being stored together in a bunker, in order to ensure that the time during which the two materials are present together in parts of the plant outside of the melter gasifier is restricted, for example, to less than a few seconds, e.g., up to 10 seconds. This reduces the risk that pyrolysis of the lumped carbonaceous material, triggered by contact with hot iron carrier material, will result in conglutination and blockages of the mixture, which is obtained by combination, in the plant parts leading to the melter gasifier.
[0019] The pyrolysis and gasification of the lumped carbonaceous material therefore first occurs in the melter gasifier.
[0020] The term melter gasifier does not include a blast furnace. In a blast furnace, layers of coke and iron carrier with fluxes are essentially added from above under environmental conditions. Pyrolysis and degasification of coal does not take place in the blast furnace, but beforehand during the production of the coke which is charged into the blast furnace. The temperatures at the top of a blast furnace range from approximately 80 to 250° C. In the case of a melting and gasification process in a melter gasifier, in contrast, not coke but carbonaceous material is charged, and the charged carbonaceous material is pyrolized in the melter gasifier. The temperatures prevailing in the melter gasifier dome are approximately 1000° C. in the region where material is charged into the melter gasifier.
[0021] As a result of charging lumped carbonaceous material and (e.g., hot) iron carrier material together, it is possible to avoid the problem of uncontrolled and unwanted inhomogeneous distribution which occurs when they are charged separately, e.g., forming vertical islands of iron carrier material in the melter gasifier. This also eliminates the expense associated with construction and maintenance of the plant parts that are required for separate charging.
[0022] A dynamic distributing device is understood to be a distributing device which can be moved in a controlled manner during the distribution process. An outlet opening of the dynamic distributing device can therefore be moved to various positions. Accordingly, the combined quantities of (e.g., hot) iron carrier material and lumped carbonaceous material can be directed to various locations of the material bed in the melter gasifier.
[0023] The dynamic distributing device can be a rotating chute or a gimbal-mounted chute, for example, which can be moved such that its outlet opening describes circular, spiral or freely definable paths, for example, it being also possible to select different distribution tracks. The movement pattern of the dynamic distributing device can advantageously be varied.
[0024] The charged material forms a material bed in the melter gasifier. The combined quantities of (e.g., hot) iron carrier material and lumped carbonaceous material are distributed by a dynamic distributing device over the cross-section of the melter gasifier, and the ratio of the combined quantities of (e.g., hot) iron carrier material and lumped carbonaceous material is set as a function of the position of the dynamic distributing device. By virtue of the position of the dynamic distributing device in the melter gasifier defining the region in which the material to be distributed strikes the material bed in the melter gasifier, the distribution of (e.g., hot) iron carrier material and lumped carbonaceous material on the material bed of the melter gasifier can be controlled and set according to the requirements of the melting and gasification process. Specific distribution patterns of (e.g., hot) iron carrier material and lumped carbonaceous material can therefore be set in the melter gasifier. For example, a dead man of mainly carbonaceous material can be selectively developed during phased charging of carbonaceous material with little iron carrier material in the melter gasifier. The setting of specific distribution patterns of iron carrier material and carbonaceous material in the melter gasifier allows better control of the processes that take place in the melter gasifier when converting iron carrier material and carbonaceous material. This results in greater operational stability and improved process yield.
[0025] For the purpose of the melting and gasification process, the region in which it is particularly beneficial to charge material onto the material bed in the melter gasifier can be derived from the properties of the surface. In this case, the surface of the material bed is also understood to mean the top layer of the material bed, viewed in a vertical direction. The top layer is understood to be a layer having a layer thickness of up to 20 cm.
[0026] According to an embodiment of the method, the ratio of the combined quantities of (e.g., hot) iron carrier material and lumped carbonaceous material is set as a function of properties of the surface of the material bed.
[0027] According to an embodiment of the method, the property of the surface of the material bed is the height level and/or the height profile of the material bed.
[0028] According to a further embodiment of the method, the property of the surface of the material bed is the temperature profile at the surface of the material bed.
[0029] Pig iron and slag are run off from a melter gasifier at approximately regular intervals during the day, in order to prevent the liquid level in the melter gasifier from rising above the level of the nozzles for the oxygen supply. Inhomogeneous gasification and reduction ratios continuously arise during operation as a result of the running off. Negative effects of such inhomogeneities on the smelting reduction process can be counteracted by selectively charging to relevant regions within the overall area. Correspondingly, an embodiment of the method provides for the ratio of the combined quantities of (e.g., hot) iron carrier material and lumped carbonaceous material to be set as a function of the run-off sequence that is followed during the operation of the melter gasifier.
[0030] Not only the ratio of the combined quantities of (e.g., hot) iron carrier material and lumped carbonaceous material, but also the grain size distribution and the types of materials have an effect on the melting and gasification process. With regard to the lumped carbonaceous material, grain size distribution in this case is understood to be the lump size of the lumped carbonaceous material. Various types of (e.g., hot) iron carrier material have different proportions of metallic iron and iron oxide or other constituents, for example. Various types of lumped carbonaceous material have different proportions of coke or other constituents, for example. Various types of (e.g., hot) iron carrier material and lumped carbonaceous material are dependent on the source from which they are obtained, for example. According to an embodiment of the method, the grain size distribution of the (e.g., hot) iron carrier material and/or the lump size of the lumped carbonaceous material are selected as a function of the position of the dynamic distributing device. According to a further embodiment of the method, the type of charged (e.g., hot) iron carrier material and/or the type of lumped carbonaceous material are selected as a function of the position of the dynamic distributing device.
[0031] The subject matter of the present application also relates to a device for charging material, including lumped carbonaceous material and (e.g., hot) iron carrier material, into a melter gasifier of a smelting reduction plant, having at least one charging bin for lumped carbonaceous material, and having at least one charging bin for (e.g., hot) iron carrier material, wherein a first discharge line for lumped carbonaceous material emerges from the at least one charging bin for lumped carbonaceous material and includes a first conveyor device for regulating the discharge of lumped carbonaceous material, and wherein a second discharge line for (e.g., hot) iron carrier material emerges from the at least one charging bin for (e.g., hot) iron carrier material and includes a second conveyor device for regulating the discharge of (e.g., hot) iron carrier material, and having an input device for inputting material into the melter gasifier wherein the first discharge line for lumped carbonaceous material and the second discharge line for (e.g., hot) iron carrier material open into the input device for inputting material into the melter gasifier, wherein the input device for inputting material into the melter gasifier includes a dynamic distributing device for distributing the material during the input, and a device is provided for controlling at least one of the conveyor devices from the group
[0032] first conveyor device for regulating the discharge of lumped carbonaceous material
[0033] second conveyor device for regulating the discharge of (e.g., hot) iron carrier material
[0000] as a function of the position of the dynamic distributing device.
[0034] The method can be performed using such a device. Carbonaceous material and (e.g., hot) iron carrier material can be combined before and/or during entry into the melter gasifier.
[0035] The input device for inputting material into the melter gasifier can include screw feeders, for example.
[0036] A device of the type can be operated in such a way that lumped carbonaceous material and (e.g., hot) iron carrier material are continuously combined. It can also be operated in such a way that iron carrier material, e.g., hot iron carrier material, is intermittently added to a continuous stream of carbonaceous material. It can also be operated such that lumped carbonaceous material is intermittently added to a continuous stream of iron carrier material, e.g., hot iron carrier material. It can also be operated in such a way that a stream of lumped carbonaceous material and a stream of (e.g., hot) iron carrier material are input alternately into the melter gasifier via the input device for inputting material.
[0037] The input device for inputting material into the melter gasifier includes a dynamic distributing device for distributing the material during the input. A distribution of the material over the horizontal cross-section of the interior of the melter gasifier is meant in this case. Specific distribution patterns of (e.g., hot) iron carrier material and lumped carbonaceous material can therefore be set in the melter gasifier. The input device for inputting material into the melter gasifier and including a dynamic distributing device can be a gimbal-mounted chute, such as driven via two axes, or a rotating chute, for example.
[0038] According to an embodiment of the device, two charging bins for (e.g., hot) iron carrier material and/or two charging bins for lumped carbonaceous material are provided. It is thereby possible to ensure more uniform charging, because a second, full charging bin can be used when the first charging bin is completely empty. While the second charging bin is being emptied, the first charging bin can then be replenished such that it is available for the charging again when the second charging bin is completely empty. Moreover, it is thereby possible to charge different types of (e.g., hot) iron carrier material and/or different types of lumped carbonaceous material, or to charge different grain sizes of (e.g., hot) iron carrier material and/or different lump sizes of lumped carbonaceous material, if the two charging bins are filled accordingly. It is also possible to provide more than two charging bins for iron carrier material, e.g., hot iron carrier material, and/or more than two charging bins for lumped carbonaceous material.
[0039] According to an embodiment of the device, the first conveyor device for regulating the discharge of lumped carbonaceous material and/or the second conveyor device for regulating the discharge of (e.g., hot) iron carrier material may include one or more material flow gates.
[0040] According to an embodiment of the device, the first conveyor device for regulating the discharge of lumped carbonaceous material and/or the second conveyor device for regulating the discharge of (e.g., hot) iron carrier material may include one or more screw feeders. Screw feeders allow more effective regulation of quantities than material flow gates and the material can be transported horizontally, wherein a plurality of charging bins can be arranged next to one another and the materials can be conveyed to the shared input device and thence to the melter gasifier.
[0041] According to an embodiment of the device, the first conveyor device for regulating the discharge of lumped carbonaceous material and/or the second conveyor device for regulating the discharge of (e.g., hot) iron carrier material may include one or more cellular wheel sluices. Cellular wheel sluices allow more effective regulation of quantities than material flow gates and, in comparison with screw feeders, can minimize an undesirable gas flow via the cellular wheel sluice if there is a pressure difference.
[0042] Hybrid forms are also possible, e.g. a device in which a screw feeder is provided for regulating the discharge of lumped carbonaceous material in the first discharge line, and a material flow gate is provided for regulating the discharge of (e.g., hot) iron carrier material in the second discharge line. Such a hybrid form is advantageous if it is necessary to generate a continuous stream of lumped carbonaceous material, for example.
[0043] According to an embodiment, a device is provided for regulating the distribution track which is realized during the input by the dynamic distributing device for the purpose of distributing the material. The dynamic distributing device has an outlet opening from which the material exits the dynamic distributing device. The distribution track is understood to be the track, as projected onto a horizontal plane, which is left on this plane by the outlet opening during charging. Specific distribution patterns of (e.g., hot) iron carrier material and lumped carbonaceous material can be set in the melter gasifier by varying the distribution track over the horizontal cross-section of the interior of the melter gasifier.
[0044] According to another embodiment, a device is provided for controlling the first conveyor device for regulating the discharge of lumped carbonaceous material, and/or the second conveyor device for regulating the discharge of (e.g., hot) iron carrier material, as a function of the distribution track which is realized during the input by the dynamic distributing device for the purpose of distributing the material. It is therefore possible to set a specific distribution pattern of (e.g., hot) iron carrier material and carbonaceous material in the melter gasifier. This device is used to control the material flow gates and/or the screw feeders, for example.
[0045] At least one device is advantageously provided for capturing properties of the surface of the material bed that has formed in the melter gasifier. Such a device may be e.g. a microwave measuring device or a radar measuring device for determining height and/or profile and/or temperature and/or the composition of the gas escaping from the material bed, or a thermometer for determining the temperature or the temperature profile at the surface of the material bed. A plurality of such devices may also be present.
[0046] Accordingly, a device is provided for controlling the first conveyor device for regulating the discharge of lumped carbonaceous material, and/or the second conveyor device for regulating the discharge of (e.g., hot) iron carrier material, as a function of the properties which have been captured by the device for capturing properties of the surface of the material bed that has formed in the melter gasifier. In this way the ratio of the combined quantities of (e.g., hot) iron carrier material and lumped carbonaceous material can be set as a function of properties of the surface of the material bed.
[0047] According to an embodiment of the device, provision is made for at least two charging bins for lumped carbonaceous material, these being filled with lumped carbonaceous material of different lump sizes. For example, a first charging bin for lumped carbonaceous material is filled with a lump size A, and a second charging bin for lumped carbonaceous material is filled with a lump size B, where the lump sizes A and B are different. If applicable, a third charging bin for lumped carbonaceous material may be present and filled with a lump size C, where the lump size C is different from the lump sizes A and B.
[0048] According to an embodiment of the device, provision is made for at least two charging bins for lumped carbonaceous material, these being filled with different types of lumped carbonaceous material. For example, a first charging bin for lumped carbonaceous material is filled with a type A, and a second charging bin for lumped carbonaceous material is filled with a type B, where the types A and B are different. If applicable, a third charging bin for lumped carbonaceous material may be present and filled with a type C, where the type C is different from the types A and B.
[0049] According to an embodiment of the device, provision is made for at least two charging bins for (e.g., hot) iron carrier material, these being filled with iron carrier material, e.g., hot iron carrier material, of different grain sizes. For example, a first charging bin for (e.g., hot) iron carrier material is filled with a grain size A, and a second charging bin for (e.g., hot) iron carrier material is filled with a grain size B, where the grain sizes A and B are different. If applicable, a third charging bin for (e.g., hot) iron carrier material may be present and filled with a grain size C, where the grain size C is different from the grain sizes A and B.
[0050] According to an embodiment of the device, provision is made for at least two charging bins for (e.g., hot) iron carrier material, these being filled with different types of (e.g., hot) iron carrier material. For example, a first charging bin for (e.g., hot) iron carrier material is filled with a type A, and a second charging bin for (e.g., hot) iron carrier material is filled with a type B, where the types A and B are different. If applicable, a third charging bin for (e.g., hot) iron carrier material may be present and filled with a type C, where the type C is different from the types A and B.
BRIEF DESCRIPTION OF THE DRAWINGS
[0051] These and other aspects and advantages will become more apparent and more readily appreciated from the following description of the exemplary embodiments, taken in conjunction with the accompanying drawings of which:
[0052] FIG. 1 is a schematic cross section of an embodiment of the device having material flow gates, and
[0053] FIG. 2 is a schematic cross section of an embodiment of the device having screw feeders.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0054] Reference will now be made in detail to the preferred embodiments, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to like elements throughout.
[0055] FIG. 1 shows a device for charging material, including lumped carbonaceous material 1 , this being represented by circles, and hot iron carrier material 2 , this being represented by squares, into a melter gasifier 3 of a smelting reduction plant. The device has a charging bin 4 for lumped carbonaceous material and a charging bin 5 for hot iron carrier material. A first discharge line 6 for lumped carbonaceous material emerges from the charging bin 4 for lumped carbonaceous material, the first discharge line including a first conveyor device 7 for regulating the discharge of lumped carbonaceous material 1 . A second discharge line 8 for hot iron carrier material emerges from the charging bin 5 for hot iron carrier material, the second discharge line including a second conveyor device 9 for regulating the discharge of hot iron carrier material 2 . The first conveyor device 7 for regulating the discharge of lumped carbonaceous material 1 and the second conveyor device 9 for regulating the discharge of hot iron carrier material 2 are embodied as material flow gates. These material flow gates can be moved, as indicated by straight dual-headed arrows. FIG. 1 illustrates the material flow gates in a position at which they do not restrict the first discharge line 6 for lumped carbonaceous material and/or the second discharge line 8 for hot iron carrier material. The illustration of a position at which they are partially pushed in, and therefore restrict the first discharge line 6 for lumped carbonaceous material or, as the case may be, the second discharge line 8 for hot iron carrier material, has been omitted for the clarity of illustration reasons. The lumped carbonaceous material 1 and the hot iron carrier material 2 are combined before they enter the melter gasifier 3 . For this purpose the first discharge line 6 for lumped carbonaceous material and the second discharge line 8 for hot iron carrier material open into an input device 10 for inputting material into the melter gasifier 3 .
[0056] Lumped carbonaceous material 1 and hot iron carrier material 2 are input into the melter gasifier via the input device 10 for inputting material into the melter gasifier. The input device 10 for inputting material into the melter gasifier 3 includes a dynamic distributing device 11 for distributing the material during the input, this being a gimbal-mounted chute in the illustrated case. The possible rotation of the gimbal-mounted chute is indicated by a curved dual-headed arrow which embraces the rotational axis of the rotational movement indicated by a dashed line. The pivoting movement of the gimbal-mounted chute is indicated by a curved dual-headed arrow. Lumped carbonaceous material 1 and hot iron carrier material 2 are distributed on the material bed 12 in the melter gasifier 3 in a controlled manner by the gimbal-mounted chute.
[0057] The ratio of the combined quantities of hot iron carrier material 2 and lumped carbonaceous material 1 can be varied. For this purpose a control device 13 is used to control at least one of the conveyor devices from the group
[0058] first conveyor device 7 for regulating the discharge of lumped carbonaceous material
[0059] second conveyor device 9 for regulating the discharge of hot iron carrier material
[0000] as a function of the position of the dynamic distributing device 10 . Toward that end, the control device 13 is connected to the dynamic distributing device 11 via the signal line 14 for the purpose of transmitting information relating to the position of the dynamic distributing device 11 .
[0060] For example, it is possible to determine the current position of the gimbal-mounted chute in relation to the circular arc that is described by the movement of the gimbal-mounted chute. The first conveyor device 7 , embodied in the form of a material flow gate, for regulating the discharge of lumped carbonaceous material 1 is controlled, via the signal line 15 , as a function of the position of the dynamic distributing device 10 .
[0061] The second conveyor device 9 , embodied in the form of a material flow gate, for regulating the discharge of hot iron carrier material 2 is controlled, via the signal line 16 , as a function of the position of the dynamic distributing device 10 .
[0062] Also provided is a device 17 for capturing properties of the surface of the material bed that has formed in the melter gasifier, the device taking the form of a radar measuring device with integrated temperature measuring device in the illustrated case. The radar measuring device collects information relating to height level and height profile of the material bed 12 in the melter gasifier 3 . The temperature measuring device collects information relating to the temperature profile at the surface of the material bed. The information relating to properties of the surface of the material bed that has formed in the melter gasifier is transmitted via the signal line 18 to the control device 13 for the first conveyor device for regulating the discharge of lumped carbonaceous material and/or the second conveyor device, where it is used to regulate the discharge of hot iron carrier material as a function of the captured properties.
[0063] In this way the ratio of the combined quantities of hot iron carrier material 2 and lumped carbonaceous material 1 can be set as a function of properties of the surface of the material bed.
[0064] Information relating to the run-off sequence that is followed during the operation of the melter gasifier can be transmitted to the control device 13 for the first conveyor device for regulating the discharge of lumped carbonaceous material and/or the second conveyor device by an information input device 19 which is connected for data transmission purposes via the signal line 20 to the control device 13 for the first conveyor device for regulating the discharge of lumped carbonaceous material and/or the second conveyor device. The ratio of the combined quantities of hot iron carrier material and lumped carbonaceous material can therefore be set as a function of the run-off sequence that is followed during the operation of the melter gasifier. The cited signal lines may be provided physically in the form of cables, although the possibility of wireless signal transmission is also included.
[0065] FIG. 2 shows a device for charging material, including lumped carbonaceous material 1 , this being represented by circles, and hot iron carrier material 2 , this being represented by squares, into a melter gasifier 3 of a smelting reduction plant. The device has two charging bins for lumped carbonaceous material, one charging bin 4 a for lumped carbonaceous material and one charging bin 4 b for lumped carbonaceous material. Lumped carbonaceous material 1 a having a lump size A is stored in the charging bin 4 a for lumped carbonaceous material, while lumped carbonaceous material 1 a having a lump size B is stored in the charging bin 4 b for lumped carbonaceous material. The lump sizes A and B are different, this being represented by circles of different sizes. The device for charging material also has a charging bin 5 for hot iron carrier material. A first discharge line 6 for lumped carbonaceous material emerges from the two charging bins 4 a / 4 b for lumped carbonaceous material, the first discharge line including a first conveyor device 7 for regulating the discharge of lumped carbonaceous material 1 . A second discharge line 8 for hot iron carrier material emerges from the charging bin 5 for hot iron carrier material, the second discharge line a second conveyor device 9 for regulating the discharge of hot iron carrier material 2 . The first conveyor device 7 for regulating the discharge of lumped carbonaceous material 1 and the second conveyor device 9 for regulating the discharge of hot iron carrier material 2 are embodied as screw feeders.
[0066] The lumped carbonaceous material 1 a / 1 b and the hot iron carrier material 2 are combined before they enter the melter gasifier 3 . For this purpose the first discharge line 6 for lumped carbonaceous material and the second discharge line 8 for hot iron carrier material open into an input device 10 for inputting material into the melter gasifier 3 .
[0067] Lumped carbonaceous material 1 a / 1 b and hot iron carrier material 2 are input into the melter gasifier 3 via the input device 10 for inputting material into the melter gasifier. The input device 10 for inputting material into the melter gasifier 3 includes a dynamic distributing device 11 for distributing the material during the input, this being a gimbal-mounted chute in the illustrated case. For clarity of illustration reasons, details of the gimbal mounting are not shown. The gimbal-mounted chute can be rotated about a rotational axis and adjusted in its inclination. The possible rotation of the gimbal-mounted chute is indicated by a curved dual-headed arrow which embraces the rotational axis of the rotational movement indicated by a dashed line. The adjustability of the inclination is indicated such that the outline of the gimbal-mounted chute is represented as a continuous line for one position and as a broken line for another position. The adjustability of the inclination is also indicated by a curved dual-headed arrow. Lumped carbonaceous material 1 a / 1 b and hot iron carrier material 2 are distributed on the material bed 12 in the melter gasifier 3 in a controlled manner by the gimbal-mounted chute. The movement pattern of the gimbal-mounted chute can be varied, describing e.g. circular or elliptical paths by different inclinations and therefore different resulting distributions on the material bed 12 .
[0068] As illustrated analogously in FIG. 1 above, the ratio of the combined quantities of hot iron carrier material 2 and lumped carbonaceous material 1 a / 1 b can be varied. For this purpose a control device 13 is used to control at least one of the conveyor devices from the group
[0069] first conveyor device 7 for regulating the discharge of lumped carbonaceous material
[0070] second conveyor device 9 for regulating the discharge of hot iron carrier material
[0000] as a function of the position of the dynamic distributing device 10 . Toward that end, the control device 13 is connected to the dynamic distributing device 11 via the signal line 14 for the purpose of transmitting information relating to the position of the dynamic distributing device 11 .
[0071] For example, it is possible to determine the current position of the gimbal-mounted chute in relation to its path of rotation, and its current inclination. The first conveyor device 7 , embodied in the form of a screw feeder, for regulating the discharge of lumped carbonaceous material 1 a / 1 b is controlled, via the signal line 15 , as a function of the position of the dynamic distributing device 10 . The discharge can be regulated by changing the rotational speed of the screw feeder, for example.
[0072] The second conveyor device 9 , embodied in the form of a screw feeder, for regulating the discharge of hot iron carrier material is controlled, via the signal line 16 , as a function of the position of the dynamic distributing device 10 .
[0073] Also provided is a device 17 for capturing properties of the surface of the material bed that has formed in the melter gasifier, the device taking the form of a radar measuring device with integrated temperature measuring device in the illustrated case. The radar measuring device collects information relating to height level and height profile of the material bed 12 in the melter gasifier 3 . The temperature measuring device collects information relating to the temperature profile at the surface of the material bed. The information relating to properties of the surface of the material bed that has formed in the melter gasifier is transmitted via the signal line 18 to the control device 13 for the first conveyor device for regulating the discharge of lumped carbonaceous material and/or the second conveyor device, where it is used to regulate the discharge of hot iron carrier material as a function of the captured properties. In this way the ratio of the combined quantities of hot iron carrier material 2 and lumped carbonaceous material 1 can be set as a function of properties of the surface of the material bed. The opening mechanism of the charging bin 4 a for lumped carbonaceous material can be activated by the control device 13 via the signal line 21 , and the opening mechanism of the charging bin 4 b for lumped carbonaceous material can be activated by the control device 13 via the signal line 22 . This activation allows the lump size of the lumped carbonaceous material to be selected as a function of the position of the dynamic distributing device. The opening mechanism of the charging bin 5 for hot iron carrier material can also be activated by the control device 13 , though for clarity of illustration reasons this is not shown here. The cited signal lines may be provided physically in the form of cables, although the possibility of wireless signal transmission is also included.
[0074] In a similar manner to the illustrated possibility of selecting the lump size of the lumped carbonaceous material as a function of the position of the dynamic distributing device, the type of lumped carbonaceous material can be selected as a function of the position of the dynamic distributing device if lumped carbonaceous materials 1 a and 1 b are of different types.
[0075] If provision is similarly made for two charging bins 5 for hot iron carrier material, these being filled with hot iron carrier material of a different grain size distribution and/or different type in each case, the grain size distribution and/or the type of the hot iron carrier material can be selected as a function of the position of the dynamic distributing device in a similar manner to the lumped carbonaceous material.
[0076] A device 23 is provided for regulating the distribution track which is realized during the input by the dynamic distributing device for distributing the material. This is illustrated schematically and works by influencing the drive mechanism of the dynamic distributing device 11 or by influencing those plant parts which are responsible for the inclination of the distributing device 11 .
[0077] By varying the distribution track over the horizontal cross-section of the interior of the melter gasifier, it is possible to set specific distribution patterns of hot iron carrier material and lumped carbonaceous material in the melter gasifier. The device 23 for regulating the distribution track which is realized during the input by the dynamic distributing device for distributing the material is connected via the signal line 24 to the control device 13 for controlling at least one of the conveyor devices from the group
[0078] first conveyor device for regulating the discharge of lumped carbonaceous material
[0079] second conveyor device for regulating the discharge of hot iron carrier material
[0000] as a function of the position of the dynamic distributing device.
[0080] Since the realized distribution track is determined by the position of the dynamic distributing device, the control device 13 also constitutes a device for controlling the first conveyor device for regulating the discharge of lumped carbonaceous material, and/or the second conveyor device for regulating the discharge of hot iron carrier material, as a function of the distribution track 23 which is realized during the input by the dynamic distributing device for distributing the material. A specific distribution pattern of hot iron carrier material and carbonaceous material can therefore be set in the melter gasifier. This device can be used to control the material flow gates and/or the screw feeders, for example.
[0081] Although the invention has been illustrated and described in detail with reference to the exemplary embodiments, the invention is not restricted by the examples disclosed herein, and other variations may be derived herefrom by a person skilled in the art without thereby departing from the spirit and scope of protection of the claims which may include the phrase “at least one of A, B and C” as an alternative expression that means one or more of A, B and C may be used, contrary to the holding in Superguide v. DIRECTV, 358 F3d 870, 69 USPQ2d 1865 (Fed. Cir. 2004).
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A melter gasifier of a smelting reduction installation is charged by bringing together coal-containing material in lump form and iron carrier material (which may be hot) before and/or while they enter the melter gasifier. The ratio of the combined amounts of iron carrier material and coal-containing material in lump form is variable. The combined amounts of iron carrier material and coal-containing material in lump form are distributed over the cross section of the melter gasifier by a dynamic distributing device, and the ratio of the combined amounts of the iron carrier material and coal-containing material in lump form is set depending on the position of the dynamic distributing device.
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TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method and apparatus for the storage and delivery of ultra pure gases for, inter alia, semiconductor processing. In particular, the present invention provides a system that maintains an elevated pressure in a bulk storage vessel without compromising the product's ultra high purity.
BACKGROUND OF THE INVENTION
In order to avoid defects in the fabrication of semiconductor devices, semiconductor manufacturers require high purity gases and chemicals for their production processes. Typical processing steps include using cleaning solvents for initial wafer preparation, wet etching, chemical vapor deposition, and the like. The presence of very minute amounts of impurities at any one step may result in contamination of the wafer and ultimately in the scrapping of the chip.
Two sources of impurities that result in wafer contamination include particulates and films. Particulates include any bits of material present on a wafer surface that have readily definable boundaries. As state of the art mask designs commonly have line widths in the sub-micron range, particulates may very easily interfere with the proper operation of the chip circuits. This is especially true in the case of charged particles, which may interfere with the electrical characteristics of the chip. Film contamination results when a layer of a foreign material remains on a chip after a processing step. Solvent residues and oils are common films that undesireably remain on a chip, cause contamination and ultimately reduce wafer yields. Additionally, the presence of heavy metals such as Fe, Ni, Cr, Cu, Al, Mn, Mo, Zn, and the like may contaminate a wafer as either a metallic film or as metallic particulates. As a means to increase yields, semiconductor fabrication houses (fabs) commonly require that their process gases meet particle specifications of less than 0.2 micron, and metals specifications on the order of 1 part per billion or less. By understanding the extremely sensitive nature of chip fabrication, one may appreciate why labs maintain such stringent purity standards for their wafer processing gases and chemicals. One may further anticipate that such standards will become more stringent in the future, as the geometry of semiconductor devices continues to get smaller.
Traditionally, semiconductor manufacturing facilities or fabs as they are referred to in the industry have used electronic grades of process gases which producers have supplied in cylinders. The cylinders contain gas volumes on the order of 40 litters and are installed in gas cabinets, which contain one or two process gas cylinders per station. The gas cabinets are maintained in a controlled temperature environment such that the vapor pressure of liquefied compressed gases may be controlled. In order to meet the ever increasing demands for semiconductor chips, labs have installed more gas cabinets. The increased number of gas cabinets has consequently challenged the user in regard to operational safety, as cylinder changes become more frequent and there is increased likelihood of component failure. Of course the increased operational and maintenance requirements also increase the likelihood that impurities may be introduced into process gas streams. Furthermore, such an approach to maintaining production is undesirable from an economic standpoint, as the need for identical delivery systems and components increases capital equipment, installation, and operational costs.
As an alternative to the above described method of delivering process gases, users of large volumes of liquefied compressed process gases have met flow demands by pumping liquid product from a storage vessel and vaporizing it prior to use. The advantage of this technique being that the pump enables a user to pressurize the delivery system according to process needs. While this method is straight forward for large volume, low purity users, the process becomes more complicated for large volume high purity users, such as the semiconductor industry. Experimental results have shown that chemical withdrawn from the liquid phase of a storage vessel contains substantially higher levels of metallic and oil contaminants than chemical that is withdrawn from the vapor phase of a storage vessel. When the withdrawn liquid is vaporized, the flow stream carries the impurities into the vapor stream to the point of use. Consequently, high purity users such as labs would have to rely on purifiers to remove the contaminants.
U.S. Pat. No. 5,242,468 discusses the problems in the semi-conductor industry and puts forth a proposed on-site solution for purifying chemicals for use in a semi-conductor fabrication house.
U.S. Pat. Nos. 4,579,566; 4,961,325 and 2,842,942 disclose methods and devices for maintaining pressurization of a cryogenic storage vessel. The 566' and '325 patents utilize vaporization of stored liquid to pressurize the vapor space in a cryogenic storage vessel. The '942 patent vaporizes cryogenic liquid using heat exchangers that provide ambient heat to vaporize the cryogen and heat exchange it with the liquid supply of the cryogen to maintain pressure. It is known to supply gaseous hydrogen from a liquid cryogen hydrogen supply by this method.
From the above discussion, it becomes clear that the semiconductor industry requires an improved technique to deliver ultra pure gases to their manufacturing processes using an operationally safe, cost effective bulk source and delivery system. Such a system must be able to maintain a minimum delivery pressure defined by the user.
SUMMARY OF THE INVENTION
In order to satisfy the need for a safe and cost effective bulk source and delivery system the present invention provides a method and apparatus for delivering ultra high purity process gas from a storage vessel containing a large quantity of non-cryogenic liquid chemical product where the chemical has at least a vapor phase and a liquid phase. Vaporized product is withdrawn from the top of the storage vessel, the vapor having a lower concentration of impurities than the compressed liquid phase. Vapor withdrawn from the tank is heated with a source of heat providing heat in excess of available ambient heat and passed in heat exchange relationship with the pool of non-cryogenic liquid to promote further vaporization of product inside of the tank. The withdrawn vapor is circulated through the pool of product for a period of time and for a number of cycles required to maintain a minimum pressurized condition inside of the vessel. During periods that the user has no need for product, the vaporized product can be withdrawn and vented through an abatement system to maintain the storage vessel under suitable pressure. Process engineering for specific installations will be influenced by the properties of the fluid being delivered, the ambient temperature, the storage vessel's heat transfer characteristics, use requirements for withdrawn product, and the pressure level desired inside of the storage vessel.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a schematic representation illustrating the method and apparatus of the present invention.
FIG. 2 is plot of mass flow against a quantity α, for various numbers of passes through the heat exchanger where α represents the heat transfer characteristics of the storage vessel for an ammonia system.
DETAILED DESCRIPTION OF THE INVENTION
The present invention permits delivery of ultra high purity (UHP) process gas in bulk quantities for use by semiconductor manufacturing facilities. The requirement for large quantities of ultra pure chemicals by semi-conductor manufacturing facilities results from processing wafers of larger diameters coupled with more stringent purity requirements. Process gases that may be delivered by the invention include NH 3 , HF, SiHCl 3 , SiH 2 Cl 2 , C 4 F 8 , C 3 F 8 , and the like. Ultra high purity gases for the electronics industry typically have less than 1 part per billion (ppb) by volume of contaminants to which the end uses are sensitive, such as metals like aluminum, boron, iron, nickel, silver and the like.
The present invention is directed to non-cryogenic liquid products which can be vaproized to gaseous products using an external heater providing heat in excess of the heat available from the ambient environment. Cryogenic liquids, those liquefying at or below -90° F., may be vaporized by merely adding heat from the ambient to reach acceptable delivery pressures. Acceptable delivery pressures vary for each product and the end user demands, but for ammonia a delivery pressure of at least 50 psig, preferably 75 psig, most preferably 100 psig is required.
Referring to FIG. 1, the system shown generally as 10 includes a storage tank 12 supported on a rack, cradle, or supports 14 as is well known in the art. Tank 12 includes a fill conduit 16 with a check valve 18 and a control valve 20 to permit liquid product 22 to be introduced into the tank. Tank 12 also includes a vent conduit 32 which in turn is connected to a system 33 to vent over pressurization of the tank 12.
Tank 12 includes a vapor withdrawal conduit 34, a vapor withdrawal valve 36, and conduit 38 which in turn is connected to a check valve 40. Check valve 40 delivers the withdrawn vapor into a conduit 46, which in turn delivers the withdrawn vapor to a multiple pass heater 48. The multiple pass heater 48 provides heat in excess of that available from ambient conditions. This could be an electric heater, a fuel fired heater or any type of heater capable of providing heat in excess of ambient conditions, including heat imported from an adjacent industrial process. Safety relief valve 44 is connected to conduit 46 and prevents over pressurization of the withdrawal system. From multiple pass heater 48 vapor passes through conduit 50 into a multiple-pass heat exchanger 52 disposed in the liquid bath 22. Multiple pass heat exchanger 52 delivers the vapor to a conduit 54 which exits the tank 12 to deliver the process gas flow to a product delivery valve 56 and then to a point of use represented by arrow 58. Pressure indicating controller 60 is disposed in conduit 38 so that when a predetermined pressure is indicated in the vapor space 62 of tank 12, heater 48 will be turned off to prevent over-pressurization of tank 12. A second vent conduit 64 communicates with the vapor space 62 in tank 12. Conduit 64 is connected to a second pressure indicating controller 66 which has a preset value. Pressure indicating controller 66 is in turn connected to a control valve 68, which in turn is connected to a vent 70, which in turn is connected to the abatement system for the tank 12. The abatement system (not shown) can include a scrubbing system or any other system or receptacle for safe disposal of vented chemicals. Conduit 64 includes a branch conduit 72 with a pressure control valve 74, check valve 76, and control valve 78, between the vent conduit 64 and the delivery conduit 54. Control valve 74 in conjunction with check valve 76 will prevent undesired product venting through control valve 68. The vent conduit 64, pressure indicating controller 66, valve 68, valve 78, and conduit 80, coupled with heater 48, conduit 50, heat exchanger 52, and conduit 54 comprise a unique pressure maintenance system for the ultra high purity process gas in tank 12.
The method and apparatus of the invention illustrated in FIG. 1 can be applied to a storage vessel of any size. In operation, tank 12 will deliver ultra high purity gaseous product through the vapor delivery valve 36. The vapor or gaseous product is heated by means of electric heater 48 and forced through the tube bundle or multiple pass heat exchanger 52 contained inside of the tank 12 in the liquid product 22. Heating of the liquid product 22 by the vapor circulating through the multiple pass heat exchanger or tube bundle 52 will continue to generate ultra high purity vapor above the liquid surface 23 in the vapor space 62 of tank 12. This will maintain a constant tank pressure. As long as the pressure indicating controller 60 does not sense that the pressure inside the tank has exceeded the pre-set pressure limit, the heater will continue to heat the process gas as it is withdrawn from the tank through conduit 54.
According to the process of the present invention, in order to maintain a certain minimum delivery pressure, the equilibrium of vapor and liquid product inside the tank (storage container) 12 must remain above a corresponding minimum bulk temperature. During gaseous flow of product to the customer's house line through conduit 54, the loss of energy in the tank 12 is balanced by the amount of energy added using the external heater 48 and the amount of heat transfer into or out of the system, which is dependent upon the ambient temperature. When the ambient temperature is equal to the specified minimum bulk temperature of the fluid in the tank, no heat transfer will take place. Therefore, the heater 48 is the only source of energy to replace the energy loss due to product flow out of the tank. As the ambient temperature drops below the minimum specified bulk temperature of the product in the tank 12, the heater duty will increase. Depending on the heat capacity of liquefied gas, it will be necessary to use a multiple pass heat exchanger containing a number of passes designated "n" in order to compensate for the vapor loss. During unsteady conditions, such as fluctuating product usage by the customer, temperature of gas inside the tube bundle may rise rapidly due to a sudden no flow condition. Pressure rise in the tube bundle due to a rapid temperature rise will be dampened or relieved by pressure control valve 74, which will recycle the vapor into the tank 12 where any extreme condition of over pressurization can be handled by the normal tank vent system (not shown). In the event there is no demand for vapor product by the customer and a cold ambient temperature causes the tank pressure to fall below the minimum delivery pressure, pressure indicating controller 66 will automatically open vent valve 68 to allow a sufficient flow of vapor product through the heater 48 to heat the liquid product by passing gaseous product through heat exchanger 52 to heat and vaporize liquid product and raise the pressure of the gaseous product in the vapor space 62, thereby elevating the tank pressure above the minimum allowable level. In the event excess pressure is generated by overshooting the pressure set point for the tank 12, the gaseous product can be delivered through pressure control valve 74 to assist in maintaining tank 12 pressure. The overall process energy balance can be expressed by the equation:
Q.sub.h +Q.sub.c +Q.sub.r =m h.sub.v +dU.sub.cv (1)
where
Q h =Heat gain in tank provided by heater
Q c =Heat gain(+) or loss(-) in tank due to convection to atmosphere
Q r =Heat gain(+) or loss(-) in tank due to radiation to atmosphere
m=Mass flow rate of gas product out of the tank
h v =Enthalpy of saturated vapor at tank pressure
dU cv =Change in internal energy of the tank
The heat terms may be represented as follows:
Q.sub.h =n m C.sub.p dT.sub.htr (2)
Q.sub.c =U.sub.o A (T.sub.o -T.sub.tank) (3)
Q.sub.r =σεA(T.sub.o.sup.4 -T.sub.tank.sup.4)(4)
where
n=Number of heat exchange passes
C p =Specific heat of gas product at the tank pressure and temperature
dT htr =Temperature increase of the gas through the heater
U o =Overall convection heat transfer constant for the tank
A=Surface area of the tank
T o =Ambient temperature in absolute scale
T tank =Bulk gas temperature in the tank in absolute scale
σ=Stephan Boltzmann constant
ε=Tank emmissivity constant
Using the above equations in conjunction with system design data, one may determine the minimum number of heat transfer tube passes that is required to maintain a designated tank pressure according to: ##EQU1## Based on this equation, there are three parameters that control what the value of n will be for a given fluid, namely, (a) the tank pressure, (b) the mass flow rate of the gas product, and (c) the heat transfer terms. The tank pressure is important as it directly affects the values for the enthalpy of the exiting vapor and the change in internal energy of the system. Assuming a constant tank pressure, the value of the vapor enthalpy remains constant, and the change in the tank's internal energy is directly proportional to the mass flow rate of the gas. The heat transfer terms from equation (5) may be collected and represented by a quantity α, where ##EQU2## The quantity α represents the amount of heat lost by the tank (due to radiation and convection) relative to the heat gained by the tank. Since the value of α includes the specific heat of the process gas, the equation is universal in that it will apply for any liquefied compressed gas. Accordingly, one may plot lines for each n number of passes on a graph of mass flow rate versus quantity α at constant pressure, as shown in FIG. 2 for an ammonia system where the tank has an 8500 gallon capacity and an operating pressure of 80 psig.
The graph shown in FIG. 2 represents the operating characteristics of an NH 3 system where the number of heat exchange passes varies between three and eight. One can see that for a given mass flow rate, the system will need an increasing number of passes for increasing values of α. Or in other words, as the ratio of heat lost to heat gained by the tank increases, the imbalance may be offset by adding more heat exchange passes in the tank. Conversely, for a constant value of α, an increasing flow rate requires fewer heat exchange passes to maintain pressure. This is because a higher flow rate makes more heat available for heat exchange in the tank to replace the heat lost due to convection and radiation. Since more heat per pass is available, and the total heat required is fixed (because α is fixed), the number of required passes decreases. A system will operate satisfactorily provided it is running at any point below the line representing the number of active heat exchange passes in the system. If the system is running substantially below that line, one may save operating expenses by decreasing the value of dT htr , which would serve to increase α and thus, run the system at a point closer to, but still below, the line representing the active number of heat exchange passes.
The method and apparatus according to the invention will be advantageous to users of high purity compressed liquefied gases for several reasons. First, by permitting delivery of ultra pure gas in bulk quantities, the invention eliminates the need for a large fab to maintain numerous cylinders and gas cabinets, which will minimize the number of components (e.g., valves, regulators, instruments, fittings, etc.), reduce equipment cost, reduce product cost, and reduce operating labor by eliminating numerous cylinder changes. The invention further eliminates equipment cost by eliminating the need for a purifier. Next, unlike a conventional pressure building circuit that vaporizes liquid and reinjects it into the vapor space of the vessel, the invention will maintain separation of vapor and liquid spaces at all times. This separation will enable the impurity concentration in the vapor space to be continually lower than that in the liquid space. Finally, since the process gas is used as the heat exchange media, any mechanical problems associated with the heat exchange tubes will not compromise the purity of the product, as would be the case if any other heat exchange fluid were selected.
The present invention is advantageous for fabs in another use. Traditionally, fabs have used large quantities of aqueous chemicals, such as ammonium hydroxide, as cleaning agents. Such chemicals are purchased in drums, and then pumped from a central storage and handling facility to the process application. As wafer diameters and production requirements continue to increase, fabs require larger volumes of the aqueous chemical products, which presents higher costs associated with transport and storage of the chemicals. The aforementioned invention will enable fabs to deliver sufficient quantities of ultra pure process gas at required pressures for on-site mixing with ultra pure water, to produce ultra pure aqueous chemicals such as ammonium hydroxide, in concentrations and volumes specific to the various semiconductor processing steps. In this regard, the production, storage, and delivery of the aqueous chemical is more controllable, and less susceptible to introducing impurities into the semiconductor manufacturing process.
Having thus described the invention, what is desired to be secured by Letters Patent of the United States is set forth in the appended claims.
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A method and apparatus for storing ultra high purity non-cryogenic liquefied compressed gases, such as ammonia (NH 3 ), and delivering a vaporized gaseous product from those liquefied gases for semiconductor processing applications. The delivery method includes withdrawing and heating gaseous product from a storage vessel containing the liquefied compressed gas, and then piping the heated gas through the liquid contained in the storage vessel in a heat exchange fashion. The heat exchange with the liquid inside the vessel induces boiling to maintain a vaporized gaseous product under a minimum positive pressure in said vessel. After liberating its heat, the gaseous product is delivered to a semiconductor manufacturing point of use.
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BACKGROUND
1. Field of the Description
The present invention relates, in general, to devices and methods for providing a three-dimensional (3D) display in a glasses-free manner, and, more particularly, to a 3D display device using content-adaptive lenticular prints and using a non-uniform lens pattern (e.g., non-uniform lenticule configuration) in the lenticular sheet (or lens array, lenticular print, or the like) to display the printed content (e.g., interlaced content provided in a planar sheet or in a non-planar arrangement when the lenses/lenticules are arranged in a non-planar configuration).
2. Relevant Background
Displays that provide the illusion of three dimensions have experienced a rebirth in the past few years. For example, lenticular displays (sometimes called lenticular prints) are a popular medium for producing automultiscopic, glasses-free 3D images. A typical lenticular display includes a lens array or lenticular sheet of lenticules or lenslets for viewing interlaced images in printed content under the lenslets. The images emitted from the lenticular sheet are offset in a way that is perceived by a viewer as a 3D image, and the 3D image changes with movement of the viewer to a new position or by movement of the lenticular display.
While most commercial displays rely on the use of special glasses, it is generally agreed by those in the industry that automultiscopic displays, i.e., displays able to provide 3D vision without glasses or headgear, offer significant advantages. The predominant automultiscopic technology presently in use (e.g., the technology behind lenticular displays) is based on parallax-type displays, which create the illusion of three dimensions by physically separating viewing rays coming from the displays. The ray separation is often achieved by placing tiny lens arrays in front of a display surface (e.g., interlaced printed content or images). However, these lenticular lens arrays are always arranged on a regular grid with the lenslets or lenticules being uniform in cross sectional shape and arranged in a plane to accommodate the maximum possible depth. Unfortunately, 3D scenes often do not cover all depth ranges throughout the scene, and local patches of the scene are not effectively presented by such displays.
Work and research has been performed to improve the quality of lenticular display devices. Most work has concentrated in areas such as integral imaging, parallax barrier-type displays, and multi-layer light field displays. Some improvements have been obtained such as with increased resolution and depth of field, but none of these efforts has been optimized for a given scene, which has led to sub-optimal results. Therefore, there remains a need for an improved lenticular display device or apparatus that more effectively displays a wide variety of captured scenes or display content (e.g., that does not use a one-size (or one lenticular lens array) fits all content-type design).
SUMMARY
A content-adaptive lenticular display device or apparatus (also called a lenticular print herein) is provided to provide enhanced glasses-free 3D images. It was recognized that traditional lenticular displays utilized lenticular sheets with uniform lenticules or lenslets, and these traditional lenticular devices emitted a light field that had a fixed spatial and angular resolution. Hence, prior lenticular devices were designed based on a trade-off between spatial resolution and angular resolution that was defined by the width of the individual lenslets as well as the number of pixels underneath each of the lenslets (e.g., size of each interlace of the underlying printed image).
The lenticular display devices described herein are effective in increasing both perceived angular resolution and spatial resolution. These desirable results are achieved by modifying the lenslet array to better match the content of a given light field. An optimization algorithm or method (which may be implemented with software run on a computing device) is described by the inventors that analyzes an input light field and computes an optimal lenslet size, shape, and arrangement of sets of lenslets across the width of the array to better (or even best) match the input light field given a set of output parameters. The resulting lenticular display device (or print) shows higher detail and smoother motion parallax compared with fixed-size lens arrays. The usefulness of these content-adaptive lenticular prints has been demonstrated or proven using rendered simulations, by generating 3D-printed lens arrays according to the present description, and with user studies.
The content-adaptive lenticular prints or display devices introduced by the inventors may be thought of as providing a static display method that uses a modified lens array, which is optimized for a given static input light field (e.g., by use of differing lens configurations in differing portions of the lens array and by placing the lenses/lenticules in differing planes). The described approach was motivated, in part, by the observation that light fields generated from real world scenes often show locally varying angular and/or spatial frequency content. Therefore, it was recognized that a regular lenticular arrangement using a single type of lenticule or lenslet often cannot reproduce such real world light fields efficiently, and it was further understood by the inventors that parts of these light fields could be better represented by using different lens sizes and arrangements by exploiting the varying frequency content.
Content-adaptive lenticular prints are achieved by computing an optimal arrangement of different lens (or lenslet, lenticule, or the like) sizes based on an analysis of an input light field. For example, a discrete optimization algorithm may be applied to distribute a precomputed set of lenslets according to the angular frequencies and spatial frequencies of the input light field. The optimization algorithm may then generate a lenticular print supporting horizontal parallax with improved angular and spatial resolution. In addition to the distribution algorithm, an optimal set of input lenses may be determined given specific manufacturing limits. Furthermore, additive 3D multi-material printing technology may be used or employed to produce a lens array with content-adaptive lenslets for use in a lenticular display device/apparatus of the present description. Using such 3D printing, general-purpose lenticular display features may be introduced or provided in the lenticular display device such as view blockers (e.g., using baffles), a non-planar projection surface or interlaced content layer, and/or oriented lenslets for better field of view usage. Again, the improved reproduction quality achieved with these techniques has been demonstrated with simulated results as well as proof-of-concept physical prototypes that were manufactured using an additive, multi-material 3D printer.
More particularly, a content-adaptive display apparatus is provided that includes a content layer (e.g., a printed image) including a plurality of images (e.g., interlaced images when the display is a lenticular device). The apparatus also includes a lens array overlying the content layer, wherein the lens array comprises a first set of lenses each with a first width and a second set of lenses each with a second width differing from the first width. In other words, the lens array does not contain uniformly sized and arranged lenses.
In some cases, the content layer has first and second portions with first and second angular frequencies, and the second angular frequency differs from the first angular frequency and the second spatial frequency differs from the second spatial frequency. In such cases, the first set of lenses is aligned with the images in the first portion and the second set of lenses is aligned with the images of the second portion, whereby the first and second widths are matched to the content layer (e.g. to provide content-adaptive lens configurations). The first angular frequency may be greater than the second angular frequency; then, the first width would be greater than the second width. In the same or other cases, the first spatial frequency may be less than the second spatial frequency; then, the first width would also be greater than the second width to improve the display's resolution.
In some implementations, the content layer is non-planar, and each of the lenses has a back surface adjacent to the content layer, whereby a projection surface defined by the back surfaces is non-planar. Further, in such cases, each of the lenses may have a front edge (or lens surface), and the front edges may be aligned to be co-planar. Additionally, in some embodiments of the display apparatus, a plurality of field-of-view baffles may be provided and sandwiched between adjacent pairs of the lenses, whereby cross-view zone artifacts are reduced in the display apparatus.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates schematic, partial end views of two conventional lenticular display devices with uniform and planar lenslets or lenticules for displaying a sampled light field;
FIG. 2 illustrates frames of an input scene along with a corresponding image of one line of this input showing differing angular and spatial frequencies in this input content that may be used with a lens array of a lenticular display device;
FIG. 3 is a functional block diagram of a system for use in designing a lenticular display that is content-adaptive;
FIG. 4 is an end view of a lenticular display device (lenticular print) with a planar content layer (or back plane);
FIG. 5 is an end view of a lenticular print with a non-planar or irregular content layer or projection surface and with a lens arrays with front edge/lens surfaces aligned or coplanar; and
FIG. 6 illustrates graphically a discrete light field optimization method of one embodiment.
DETAILED DESCRIPTION
Briefly, the present description is directed toward content-adaptive lenticular display devices (or prints) configured to better cover all or more depth ranges throughout a selected input scene (content or input static light field). The display devices differ from conventional lenticular devices in that the lenticules differ in size across the width of the lens array such that sets of lenticules can be provided to suit the differing content across a scene. Further, the lenticules may also be non-planar such as with the back planes or surfaces of the lenticules being in two, three, or more parallel but offset planes with the content printed or provided on or adjacent to these back planes/surfaces (e.g., the content or interlaced image layer also being non-planar).
Prior to describing the new content-adaptive lenticular prints, it may be useful to explain conventional lenticular display devices and their operation. The following provides a summary of the principles of automultiscopic displays based on lenticular lens arrays, with the assumption that each lens or lenticule is modeled using a perfect pinhole.
FIG. 1 illustrates first and second lenticular displays 110 , 130 each with a plurality of uniform lenses or lenticules (or a lens array) in arrays 112 , 132 with an image pattern or layer 114 , 134 located at the planar, back surface of the lenses in arrays 112 , 132 so as to be located at the focal planes of these lens arrays 112 , 132 . Different viewing directions are multiplexed to different pixels on the image plane, giving rise to an automultiscopic display.
The (u,s) sampling patterns 120 , 140 (or 2D light field) of these lenslet arrays 110 , 130 are shown adjacent the arrays 110 , 130 . The width w of the lens defines its extent in the spatial (s) domain. The focal length f and width w define the field of view of the lens, which in turn defines the angular (u) support. Note, the sampling pattern will get increasingly dense in angular direction at the cost of trading it against spatial resolution when keeping the field of view constant.
FIG. 1 may be thought of as showing one line of lenticular displays 110 , 130 , with different viewing directions being angularly multiplexed through the lenses of arrays 112 , 132 and being mapped to different pixels on the image planes or planar image layers 114 , 134 . An observer (not shown) at some distance from the lens arrays 110 , 130 will, therefore, see different pixels for different positions along the horizontal axis and will perceive motion parallax as well as stereoscopic depth cues. The lens arrays 110 , 130 emit output light fields that can each be characterized by a spatial and angular pattern (s,u), as shown in FIG. 1 . The spatial sampling domain is denoted by s, and the angular domain is denoted by u. The angular sampling points are defined relative to their respective spatial sampling points. In other words, s denotes the origin of the ray, whereas u describes the direction of the emitted ray.
Using this definition, each lens in arrays 112 , 132 defines a spatial sampling location and emits multiple angular samples from the display planes 114 , 134 , as shown in FIG. 1 . The spatial sampling density is defined by the lens width w, whereas the angular sampling density is characterized by the focal length f and underlying pixel density Δc. Each column in the (u,s) plots 120 , 140 denotes one lens in arrays 112 , 132 , and each row denotes a set of parallel rays. The exact sampling densities can be arbitrary but are often bound by the possible resolution of the display surface as well as the optical qualities of the employed lenses.
FIG. 1 shows two different configurations with display devices 110 , 130 , assuming a constant density on the display surfaces 114 , 134 as well as a constant field of view. As can be seen in FIG. 1 , increasing the width of the individual lenses in arrays (from array 132 to array 112 ) increases the number of angular samples and subsequently allows the support of more angular variation. However, the increased angular resolution comes at the cost of a reduced spatial resolution in display device 110 compared to device 130 . Unfortunately, this is a fundamental trade off for conventional lenticular and parallax barrier-based displays, such as those shown in FIG. 1 .
As can be seen from the above discussion, prior or conventional lenticular displays were based on regular (u,v) sampling patterns. However, the local angular and spatial frequencies of natural light fields often differ considerably, and, as a result, many of the (u,v) samples are often either wasted or not optimally placed for a given light field content with a uniform lens configuration-type lens array.
For example, FIG. 2 illustrates three frames or images 210 , 214 , 218 of an input scene. The local angular and spatial frequency content of the light fields differs considerably in these frames 210 , 214 , 218 . This can be seen with the frequencies for one line of the input light field as shown with epipolar plane image (EPI) representation 220 . In the frames 210 , 214 , 218 , the background wall 211 is positioned approximately at the focal plane of the display, and the two images/objects (foreground objects) 212 float at different distances in front of the focal plane or wall 211 . As can be seen in EPI representation 220 , the angular frequencies of the wall 211 are very low while its spatial frequencies are very high, as shown with high spatial, low angular regions/portions 222 , 226 of EPI representation 220 . In contrast, the foreground objects (apples, in this example) 212 features or provides high angular frequencies at low or moderate spatial frequencies, as shown with low spatial, high angular region/portion 224 of EPI representation 220 .
In the example of FIG. 2 , the wall 211 is located right at the focal point such that the angular frequency content at each point on the wall is low. In other words, all viewing directions see the same color. However, the spatial frequency content is high (i.e., the wall 211 is textured). The objects in front of the focal plane (and the wall 211 ) require much less spatial frequency and much more angular frequency due to their distance from the display.
The following insight, hence, motivated the inventors: while objects close to the display would ideally have lenses with low angular variation (e.g., lens width of one pixel or the like), objects further away from the display plane would benefit from larger lenses. Therefore, the inventors determined that is would be useful to have lenticular display devices with lens arrays in which the lenses are adjusted “locally” in the array in order to better replicate the input light field. This can be achieved, in some embodiments, by distributing lenses (or sets of lenslets/lenticules) of varying size in conjunction with optimizing the image pattern, such that the light field emitted from the display device generates the least error compared to the input light field. With this in mind, the following paragraphs describe a discrete optimization method or process for generating an adaptive lens distribution. Then, the description turns to a discussion of a strategy/process for finding optimal shapes for the individual lens elements/lenticules in a lens array.
With regard to discrete light field optimization, one goal of the discrete optimization is to find a lens distribution for a lens array that generates an output light field l out that matches an input light field l in as closely as possible. More formally, the discrete light field optimization algorithm or method finds the optimal lens distribution such that:
L O =min L (norm(l in ,l out (L))) (Eq. 1)
where L O ={l i |=1 . . . n} denotes the optimal lens distribution, and norm( ) can be any appropriate norm, e.g., L 2 or gradient based. Each lens l i ={w i , c i , f i } may be characterized by its width w i , the color content of the back surface c i , and the focal length f i .
The optimization may be restricted to a pre-defined discrete set of widths that are possible (or practical) for a given manufacturing process. The field of view of all lenses and the resolution of the color content are kept constant across the whole display. As a result, the angular resolution of a lens increases with its width w i .
Solving for the optimal distribution given a discrete set of lenses is a packing problem, similar to the knapsack problem. In the discrete optimization cases, however, the weights are not known a priori, as each lens will result in different error terms for a given light field. Therefore, one technique is to use a bottom-up dynamic programming approach to find an optimal distribution L O for an input light field l in . Briefly, an algorithm/method may place a candidate lens/lenticule and then recursively determine the best solution for the remainder of the light field. In some embodiments, the optimization involves only solving for horizontal parallax, and, therefore, the algorithm/calculation method can be evaluated independently on single scanlines.
In each recursion step, all possible lenses from a discrete set of candidates are placed on one side of the input light field. Then, the same procedure is evaluated recursively on the remaining subset of the light field not covered by the lens. The recursion stops as soon as the width of the remaining subset is equal to or smaller than the smallest candidate lens. Then, the error induced by the current lens placement is propagated up and in each stage of recursion the lens arrangement with the lowest error is selected. The following pseudo-code summarizes the optimization algorithm (Algorithm 1: e=computeLensDistribution(l in )):
for all possible candidate lenses l i e i = error(l i ∩ l in ) + computeLensDistribution(l in \l i ) return lens l i with lowest error e i
The error that a lens incurs follows the same metric as defined in Eq. 1, but it is computed only over the subset of the light field covered by the lens. Therefore, Algorithm 1 provides an optimal solution for Eq. 1.
As shown in FIG. 1 , each lens covers a number of spatial and angular samples from the input light field, and the input samples should be resampled at the spatial-angular samples of the lens. A box filter may be employed according to the output sampling width, and, as a result, each pixel u on the display surface is computed from the mean color of the input rays covered by each output sample. When employing an L 2 norm, the squared difference between the color of the input rays and output rays defines the error between input and output light fields, for a given lens placed at one position.
With regard to spatial weighting versus angular weighting, the L 2 error described in the previous paragraph can directly be computed in the light field domain. However, the angular and spatial dimensions can be reweighted in some embodiments if desired. Instead of computing a 2D box filter along both dimensions, the angular and spatial errors can be computed individually and then combined using a spatial-angular weighting factor. This way, the surface generation can be steered to either focus on reproducing the angular variation or on reproducing spatial variation. In some embodiments or implementations produced by the invention, both dimensions were weighted equally (but this is not required to practice the invention).
Regarding multi-scanline solves, the discrete light field optimization algorithm described above computes the optimal lens distribution for each scanline individually, which can lead to spatial noise along otherwise crisp edges. This can be mitigated by choosing similar lenses in neighboring scanlines. To this end, this algorithm can be extended such that a sliding window of multiple scanlines is used to compute the lens arrangement for each particular scanline. This allows an increase in smoothness at a small overhead in computational cost.
Turning now to lens optimization, an appropriate set of candidate lenses (or lenticules or lenslets) is determined before the full surface is generated in order to generate the desired lens arrangement computed using the discrete light field optimization algorithm. Given a minimum lens size for a lens array of a lenticular display device and a target display resolution, a first step may be to optimize for lenses of the desired widths. In general, lenticular lenses or lenticules are formed by combining 1D cylindrical lenses with a planar back surface. While multi-lens systems are possible, the resulting manufacturing complexity is inhibitive for practical systems, as well as for automatic printing. Therefore, the inventor determined it may be useful to employ plano-convex lenses, and search for lenses that result in the best focusing quality across all views for a given overall field of view. While analytical solutions for minimizing spherical aberration for the center views exist, yielding similar solutions for multiple off-center views is tedious to achieve, especially if one wishes to minimize coma aberrations.
Hence, it was decided by the inventors that it may be useful to employ numerical optimization to generate the optimal lens shape, given a specific lens model. The numerical optimization not only minimizes (or reduces) aberrations but also optimizes (or at least enhances) the display surface to arbitrary shapes for better focusing properties. Spherical lenses and aspherical lenses were investigated for use in the lens arrays. In general, aspherical lenses tend to be superior compared to spherical lenses, especially for the center views. The result of a numerical optimization for a 5 mm lens with a 30° field of view were obtained with ray tracing supporting the above generalized results (average focus errors being less for aspherical lenses).
A variety of manufacturing or fabrication processes may be used to produce the lenticular display devices of the present invention, and these processes may be relatively flexible such that a number of optimization processes can be used to provide more optimal lenses/lenticules for the array. First, for example, the shape of the display surface may be adapted, and second, for example, the lenses may be rotated towards the primary viewing location.
One way to provide an improved lens array that may be content-adaptive is to provide or use a non-planar display surface (e.g., the planar back surface of a conventional lens array is replaced with a non-planar back surface or display surface on which the display content or interlaced images are printed or otherwise provided underneath corresponding lenticules/lenslets). Interestingly, the optimal focusing distance for different views does not lie on a plane, and, ideally, the back plane should be at a different depth for different views (content layer should be non-planar to coincide with these differing focusing distances).
With this in mind, alternative back plane shapes were incorporated into the lens optimization: axis-aligned planar patches, non-axis aligned facets, and parametric curves. In general, the views close to the optical axis of the lenses can be improved greatly by this optimization, whereas the off-axis views tend to perform similar to the initial optimization result. One set of optimization results indicated that the resulting focus error can be reduced by 17.5 percent and 20.8 percent, respectively, for axis-aligned and non-axis aligned facets for a material with index of refraction of 1.47.
Another lens optimization technique involves lens rotation. Using regular lenses with their optical axis aligned to one direction may waste many rays on the borders of the lenslet array, as these rays fall outside the combined field of view of all lenses. Due to the lens characteristic for off-axis views, lenses on the borders of the lens array may show increased crosstalk. In order to reduce or even minimize these effects, the optical axis may be aligned to the expected center position of the viewer. More specifically, the amount of rotation for each lens is chosen such that all optical axes intersect at the center position for an assumed viewer distance.
FIG. 3 illustrates a functional block diagram of a lenticular display design system 310 that may be used by an operator to design a lenticular display device that is content-adaptive as discussed herein. The system 310 may be provided on one or more computer devices running software or computer code to perform the functions described, and, to this end, the system 310 includes a processor 312 managing input/output (I/O) devices 314 such as a monitor, touchscreen, touchpad, keyboard, mouse, and the like as well as memory or memory devices 340 (e.g., computer readable medium on the system 310 or accessible by the system 310 and/or CPU 312 ). The CPU 312 runs software or computer programs including a discrete light field optimization module 316 , which may use a lens distribution routine 318 (e.g., to implement Algorithm 1 defined above), and a lens optimization module 320 . The module 316 may be used to perform the discrete light field optimization steps or functions described above while the module 320 may be used by the system 310 to perform the lens optimization steps or functions described above.
During operation of the system 310 , the memory 340 is used to store an input light field 342 corresponding to a scene that is to be displayed by a lenticular display device. The discrete light field optimization module 316 uses the distribution routine 318 to generate a lens distribution 350 , in a recursive manner as described above, to produce a number of lenses 352 across the width of a lens array such that the output light field 344 provided by these lenses matches or most closely matches the input light field 342 (e.g., based on reducing mean squared projection errors 346 for the lenses 352 or the like).
Each lens 352 in the array is defined or characterized by its width 354 , the color content at its back surface 356 , and a focal length 358 . In the lens array defined by these lenses, each lens 352 across the width of the lens array may differ in these three parameters 354 , 356 , 358 , but, in a typical array, the lenses may be arranged in sets in which the lenses are uniform within the set but differ from other sets. For example, wider lenses with a greater focal length may be placed at the two ends of the array, intermediate width lenses may then be provided adjacent to these two sets of wider lenses, and then one or more narrower and narrower lens sets may be placed in the center for the array. However, wider lenses with larger focal lengths may also be provided in the center of the array if that suits or adapts to the particular input light 342 . The number of differing lens sets is not limiting to the invention, but it may often include at least two differing widths with 3 to 10 or more being useful, in some cases, across a particular array so as to suit the differing angular and spatial frequencies of the content.
The lens optimization module 320 is used to define a set of array configuration or fabrication parameters such as whether the back plane is planar or non-planar. The module 320 may be used to implement a lens optimization process such as to define a non-planar display surface with content locations 364 stored in memory 340 . This may involve setting the front edges or surfaces of each of the lenses in a plane (i.e., a front plane or light receiving surface) but placing the content layer or display images at or near the focusing distances of each lens 352 (which may differ across the width of the array such that the back plane or content layer is non-planar or stepped). In other words, the content locations 364 relative to a rear plane such as a backing surface or backlight will vary for the lens array defined by the lens distribution 350 and array configuration parameters 360 (as shown in FIGS. 5 and 6 ).
Lenticular display devices (or lenticular prints) often are fabricated with a lens sheet or array with a printed image sheet or layer that is glued underneath on the planar back surface (e.g., the content is arranged in a single plane or to be planar). FIG. 4 illustrates a lenticular display device 400 according to the present invention with such a planar content configuration. As shown, the device 400 includes a lens array or sheet 410 with lenses/lenticules 412 , 414 , 416 with differing configurations as shown by the three differing widths (w 1 >w 2 >w 3 ). The lenses 412 , 414 , 416 were distributed to suit an input light field, and content or images associated with such a light field are provided in content/ink layer 420 that may be glued/adhered or directly printed with 2D printing onto the array 410 . Particularly, the back surfaces of each lens 413 , 415 , 417 are in a planar backplane 418 , and these surface 413 , 415 , 417 may receive the content layer/ink layer 420 in the lenticular print 400 . By varying the configuration of the lenses 412 , 414 , 416 , the array 410 can be thought of as being content-adaptive to suit the underlying spatial and angular frequencies of the content layer 420 .
The lenticular sheet 410 may be composed of optical quality plastic resin and may be created by extruding plastic underneath a drum shaped with the inverse of the required lens profile. Affixing the image 420 to the lens array 410 may require pixel-accurate registration in order for the light field to appear correctly. As the lens array 410 changes shape and position of the lenses 412 , 414 , 416 over the image layer 420 , existing lenticular fabrication processes may be less practical. For example, a drum or mold may be manufactured to create the correct lens array shape, but, the present invention teaches the usefulness of changing the lens array shape (use differing lenses 412 , 414 , 416 ) for each input light field or content layer 420 . Therefore, it may only be economical to use conventional fabrication processes for large print runs to display a particular scene/input light field.
With the advent of high-accuracy 3D printing technology, the content-adaptive lenticular display devices become much more applicable and accessible. For example, the lens array 410 may instead be fabricated using 3D printing devices. The inventors, in one case, employed an additive multi-material printer that fabricates 16 μm-accurate object layers using UV-curable resin (e.g., an Objet Connex 3D polymer printer or the like may be used). This printer was able to print two different material simultaneously so that the prototype lenticular print was fabricated by fabricating the lens array concurrently with the content layer (or display surface) rather than using separately printed cards.
FIG. 5 illustrates a more preferred embodiment of a lenticular print 500 . The print 500 includes a lens array or lenticular sheet 510 made up of a number of lenses/lenticules 512 , 514 , 516 that, like print 400 , have differing widths, color content on their back surfaces, and focal lengths that are selected to suit the content or input light field corresponding with content or image layer 520 . The print 500 differs from print 400 , though, because the front edges or receiving surfaces of the lenses 512 , 514 , 516 are arranged in plane (or frontplane) 518 so that the array 510 has a correct view across the field of view.
Further, this results in the back surfaces 513 , 515 , 517 of the lenses 512 , 514 , 516 being non-planar as shown by the differing distances, d 1 <d 2 , from a backplane or rear reference plane 524 , with the largest width lenses 512 having their back surfaces 513 co-planar with this plane 524 and the offsets increasing as the width of the lens decreases (or its focal length decreases). Since the back surfaces 513 , 515 , 517 are non-planar in array 510 , the content layer is also nonplanar or arranged with a multi-step alignment so that the content/interlaced images are placed at or near the focal distance of each overlying lens 512 , 514 , 516 . Although not shown, a diffuse backing and/or backlight may be provided in the display device 500 such as to be coplanar with the reference plane 524 or to sandwich the content layer 520 between the back surfaces 513 of larger lenses 512 .
Hence, instead of using one display or projection surface for all lenses (e.g., content layer 420 in display device 400 of FIG. 4 ), the lens surfaces may be aligned with plane 518 in device 500 rather than their focal planes. This reduces crosstalk through adjacent, higher lenses. One benefit of 3D printing the lenses 512 , 514 , 516 of array 510 concurrently with content 520 is that the display surface or content layer 520 is aligned with the lens surface. Furthermore, 3D printing of device 500 allows for printing lenses with non-planar projection or back surfaces 513 , 515 , 517 .
In one implementation, the 3D printer is only able to print two materials at the same time. In this limited embodiment, the first material may be a transparent resin to realize the lens shape and the second material may be used to display content, e.g., a black material to display content. While this printer was limited to providing gray scale values for content 520 , it is expected that future 3D printers will support multiple colors, thus more effectively providing colored content-adaptive lenticular prints (such as print 500 ). Another technique may involve a multi-step printing process. A first step may involve manufacturing the lenses with non-planar/regular focal planes or projection surfaces. Then, second, third, and more steps may be performed to fabricate or provide pixels of different colors for content/display layer 520 , and the colored pixel surfaces could then be combined onto the lens shape as shown in FIG. 5 .
In one embodiment, field-of-view (FOV) baffles are provided in lenticular print. Particular, the use of a multi-material or 3D printer allows one to print black (or other colored) strips between consecutive lenses/lenticules so as to reduce cross-view zone artifacts. Such effects can occur when an observer is in a viewing position outside the combined field of view of the display and are most noticeable as inconsistent view transitions across the display. Due to the material transparency, the baffle preferably is of sufficient thickness to block all or a significant amount of light striking the baffle. In some embodiments, a printer supporting multiple colors may be used such that the baffle can be printed with actual content, but the lens would have to focus on the backplane as well as the baffle in such embodiments.
FIG. 6 illustrates a graph 600 showing an example of one use of the discrete light field optimization method to distribute a set of lenses/lenticules for a lens array based on a local analysis of the 2D light field (input light field). At the top of the FIG. 600 , it can be seen that an input light field is provided with a width w L =5, and a set of candidate lenslets with differing widths W={1, 2, and 4}. As mentioned above, each lenslet covers a sub-area (e.g., a rectangle) of the input light field.
The optimization algorithms starts with the full light field width of w L =5. It places candidate lenslets starting with w=1 on the right side of the light field and recurses to find the optimal lens distribution for the remaining left subset. This recursion continues until the base case of w L =1 and w=1. The incurred error for placing this single lens is then used (shown with black arrow) to find the optimal lenslet distribution for w L =2, as it now allows one to compute the error for each of the two possible lens distributions [11] (left side used optimal distribution from recursion at w L =1) and [2]. [2] has the lower error and is recorded/stored in memory as the optimal lens distribution for w L =2. This continues back up to w L =5, where [212] has the lowest error and is the final optimal distribution in this example.
Although the invention has been described and illustrated with a certain degree of particularity, it is understood that the present disclosure has been made only by way of example, and that numerous changes in the combination and arrangement of parts can be resorted to by those skilled in the art without departing from the spirit and scope of the invention, as hereinafter claimed.
As will be appreciated, the above description teaches content-adaptive lenticular displays that are or can be optimized for static light field content. The concepts described above, though, are applicable to electronically changeable lenses and, therefore, to dynamic content. The description also explains a light field analysis and optimization strategy to yield an ideal lenslet layout for a lens array of a lenticular display device to provide an automultiscopic representation of a given scene. The lens array and its lenslets/lenticules can be, according to the teaching provided herein, optimized to have a design facilitating 3D printing.
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A lenticular display device that is effective in increasing both perceived angular resolution and spatial resolution. These desirable results are achieved by modifying the lenslet array to better match the content of a given light field. An optimization algorithm or method (which may be implemented with software run on a computing device) is provided that analyzes an input light field and computes an optimal lenslet size, shape, and arrangement of sets of lenslets across the width of the array to better (or even best) match the input light field given a set of output parameters. The resulting lenticular display device (or print) shows higher detail and smoother motion parallax compared with fixed-size lens arrays. The usefulness of these content-adaptive lenticular prints has been demonstrated or proven using rendered simulations, by generating 3D-printed lens arrays according to the present description, and with user studies.
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