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BACKGROUND OF THE INVENTION
[0001] The present invention relates to a transmission system for a vehicle, and more particularly to a transmission for a motorcycle-type vehicle or the like.
[0002] Conventional motorcycles allow the rider to control the use of the motorcycle without removing the user's hands from the handlebars. In most conventional motorcycles, the control system uses a manual transmission. Suitable torque, or turning force, is generated by the engine only within a narrow range of engine speeds, i.e., rates at which the crankshaft is turning. However, the wheels must turn with suitable torque over a wide range of speeds. While its speed is held roughly constant, the engine turns an input shaft on the transmission whose output shaft can be adjusted to turn the wheels at an appropriate speed.
[0003] The manual transmissions consist of a system of interlocking gearwheels. These wheels are arranged so that by operating a lever on the handlebar, the driver can choose one of several ratios of speed between the input shaft and the output shaft. The first gear gives the lowest output speed, second gear the next lowest, and so forth. To allow smooth shifting from one gear to another, a clutch is provided to disengage the engine from the transmission. When the rider takes his hand off the clutch lever, springs squeeze the friction disk into the space between the flywheel and the pressure plate, enabling the engine shaft to turn the transmission. However, the manual transmissions in motorcycles suffer the same disadvantages as manual transmission on any other type of vehicle—they require additional movement by the user and continuous attention to the speed of the motorcycle.
[0004] The shift switch with an upshift button and a down shift button are provided on the right handle bar while the left handle bar has normal clutch lever mounted thereon. In operation, the user depresses the clutch lever and the up shift button which causes the upshift control solenoid to open to permit a burst of air to flow to the actuator and change the transmission gear ratio. The downshifting is performed by pushing the down shift button.
[0005] An automatic transmission in a vehicle switches to the optimum gear without driver intervention except for starting and going into reverse. The type of automatic transmission used on current American cars usually consists of a fluid torque converter and a set of planetary gears. The torque converter transmits the engine's power to the transmission using hydraulic fluid to make the connection. For more efficient operation at high speeds, a clutch plate is applied to create a direct mechanical connection between the transmission and the engine. The 4-5 speed automatic transmissions that are available in automobiles are not currently available in the motorcycle industry.
[0006] A continuously variable transmission (CVT) uses a belt that connects two variable-diameter pulleys to provide an unlimited number of ratio changes and uninterrupted power to the wheels. CVT transmissions offer better fuel efficiency than conventional automatic transmissions, which change the transmission ratio by shifting gears. There are numerous problems associated with the CVT-type transmission. One of the problems is that this type of design requires tension on the belt/chain at all times, otherwise the belt tends to slip. This means that one pulley must expand/contract exactly in accordance with the other pulley, creating a task of keeping the tension on the belt at all times as it moves up and down the center groove of the two pulleys.
[0007] Additionally, the CVT-type transmissions have certain limitations, such as the pulley drive consisting of a belt with numerous metal links that are held together by being sandwiched between an upper and lower rubber belts. If the belt breaks down, it releases all the metal links with the transmission case or a slick belt slips. Additionally, the CVT transmission results only in two speed transmission, high and low, not a four or five speed automatic transmission available in conventional land vehicles.
[0008] Further, the motorcycle version of the CVT transmission is limited due to its size and cannot be fitted to motors larger than 1100 cc. Even further, a CVT transmission cannot handle the power of the large motors due to belt slippage. While this type of transmission works satisfactory under some conditions, it may develop a problem over a period of time due to the presence of multiple mechanical links and may not hold up in a high performance situation.
[0009] The present invention contemplates elimination of drawbacks associated with the prior art and provision of a device for regulating and enabling an automatic transmission that can be used with motorcycle-type vehicles providing convenience and ease of operation for the user.
SUMMARY OF THE INVENTION
[0010] It is, therefore, an object of the present invention to provide a control system for an automatic transmission system which does not require manual right and left handle bars coordination of movement.
[0011] It is another object of the present invention to provide a user-friendly automatic transmission control system which allows for a smooth shifting between the gears with an automatic control provided by a central processing unit.
[0012] It is a further object of the present invention to provide an automatic transmission control system, which uses a central processing unit to receive data signals from a plurality of sources associated with operation and movement of the motorcycle.
[0013] These and other objects of the present invention are achieved through a provision of an electronic transmission control system for controlling the functions of a transmission in a land vehicle, such as a motorcycle equipped with an engine. The control system comprises an electronic transmission controller having a memory for storing control parameters for controlling the functions of the transmission and a processor for processing signals indicative of movement of the motorcycle and a user interface device with a display thereon for communicating with the controller. A plurality of sensor means detect various functions of the vehicle operation, such as speed of rotation of the motorcycle engine, speed of movement of the motorcycle, position of a motorcycle throttle, and solenoid line pressure. The interface device is connected to the controller for sending overriding signals to the controller and selectively controlling operation of the transmission.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Reference will now be made to the drawings, wherein like parts are designated by like numerals and wherein
[0015] FIG. 1 is a schematic view of a motorcycle, in which the control system for the automatic transmission in accordance with the present invention can be used.
[0016] FIG. 2 is a schematic view of the automatic transmission control system of the present invention.
[0017] FIG. 3 is a schematic view of the automatic transmission control system of the present invention using a variation of the gear shifting means.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0018] Turning now to the drawings in more detail, numeral 10 designates a motorcycle in which the automatic transmission control system of the present invention can be employed. The motorcycle has a frame 12 , which supports the engine/transmission assembly for operating the motorcycle. Mounted on the frame 12 is a front wheel 14 and a rear wheel 16 rotatable by an internal combustion engine 18 . The front wheel 14 is protected by a front wheel fender 20 , while the rear wheel 16 is protected by a rear wheel fender 22 . A handle bar 24 controls operation and direction of movement of the front wheel 14 .
[0019] A rider seat 26 is supported by the frame 12 behind a fuel tank 28 . A transmission assembly 30 is connected to the cylinder block 32 of the engine assembly. A carburetor assembly 34 is positioned between the cylinder blocks 32 of the engine assembly.
[0020] In order to change transmission speeds, the rotational motion from one set of gears positioned in the motorcycle engine is transmitted to another set of gears which form a part of the engine assembly. The switching of the gears is effected by engaging and disengaging of clutch packs which receive oil pressure from the oil reservoir. When the engine is started, the pressure is relatively high, in the order of 150 pounds and, if engaged at once, it results in a jumping or jerking movements of the motorcycle. By regulating the pressure into the clutch packs through the solenoids, the present invention allows to deliver gradually increasing oil pressure from 20 pounds to a full engagement with the pressure of about 150 pounds.
[0021] The control system of the present invention comprises an electronic central processing unit, or CPU 40 , which processes signals received from control buttons and a number of sensors operationally connected to the operating parts of the motorcycle 10 . The microprocessor 40 controls operation of electronic sensors, which enhance the performance of the automatic transmission. As described in more details hereinafter, data about engine speed, exhaust pressure, and other performance characteristics are sent to the processor 40 , which controls the switching of gears and the clutch plate in the torque converter via electrical switches, or solenoids.
[0022] The CPU 40 stores control parameters for controlling the functions of the transmission 30 and has a processor for processing data indicative of the motorcycle functions, such as motor RPMs, speed of movement, degree of opening of the throttle and function of the solenoids in a location where the solenoids act on the engine valves. The pressure sensors regulate the amount of oil pressure sent to the clutch pack of the engine through the solenoids.
[0023] To start moving, the user selects the speed, for instance Drive by pushing one of the buttons 42 positioned on a left grip 44 of the motorcycle. The signal from the control button 42 is transmitted to the central processing unit 40 , which will energize the first gear 46 , then the second gear 48 , the third gear 50 and the fourth gear 52 in sequence, depending on the speed of the movement.
[0024] As the road speed of the motorcycle 10 increases, the CPU 40 energizes the respective electrically operated solenoid valves (not shown) while simultaneously releasing the first gear 46 to achieve the second gear 48 . Only one set of gears can be engaged at one time. The increase in speed of movement of the motorcycle 10 causes the CPU 40 to regulate switching of gears to the third gear 50 and then to the fourth gear 52 , one at a time.
[0025] The shift in gears and timing of the switch between the gears is determined by the central processing unit 40 depending on a variety of signals received by the central processing unit. The control system of the present invention employs one or more of sensing means that detect the operational condition of the vehicle at a given time. One of the data signals received by the central processing unit 40 is the speed of the revolutions of the motor (RPM) as detected by a tachometer 54 . Another set of data, which may be employed in detecting the operational position of the vehicle is a throttle sensor, where a throttle 56 sends a signal to a throttle position sensor 58 . The signal from the sensor 58 is transmitted to the central processing unit 40 . The throttle position sensor 58 detects the amount of fuel delivered to the motor.
[0026] Still another set of data may be collected by a speed sensor 60 , which receives data from the speedometer and sends the signal for processing by the central processing unit 40 in combination with other data received from the throttle sensor 58 and the tachometer 54 . Additionally, each of the solenoids 62 , 64 , 66 , and 68 has sensors which send signals to the central processing unit 40 for processing. These signals are combined with a signal from a pressure sensor 70 , which is also input into the central processing unit 40 as a signal of operating condition of the vehicle hydraulic system (not shown). The CPU 40 also receives a signal from the ignition 82 (positive and ground).
[0027] The current position of the transmission is shown by indicators in one of the control panel windows 72 of a gear position indicator, or display means 74 , which is mounted on the panel 76 forming a part of the handle bar assembly 24 . The indicators in the control panel windows 72 can show when the transmission is in a neutral position, a drive position, first, gear, second gear, third gear, etc.
[0028] Under some circumstances, the user may desire to retain the transmission in low gear, such as when moving slowly or driving on a steep hill. The present invention provides for a means to override the control signal of the CPU 40 . A selected button 42 on the gear shifting assembly 78 can be depressed to hold the transmission in the selected gear. For instance, if the user pushes the third gear button, the transmission will remain in the third gear. If the user chooses to press the button corresponding to the second or the first gear, the transmission will remain in second or third gear, respectively.
[0029] The user may also perform gear selection depending on the desired effect of movement of the motorcycle 10 . For instance, when the person desires to do a burnout, the user will press the hold button in the first gear and the transmission will not up shift until the button is depressed again. The transmission will then begin to up shift to the next gear ratio until or unless the hold button is pressed again.
[0030] As an alternative to the buttons 42 , the present invention provides for the use of a manual handle 80 ( FIG. 3 ) for gear shifting, which allows the user to override the automatic transmission controlled by the central processing unit 40 and retain the transmission in the desired gear.
[0031] It is envisioned that the automatic transmission of the present invention can be used on other land vehicles, such as all terrain vehicles, motorized bicycles and the like.
[0032] Many changes and modifications can be made in the design of the present invention without departing from the spirit thereof. I therefore pray that my rights to the present invention be limited only by the scope of the appended claims. | An electronic control for an automatic transmission of a vehicle, such as a motorcycle, has a central processing unit with a memory for storing control parameters for controlling the functions of the transmission and a processor for processing signals indicative of movement of the vehicle. The control system employs various sensors to facilitate smooth switching of gears in the automatic transmission, the sensors including speed sensor, tachometer, solenoid line pressure sensors and a throttle sensor. A user interface allows the user to selectively override pre-programmed gear selection of the transmission and choose operation at lower or higher gears. | 8 |
FIELD OF THE INVENTION
This invention relates generally to methods for removing adherent materials, for example, paint, flashes, photoresists, contaminants, and other materials from external surfaces. In particular, the method employs an improved media comprising core/shell particles.
BACKGROUND OF THE INVENTION
For various types of structures, it is often desirable to remove a coating that has been formed on an exterior surface area. In one case, the coating may be unwanted contamination. In another case the coating may be an intentionally applied material such as a decorative or protective layer. Numerous techniques exist for removing paint, sealants, lacquers, rust, scale, biogrowth and other adherent materials from virtually any type of surface. Surface cleaning or stripping methods range from mechanical abrasion to the use of strong chemicals and involve varying degrees of time, effort and expense. For any given type of coating, the character and function of the substrate material from which a coating is to be removed usually dictates the stripping method, at least in industrial settings.
In view of the environmental and health hazards involved in the use of solvents for cleaning surfaces, in particular, large exterior surfaces, it has become common practice to use an abrasive blasting technique wherein abrasive particles are propelled by a high pressure fluid against the solid surface in order to dislodge previously applied coatings, scale, dirt, grease or other contaminants. Hard, durable surfaces, such as heavy steel plating can be cleaned or stripped by a hard abrasive such as sand. Softer metals such as aluminum or more delicate surfaces such as polymer composite layers may require the use of a softer abrasive material during blasting such as plastic pellets or sodium bicarbonate.
Sand blasting of steel plate or other hard surface to remove adherent coatings and the like, while successful in removing the coatings, has several disadvantages. For one, the sand abrasive is very friable such that upon contact with the surface, a vast amount of silica dust is formed. There is a concern that the minute air-borne free-silica particles which are formed during blasting present a substantial health hazard, in particular, if ingested into the lungs. Secondly, very large amounts of sand are required for cleaning large structures such as bridges, stacks, etc. such that after blasting, this sand remains and must be removed from the blast cleaning area adding substantially to the time and expense of the blasting process.
Alternative abrasives for blast cleaning hard surfaces are known. For example, U.S. Pat. No. 3,775,180 is directed to a method for descaling steel in which the steel is descaled by spraying a mixture of a solid such as aluminum oxide or silicon carbide with water and a gas such as air under specified conditions onto the steel. In removing a coating or a scale on the surface of a metal, however, it is important that the anchor pattern (surface roughness) of the metal surface be uniform and not too extensive such that the surface and even the metal structure is damaged. A blast media composed only of hard aluminum oxide and silicon carbide can be detrimental to the metal structure.
Hard abrasives such as alumina, silicon carbide, or glass bead, or a soft abrasive such as a walnut shell flour has been blasted at a high speed onto molded products to remove flashes. U.S. Pat. No. 4,548,617 describes the problems associated with using these abrasives.
For certain surfaces such as metals softer than steel, a softer abrasive can be used with the blast stripping method. An example of such is disclosed in U.S. Pat. No. 4,878,320 to remove coatings from aluminum, fiberglass or carbon fiber laminate. As disclosed in the patent, an abrasive particle is used which has a Mohs hardness of about 3. Sodium bicarbonate is a preferred material.
Other patents which disclose cleaning metal surfaces with an abradant other than sand include U.S. Pat No. 2,624,988 which utilizes a mixture of Tripoli paste and a liquid vehicle to which mixture can be added sponge rubber fragments which carry the abradant to the metal surface and which provide a rubbing action to polish and buff the metal surface.
U.S. Pat. No. 2,710,286 discloses a method of removing fluorescent and other materials from viewing screens of cathode ray tubes in which sodium and potassium carbonate are used as the abrasive material. U.S. Pat. No. 4,588,444 discloses removing calcium from polymeric contact lenses by using as an abradant sodium chloride, sodium bicarbonate or a mixture of same. U.S. Pat. No. 4,731,125 discloses a method for removing adherent material from composite surfaces made of a reinforced matrix material using a granular media composed of particles which have a Mohs hardness of lower than 3.5. Preferably the abradant is polymeric particles.
Polymer particles are commercially available for use as non-abrasive stripping, cleaning, deburring, and deflashing media. These non-abrasive media are particularly useful when the substrate is susceptible to damage. Such substrates include aircraft and aerospace components, dye castings, computer housing panels, vehicle and boat bodies.
U.S. Pat. Nos. 5,505,749 and 5,509,971 to Kirshner et al. disclose the use of a major amount of a granular relatively soft abrasive having a Mohs hardness of less than 4 and a minor portion of a granular hard abrasive having a Mohs hardness of greater than 5. U.S. Pat. No. 5,234,470 to Lynn et al. discloses a granulated composite, in particular, a flexible open cell water-foamable material and an abrasive mineral such as garnet.
PROBLEM TO BE SOLVED BY THE INVENTION
It would be desirable to be able to clean an external surface more rapidly without damaging the underlying surface. It would also be desirable to be able to more finely control or tailor the abrasive properties of the media to balance its ability to remove a particular coating without attacking a particular surface material. It would be desirable for the media to be durable and non-friable and not produce dust during use. It would also be desirable for the media to flow through the propelling equipment without clogging nozzles or requiring special treatment to prevent static cling.
It would be desirable to be able to economically manufacture and customize such particles for a particular application.
It would be desirable to accomplish this without using chemicals that present environment or health problems. It is an object of the invention to remove surface materials without harming the underlying surface of the structure and which is more effective than other known non-abrasive media.
SUMMARY OF THE INVENTION
The above objects are achieved by providing an abrasive media that comprises a polymeric core surrounded by a layer of inorganic particles. The media can be propelled against or along an external surface by a gaseous or liquid carrier medium or a mixture of gas and liquid to remove the unwanted surface material. By the term “external surface”, with respect to the surface being cleaned, is meant a surface that, during use, is not enclosed but rather is freely open or exposed to the ambient atmosphere, as it will be exposed to the cleaning composition of the present invention. Thus, internal surfaces, such as the concave surface of a conduit or an enclosed tank, is excluded. Typically the abrasive media of the present invention is applied by shooting or blasting the media through air, specifically the air space between the external surface to be cleaned and the means for shooting or propelling the particles.
This invention can be used for removing adherent materials, for example, paint, flashes, burrs, photoresists, contaminants, biogrowth, and other materials from various surfaces. Contaminants to be removed from a surface may include any foreign substance attached to or carried by the surface such as scale, soil, grease, oil, soot, solvents and other objectionable deposits. In another type of situation, the surface material may be a previously applied material such as a paint or photoresist.
In one embodiment, suitable blasting equipment propels the media, via a pressurized air stream, against a surface of an object to dislodge and/or absorb any contaminant thereon.
DETAILED DESCRIPTION OF THE INVENTION
In its broadest aspect, the abrasive media of the present invention comprises a polymeric core surrounded by a shell of inorganic particulate. The polymeric core can be any naturally occurring or synthetic polymer such as, for example, olefin homopolymers and copolymers, such as polyethylene, polypropylene, polyisobutylene, polyisopentylene and the like; polyfluoroolefins such as polytetrafluoroethylene, polyvinylidene fluoride and the like, polyamides, such as, polyhexamethylene adipamide, polyhexamethylene sebacamide and polycaprolactam and the like; acrylic resins, such as polymethylmethacrylate, polyethylmethacrylate and styrene-methylmethacrylate or ethylene-methyl acrylate copolymers, ethylene-ethyl acrylate copolymers, ethylene-ethyl methacrylate copolymers, polystyrene and copolymers of styrene with unsaturated monomers mentioned below, polyvinyltoluene, cellulose derivatives, such as cellulose acetate, cellulose acetate butyrate, cellulose propionate, cellulose acetate propionate, and ethyl cellulose; polyvinyl resins such as polyvinyl chloride, copolymers of vinyl chloride and vinyl acetate and polyvinyl butyral, polyvinyl alcohol, polyvinyl acetal, ethylene-vinyl acetate copolymers, ethylene-vinyl alcohol copolymers, and ethylene-allyl copolymers such as ethylene-allyl alcohol copolymers, ethylene-allyl acetone copolymers, ethylene-allyl benzene copolymers ethylene-allyl ether copolymers, ethylene-acrylic copolymers and polyoxy-methylene, polycondensation polymers, such as, polyesters, including polyethylene terephthalate, polybutylene terephthalate, polyurethanes and polycarbonates. Styrenic or acrylic polymers are preferred. Polystyrene and polymethylmethacrylate are especially preferred.
The polymeric core can be selected in order to provide desirable properties. For instance, polymers are well known which are soft or hard, elastic or inelastic, etc. It can be particularly advantageous to crosslink the polymer in order to increase it's strength and make it resistant to fracture. In its broadest aspect, the blast media of the present invention encompasses the use of a polymeric core having a hardness of less than 5.0, preferably less than 4.0 and even less than 3.0 on the Mohs scale
The shell of the abrasive blast media of this invention, which adheres to the polymeric core, is an inorganic particulate which can act as a hard abrasive to provide a grit which abrades the surface in a controlled fashion without effecting the mechanical integrity of the structure being blast cleaned for the removal of coating layers. In its broadest aspect, the blast media of the present invention encompasses the use of an inorganic particulate having a hardness of at least 5.0, preferably at least 6.0 and even about 7.0 and above on the Mohs scale. Non-limiting examples include aluminum oxide, silicon carbide, tungsten carbide, silica, alumina, alumina-silica, tin oxide, titanium dioxide, zinc oxide or garnet and the like. The hard abrasive can be from about 5 nanometers to 1000 nanometers in size, preferably from about 10 nm to 100 nm in size. The preferred hard abrasive is colloidal silica.
The media in accordance with the present invention flows readily through the propelling equipment. However, it may also be useful in accordance with the present invention to include a flow aid or an anti-caking agent with the blast media. Most preferably, the flow aid is a hydrophilic silica, hydrophobic silica, hydrophobic polysiloxane or mixture thereof.
Any suitable method of preparing core/shell particles having a polymeric core adherently covered with a shell of inorganic particles may be used to prepare the particulate media for use in accordance with this invention. For example, suitably sized polymeric particles may be passed through a fluidized bed or heated moving or rotating fluidized bed of inorganic particles, the temperature of the bed being such as to soften the surface of the polymeric particles thereby causing the inorganic particles to adhere to the polymer particle surface. Another technique suitable for preparing polymer particles surrounded by a layer of inorganic particles is to spray dry the particles from a solution of the polymeric material in a suitable solvent and then before the polymer particles solidify completely, pass the particles through a zone of inorganic particles wherein the coating of the polymeric particles with a layer of the inorganic particles takes place. Another method to coat the polymer particles with a layer of inorganic particles is by mechanofusion.
A still further method of preparing the particulate media in accordance with this invention is by limited coalescence. This method includes the “suspension polymerization” technique and the “polymer suspension” technique. In the “suspension polymerization” technique, a polymerizable monomer or monomers are added to an aqueous medium containing a particulate suspension of inorganic particles to form a discontinuous (oil droplets) phase in a continuous (water) phase. The mixture is subjected to shearing forces by agitation, homogenization and the like to reduce the size of the droplets. After shearing is stopped an equilibrium is reached with respect to the size of the droplets as a result of the stabilizing action of the inorganic particulate stabilizer in coating the surface of the droplets and then polymerization is completed to form an aqueous suspension of polymeric particles in an aqueous phase having a uniform layer thereon of inorganic particles. This process is described in U.S. Pat. Nos. 2,932,629 and 4,148,741 incorporated herein by reference.
In the “polymer suspension” technique, a suitable polymer is dissolved in a solvent and this solution is dispersed as fine water-immiscible liquid droplets in an aqueous solution that contains inorganic particles as a stabilizer. Equilibrium is reached and the size of the droplets is stabilized by the action of the inorganic particles coating the surface of the droplets. The solvent is removed from the droplets by evaporation or other suitable technique resulting in polymeric particles having a uniform coating thereon of inorganic particles. This process is further described in U.S. Pat. No. 4,833,060 issued May 23, 1989, assigned to the same assignee as this application and herein incorporated by reference.
In practicing this invention, using the suspension polymerization technique, any suitable monomer or monomers may be employed such as, for example, styrene, vinyl toluene, p-chlorostyrene; vinyl naphthalene; ethylenically unsaturated mono olefins such as ethylene, propylene, butylene and isobutylene; vinyl halides such as vinyl chloride, vinyl bromide, vinyl fluoride, vinyl acetate, vinyl propionate, vinyl benzoate and vinyl butyrate; esters of alphamethylene aliphatic monocarboxylic acids such as methyl acrylate, ethyl acrylate, n-butylacrylate, isobutyl acrylate, dodecyl acrylate, n-octyl acrylate, 2-chloroethyl acrylate, phenyl acrylate, methyl-alphachloroacrylate, methyl methacrylate, ethyl methacrylate and butyl methacrylate; acrylonitrile, methacrylonitrile, acrylamide, vinyl ethers such as vinyl methyl ether, vinyl isobutyl ether and vinyl ethyl ether; vinyl ketones such as vinyl methylketone, vinyl hexyl ketone and methyl isopropyl ketone; vinylidene halides such as vinylidene chloride and vinylidene chlorofluoride; and N-vinyl compounds such as N-vinyl pyrrole, N-vinyl carbazole, N-vinyl indole and N-vinyl pyrrolidone, divinyl benzene, ethylene glycol dimethacrylate, mixtures thereof; and the like. Preferred are styrene or methyl methacrylate.
If desired, a suitable crosslinking monomer may be used in forming polymer particles by polymerizing a monomer or monomers, including a monomer or monomers that are polyfunctional with respect to the polymerization reaction, within droplets in accordance with this invention to thereby modify the polymeric particle and produce particularly desired properties. Typical crosslinking monomers are aromatic divinyl compounds such as divinylbenzene, divinylnaphthalene or derivatives thereof; diethylene carboxylate esters and amides such as diethylene glycol bis(methacrylate), diethylene glycol diacrylate, and other divinyl compounds such as divinyl sulfide or divinyl sulfone compounds.
In the suspension polymerization technique, other addenda are added to the monomer droplets and to the aqueous phase of the mass in order to bring about the desired result including initiators, promoters and the like which are more particularly disclosed in U.S. Pat. Nos. 2,932,629 and 4,148,741, both of which are incorporated herein in their entirety.
Useful solvents for the polymer suspension process are those that dissolve the polymer, which are immiscible with water and which are readily removed from the polymer droplets such as, for example, chloromethane, dichloromethane, ethyl acetate, propyl acetate, vinyl chloride, methyl ethyl ketone, trichloromethane, carbon tetrachloride, ethylene chloride, trichloroethane, toluene, xylene, cyclohexanone, 2-nitropropane and the like. Particularly useful solvents are dichloromethane, ethyl acetate and propyl acetate because they are good solvents for many polymers while at the same time, being immiscible with water. Further, their volatility is such that they can be readily removed from the discontinuous phase droplets by evaporation or boiling.
The quantities of the various ingredients and their relationship to each other in the polymer suspension process can vary over wide ranges. However, it has generally been found that the ratio of the polymer to the solvent should vary in an amount of from about 1 to about 80% by weight of the combined weight of the polymer and the solvent and that the combined weight of the polymer and the solvent should vary with respect to the quantity of water employed in an amount of from about 25 to about 50% by weight. The size and quantity of the inorganic particulate stabilizer depends upon the size of the particles of the inorganic particulate and also upon the size of the polymer droplet particles desired. Thus, as the size of the polymer/solvent droplets are made smaller by high shear agitation, the quantity of solid colloidal stabilizer is varied to prevent uncontrolled coalescence of the droplets and to achieve uniform size and narrow size distribution of the polymer particles that result. The suspension polymerization technique and the polymer suspension technique herein described are the preferred methods of preparing the particulate media having a core/shell structure comprising a polymeric core with a shell of inorganic particles for use in accordance with this invention. These techniques provide particles having a predetermined average diameter anywhere within the range of from 10 micrometer to about 2000 micrometers with a very narrow size distribution. The coefficient of variation (ratio of the standard deviation) to the average diameter, as described in U.S. Pat. No. 2,932,629, referenced previously herein, are normally in the range of about 15 to 35%.
The particle size of the abrasive particulates will range from about 10 to 2,000 μm, preferably from about 30 to about 1,000 μm, and most preferably from about 100 to 700 μm.
The process of this invention is particularly useful for applications where the surface being cleaned is susceptible to damage such as those listed below:
In one embodiment, a method according to the present invention is used in the printed circuit industry to remove resist from printed circuit boards. In particular, resist removal from a processed printed circuit substrate is facilitated using the core/shell particles as described above. The use of such particles helps to simplify and shorten the resist removal process without damaging the delicate printed circuit lines or the underlying substrate material. The use of such particles also enables a process yielding an environmentally safe waste, one without caustic liquids intermingled with spent resist as described, for example, in U.S. Pat. No. 5,145,717.
In another embodiment, a method according to the present invention is used for flash removal from a molded product. Molded products, such as obtained through a plastic encapsulation step of semiconductor devices such as ICs or LSIs often have flashes. Flash removal is facilitated using core/shell particles of this invention. This avoids the use of a hard abrasive as discussed above and the problems associated with using these abrasives.
In another embodiment, a method according to the present invention is used for removing a coating from an airplane, missile or other substrates or skins in the aerospace industry. Plastic media blasting (PMB) has been in use since the late 1980's, principally for stripping paint and cured powder coatings from aircraft and aerospace components which can not survive more aggressive removal processes. Substrates such as aluminum and aluminum alloys are especially sensitive. See, for instance, “Using Plastic Media Blasting to Remove Powder Coatings from Parts”, Powder Coating, April 1996, incorporated by reference in its entirety. The use of PMB using core/shell particles of the present invention allows for the faster removal of coatings in the aerospace industry.
In another embodiment, a method according to the present invention is used to remove coatings from composites. The class of materials referred to as composites present special problems. Composites are usually made of a matrix material, such as plastic or epoxy, which often contains fibers such as glass strands, graphite, KEVLAR polymer or the like for reinforcement. Layers of the material are laminated together or pressed onto a honeycomb base to form structural material. Such composites are strong and light and are increasingly used in aircraft, boats and other manufactured products where weight savings are important. Because composites usually have surfaces which are softer than metals, removal of paint or other coatings from composites must be done carefully to avoid excessive abrasion or chemical damage. U.S. Pat. No. 4,731,125 teaches paint removal from composites using a granular plastic material, which patent is hereby incorporated by reference. The use of core/shell particles according to this invention allows for faster removal of paint from composites.
Various abrasive blasting techniques can be utilized to remove coatings from surfaces. Thus, blasting techniques include, for example, dry blasting which involves directing the abrasive particles to a surface by means of pressurized air typically ranging from 30 to 150 psi; wet blasting in which the abrasive blast media is directed to the surface by a highly pressurized stream of water typically 3,000 psi and above; multi-step processes comprising dry or wet blasting and mechanical techniques such as sanding, chipping; and single step processes in which both air and water are utilized in combination to propel the abrasive blast media to the surface as disclosed, for example, in U.S. Pat. No. 4,817,342, incorporated by reference.
In some cases, an anchor pattern (some surface roughness) may be desirable or allowable, for example, when removing or stripping old paint to be replaced with new paint.
In methods of this invention, the media is accelerated to a flow which is effective for blast cleaning. Acceleration can be accomplished by a suitable media propelling means, such as a pneumatic sand blaster, or similar device. Preferably, the media propelling means will have a movable media outlet such as a nozzle, which allows the media flow to be directed over a target surface area to be cleaned. The media propelling means should produce an output pressure for the media flow of approximately 40 to 150 pounds per square inch (psi). 40 psi is a lower pressure than is used in most sand blasting operations. Conventional sand blasters can often be modified to output media at 40 psi by a simple adjustment, or, in some cases, by the addition of a pressure regulator to the equipment. Although the pressure of the media flow need not be exact to practice the present invention, it is often important that pressures substantially higher than desired are not used since higher pressures tend to damage delicate substrates.
A typical configuration for practicing the present invention includes pressure blast cleaning equipment manufactured by Clemco Industries. Such equipment includes a reservoir of media to be accelerated. Pneumatic pressure blast cleaners also include an inlet line from a source of pressurized air or other gas. A pressure regulator may also be provided to reduce the inlet pressure supplied through the inlet line. The outlet from media propeller includes a long flexible tube or hose through which the pressurized media flows. At the end of hose is a nozzle which serves as a media outlet and as a means for directing the media flow emerging from the nozzle. The media flow will be a mixture of pressurized air or other pressurizing gas and the media particles, which will emerge in high volume and at relatively high speed. For the purposes of practicing the present invention, media flow will be substantially continuous and have a pressure at the nozzle of approximately 40 to 150 psi
The nozzle diameter determines the diameter of media flow. A larger nozzle size requires a greater volume of pressurized air at the inlet line and produces a correspondingly larger volume of media flow at the nozzle. Nozzle sizes of ¼ inch and ½ inch are effective with the present invention, although larger sizes can be used if pressure blast equipment of sufficient capacity is available. Regardless of the nozzle size, it is anticipated that the media flow will be confined by the nozzle to a diameter which is substantially smaller than the size of the target surface to be cleaned. As such, the media flow will be directed over the target surface in the manner described below in order to remove adherent material from the surface being treated.
Directing the media flow at the target surface constitutes the next step in the method of the present invention. It is anticipated that in most applications of the present invention the surface to be cleaned will be stationary and the nozzle will be moved to clean the surface. For example, in cleaning composite surfaces on an aircraft fuselage or the like, a person holding the nozzle will direct the media flow over the target surface in a varying manner until the surface is cleaned.
In order to remove paint and other adherent material efficiently from surfaces, it is preferable that the path of the media flow against the target surface be optimized. An optimal path of media flow will be one in which the angle and direction of the media flow produces highly efficient removal of adherent material from the surface without damage to the surface. This is generally done by angling the media flow away from a perpendicular direction with respect to the target surface so that the leading edge of the coating being removed is exposed to the force of the media flow. An optimal path of media flow with respect to a surface will be directed at the leading edge of the adherent material to be removed. The angle of the media flow with respect to perpendicular is increased to increase the rate of removal. An increase in the angle results in more media particles being available to dislodge the adherent layers at the leading edge. For this reason, it is preferred that the angle be increased until the observed effectiveness of the removal action is maximized, and that angle then becomes the optimal path of media flow.
Another preferred step in the cleaning process is the efficient redirection of the media flow over the target composite surface until the entire surface is cleaned. It has been found that this is best accomplished by directing the media flow primarily at areas of adherent material remaining to be removed, and then redirecting the media flow to other unremoved areas whenever removal in the first area is substantially accomplished. In this way, exposure of cleaned, and therefore unprotected, surface to the full force of the media blast is minimized. During the entire cleaning process, an optimal path or angle of media flow is preferably maintained. Only at the start of the cleaning process or at other times when obstructions prohibit selection of an angle for the media flow will it be best to keep the media flow perpendicular to the target surface. At other times, the maintenance of an optimal path in response to the observed effectiveness of action of the media flow will produce the most efficient and effective surface cleaning action by the media flow.
The above-described process for the removal of adherent material from surfaces has proven to be superior to prior art surface cleaning techniques. Media blast eliminates entirely the need to use hazardous chemicals for surface cleaning. Not only is there a substantial savings of both time and labor, but the health, safety, pollution and disposal problems associated with chemical paint stripping are entirely eliminated. Other advantages of surface cleaning by the present invention include the ability to selectively remove outer layers of material while having underlying layers intact. This can be done by carefully directing the media flow at an area only until the desired layers are removed, leaving remaining layers intact. While such selective removal cannot be performed in some circumstances, such as where an underlying layer is too soft to remain intact, it is virtually impossible to perform selective removal with chemicals. It is also possible to modify the core/shell in order to achieve specific results. Such modifications include, for example, variations in the particle size, hardness, elasticity etc of the core and variations in the particle size, hardness and material of the abrasive grit shell.
The composite surface cleaning system can be modified to meet the needs of particular situations. For example, the blast pressure media particle size and angle of media flow can all be modified in order to facilitate efficient cleaning without damage to the composite surface. Small or angled nozzles can be employed in confined areas or to reach otherwise inaccessible parts of a composite surface. Other modifications within the scope of this invention include the use of other types of media propelling means or of other means to direct the media flow.
EXAMPLE 1
This example illustrates the synthesis of various core/shell particles for use in a method according to the present invention.
Preparation of 575 μm Crosslinked Beads
Inhibitor is removed from a mixture of 1320 g of styrene and 5280 g divinylbenzene (55% grade from Dow Chemical Co.) by slurrying with 132 g Dowex SBR-P(OH) Anion Exchange Resin for 15 minutes followed by filtering off the resin. 129 g of benzoyl peroxide (sold as Lucidol 75®) by Pennwalt Corp) are then dissolved in this uninhibited monomer mixture. In a separate vessel is added 8745 g of demineralized water to which is added 8.6 g of citric acid, 8.6 g of potassium hydrogen phthalate, 4.7 g of poly(2-methylaminoethanol adipate), and 8.9 g of Nalco 1060®, a 50% colloidal suspension of silica sold by Nalco Corp. The uninhibited monomer mixture is added to the aqueous phase and stirred to form a crude emulsion. This is passed through a Gaulin colloid mill operated at 7.56 1/minute feed rate, 1500 rev/min and gap setting of 0.0381 cm. To this is added a solution of 33.6 g polyvinyl alcohol (Airvol® 523) dissolved in 2200 g of demineralized water. The mixture is heated to 61° C. for 16 hours followed by heating to 85° C. for 4 hours. The resulting solid beads are sieved through an 18 mesh sieve screen to remove oversized beads and the desired beads which pass through the screen are collected by filtration. The collected beads are placed on a 70 mesh screen and washed with distilled water to remove undersized particles. The beads are then collected by filtration and the filter cake is rinsed with 6000 g demineralized water. The beads are then vacuum dried at 50° C. for 3 days. The resultant particles are 575 μm in size and are a crosslinked polystyrene core covered with colloidal silica.
Preparation of 575 μm Crosslinked Beads without Shell of Inorganic Particles (Comparative)
The beads from above are slurried in 4 L of 1 N NaOH solution and stirred for 1 hour. The beads are filtered and redispersed in 4 L of 0.1 N NaOH solution and stirred overnight. The beads are filtered and successively re-slurried in 4 L of demineralized water until the filtrate pH is <8.5. The beads are then filtered and dried in a vacuum oven overnight at 80° C. for 2 days. The resultant particles are 575 μm in size and are a crosslinked polystyrene bead without a shell of inorganic particles.
EXAMPLE 2
This Example demonstrates the cleaning efficacy of the method of the present invention.
Preparation of Test Panels
One-foot-by-one-foot squares were cut from a 4-foot-by-12 foot piece of Aircraft Aluminum 6061 T6. These were coated with a typical aircraft paint system purchased from DuPont. The system consisted of one coat of Imron 6000 Low VOC polyurethane enamel basecoat applied at 1 mil (0.001 inches) thick followed by one coat of 3440 Low VOC polyurethane clearcoat applied at 2 mils thick. These were allowed to cure for approximately 2 weeks at 100 F.
Paint Removal Procedure
A standard blast chamber equipped with a production size blastpot and a ¼-inch venturi nozzle (commonly used in the industry) on a ten foot, 1-inch blasting hose was used. The painted test panels from above were mounted on a steel plate with two-sided tape. They were blasted from a distance of 12 inches with a pressure of 100 psi.
Test 1
A 2268-gram quantity of 570 μm beads as prepared in Example 1 above, with a shell of colloidal silica, were placed in the equipment. Blasting at 100 psi continued until the abrasive stopped flowing; approximately 3.5 minutes. The paint was removed from the panel and the powder flow through the equipment was good. The panel was viewed with a 200× stereo zoom microscope. No damage to the aluminum panel was found.
Comparative Test 2
A 3629-gram quantity of beads without a shell of colloidal silica, for comparison, were placed in the blast pot. The material did not flow though the venturi nozzle.
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 spirit and scope of the invention. | This invention relates generally to methods for removing adherent materials, for example, paint, flashes, burrs, photoresists, contaminants, and other materials from various external surfaces. In particular, the method employs an improved media comprising core/shell particles. The media can be propelled against or along the surface by a gaseous or liquid carrier medium or a mixture of gas and liquid to remove the unwanted surface material. In one embodiment, suitable blasting equipment propels the media, via a pressurized air stream, against a surface of an object, for example an airplane skin, to dislodge the material to be removed. | 1 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a meter and disposable device for measuring the concentration of an analyte in a biological fluid; more particularly, an apparatus for which the disposable device is a hollow frustum.
2. Description of the Related Art
Medical diagnosis often involves measurements on biological fluids, such as blood, urine, or saliva, that are taken from a patient. Generally, it is important to avoid both contamination of equipment and personnel with these fluids and to avoid contamination of the patient with fluids from others. Thus, there is a need for diagnostic devices that minimize the risk of such contamination.
Among the medical diagnostic devices that are in most widespread use today is the blood glucose monitor. In the U.S. alone, there are an estimated 14 million people with diabetes. In order to avoid serious medical problems, such as vision loss, circulatory problems, kidney failure, etc., many of these people monitor their blood glucose on a regular basis and then take the steps necessary to maintain their glucose concentration in an acceptable range.
Blood contamination is of concern when making a blood glucose measurement. For example, when using the most common types of whole blood glucose meters (photometric), the glucose determination is generally made from a blood sample that is applied to a test strip that is on the meter. To apply the patient's finger-stick blood sample, the patient's finger must be positioned above and near to the test strip in order to inoculate the test strip with the blood sample. There is a risk that the patient's finger may come into contact with a portion of the meter that is contaminated with blood from previous use by others, particularly when used in a hospital.
This risk to the patient is minimized if the test strip is inoculated before it is placed into the meter. This is the so called "off-meter dosing" approach. With this approach, the patient applies his blood sample to a reagent test strip as the first step in the measurement process. Then the strip is inserted into the meter. The patient's finger only comes into contact with a new (clean) disposable, which cannot be contaminated by another patient's blood. The finger never comes into contact with a contaminated portion of the meter. The approach of off-meter dosing has been used for some time, particularly with meters that operate photometrically, as well as in systems that measure hematocrit. A disadvantage of off-meter dosing is that the meter cannot take a measurement at or before "time-zero", the time when the sample was applied to the strip. In a photometric meter, a reflectance reading prior to strip inoculation permits the meter to correct for variations in strip background color and positioning. The meter can also determine time-zero more directly and more accurately, which facilitates accurate measurements. By contrast, time-zero may be difficult or impossible to determine if the strip is inoculated off-meter.
Although off-meter dosing reduces the contamination problem for the patient, the meter can still become contaminated with blood. There is thus a risk to others who may come into contact with the contaminated meter, such as workers in a hospital and meter repair technicians. Furthermore, if the patient is being assisted by a healthcare worker, that worker could come into contact with the patient's blood while removing the strip for disposal, after the test has been completed.
Meters that operate electrochemically typically use "remote dosing", in which the test strip is placed in the meter before inoculation, but the blood application point is remote from the meter surfaces that can become contaminated. For example, the Glucometer Elite® from Bayer Diagnostics and the Advantage® from Boehringer Maruheim incorporate electrodes with remote sample application. As with off-meter dosing, strip removal may also pose a risk for meters that use remote dosing.
A number of systems have been disclosed that are aimed at reducing the risk of contamination to a patient and/or to others in connection with diagnostic tests.
U.S. Pat. No. 4,952,373, issued Aug. 28, 1990, to Sugarman et al., discloses a shield that is designed to prevent excess liquid on diagnostic cartridges from being transferred to a monitor with which the cartridge is used. The shield is fabricated from thin plastic or metallic film and is attached to a cartridge that is generally the size of a credit card.
U.S. Pat. No. 5,100,620, issued Mar. 31, 1992, to Brenneman, discloses an inverse funnel shaped body with a central capillary tube to transport a liquid sample from a remote sample-application point to a test surface. The device can be used to transfer blood from a finger stick to a reagent film.
U.S. Pat. No. 3,991,617, issued Nov. 16, 1976, to Marteau d'Autry discloses a device that is used with a pipette intended to be used with disposable tips. The device provides a push button mechanism for ejecting the tip from the end of the pipette.
The common element of the above patents is that each of the devices disclosed addresses the risk of contamination that is posed by biological fluids and other potentially hazardous liquids.
SUMMARY OF THE INVENTION
In accordance with the present invention, a device for use in an apparatus for measuring a concentration of an analyte in a sample of a biological fluid comprises
(a) a hollow frustum, having open ends of unequal size and
(b) a porous membrane for accepting the sample, attached to, and substantially closing, the smaller open end, the membrane comprising
(i) a surface for accepting the sample and
(ii) a reagent for reacting with the analyte to cause, in a physically detectable parameter of the membrane, a change that can be measured and be related to the concentration of the analyte in the sample.
A method of this invention for measuring a concentration of an analyte in a sample of a biological fluid comprises
(a) providing a device that comprises a hollow frustum having open ends of unequal size, whose smaller end is substantially closed by a membrane that has
(i) a surface for accepting the sample and
(ii) a reagent for reacting with the analyte to cause, in a physically detectable parameter of the membrane, a change that can be measured and be related to the concentration of the analyte in the sample;
(b) applying the sample to the membrane surface;
(c) measuring the change in the parameter; and
(d) determining the analyte concentration from the measurement of the parameter change.
The device of the present invention can be used advantageously with a meter for measuring a concentration of an analyte in a sample of biological fluid that is applied to a first surface of a porous membrane that contains a reagent, which reacts with the analyte to cause a change in reflectance of a second surface of the membrane, the membrane being attached to and substantially closing an end of a hollow frustum device. The meter comprises
(a) a body having a frustum-shaped distal section for mating engagement with the device, the section tapering inwardly to an end that faces the second surface of the membrane,
(b) an optical system in the body to direct a beam of light out from the distal end and to accept light reflected back from the second surface of the membrane,
(c) means for measuring the light reflected back into the body both before and after the sample is applied to the membrane, and
(d) means for computing the analyte concentration in the fluid from the measured values of reflected light.
The device of the present invention permits a person to measure the analyte concentration in a biological fluid, while minimizing the risk that the fluid or the user will come into contact with the measurement apparatus. Thus, the device reduces both the likelihood of contamination of the apparatus by the user and vice versa. The device is disposable, and the terms "device" and "disposable" are used interchangeably throughout this specification and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a device of this invention with a portion broken away for clarity;
FIG. 2 is a cross-sectional view taken along line 2--2 of FIG. 1;
FIG. 3 is a perspective view of a meter and device of the invention prior to their being attached;
FIG. 4 is a perspective view of the meter and device in the process of obtaining a blood sample;
FIG. 5 is a partial cross-sectional view of the meter and device of FIG. 4, taken along line 5--5 of FIG. 4;
FIG. 6 is a side view in partial cross section of a plurality of devices in a package;
FIG. 7 is a perspective view of a meter of this invention ejecting a device;
FIG. 8 is a longitudinal cross section, with certain parts in elevation for clarity, of the meter of FIG. 7 in a first, in-use, position;
FIG. 9 is a side elevational view, partially in cross section, of the meter of FIG. 7 in a second, ejection, position;
FIG. 10 is a perspective view of an alternate embodiment of a meter;
FIG. 11 is a perspective view of an alternate embodiment of a device of this invention;
FIG. 12 is a fragmentary perspective view of the distal end of the device of FIG. 11;
FIG. 13 is a cross-sectional view taken along line 13--13 of FIG. 12;
FIG. 14 is a cross-sectional view taken along line 14--14 of FIG. 12;
FIG. 15 is a cross-sectional view of a further embodiment of the distal end of a device of the invention;
FIG. 16 is a perspective view of another embodiment of a meter and device prior to their being attached;
FIG. 17 is another embodiment of a meter and device;
FIG. 18 is a perspective view of the distal end of a further embodiment of the meter and device;
FIG. 19 is a side view of the distal end of the meter and device of FIG. 18 shown in an assembled position.
DETAILED DESCRIPTION OF THE INVENTION
The device of the present invention is generally adapted for use in an apparatus for measuring the concentration of analytes, such as alcohol, cholesterol, proteins, ketones, enzymes, phenylalanine, and glucose, in biological fluids such as blood, urine, and saliva. For brevity, we describe the details for using the device in connection with self-monitoring of blood glucose; however, a person of ordinary skill in the art of medical diagnostics would be able to readily adapt the technology for measuring other analytes in other biological fluids.
Self-monitoring of blood glucose is generally done with meters that operate on one of two principles. The first is the photometric type, which is based on reagent strips that include a composition that changes color after blood is applied. The color change is a measure of the glucose concentration.
The second type of blood glucose monitor is electrochemical and operates on the understanding that blood applied to an electrochemical cell can cause an electrical signal--voltage, current, or charge, depending on the type of meter--that can be related to the blood glucose concentration.
The present invention permits convenient, remote dosing for both photometric and electrochemical systems. For brevity, the description below focuses on a photometric system. Similar devices can be used with an electrochemical system. With either type of system, the present device permits the meter to monitor the complete course of the reaction, from the time the sample is applied until a glucose determination is made. The ability to measure the test start time makes it easier to determine the glucose concentration accurately.
There are some advantages to using a photometric rather than an electrochemical system to make a glucose determination. One advantage of a photometric system is that measurements can be made at more than one wavelength of light, and corrections can be made for variations in blood hematocrit. The disposable disclosed here provides these advantages of the photometric system, while also permitting minimal meter contamination.
The disposables used in photometric measurement systems are generally made in the form of a thin rectangular strip. The shape derives from the original so-called "dip and read" test strip configuration. One end serves as a handle, while the chemical reaction with the fluid sample is carried out at the other end.
These rectangular disposables form the male portion of the interface with the meter. That is, the strip is retained by features on the meter that enclose the disposable. This method of retention invites contamination of the meter with the fluid sample.
In order to avoid the problems of contamination the present disposable takes the form of a hollow frustum, which provides the female portion of the interface with the meter. That is, the disposable encloses a portion of the meter and serves as a cover to prevent contamination of the meter by the fluid sample.
FIG. 1 depicts in partial cutaway an embodiment of this invention in which the disposable 10 is a hollow frustum of a cone. Membrane 12 is attached to the smaller end 14. Optional lip 16 provides a surface to which membrane 12 is attached with adhesive 18. Optional indentations 20 are spaced around the circumference of the cone to provide a retention mechanism, in conjunction with a groove on a meter.
FIG. 2 is a cross section of the disposable of FIG. 1 taken along the line 2--2. As shown in FIG. 2, the membrane is attached to the outside of the disposable. Alternatively, as shown in FIG. 11, the membrane may be attached to the inside of the disposable.
FIG. 3 is an exploded perspective view of a photometric meter and a disposable device of the type shown in FIG. 1. Meter 30 has an elongated configuration with a distal section 32 that is a substantially cylindrically symmetrical frustum, along whose perimeter is optionally a groove 34. Note that the disposable nests on the distal section of the meter in such a way that there is an accurately defined gap G between the distal end 36 of meter 30 and the bottom surface of membrane 12. The accurate positioning contributes to measurement precision and reliability. In the cutout can be seen a light source 38 and detector 40, which provide for illuminating a disposable and for detecting light reflected from the disposable, respectively. As discussed below, measuring light reflected from the disposable yields the glucose concentration in the sample applied to the membrane. Although only one source and detector are shown in FIG. 3, multiple sources, optionally having different output spectra, and/or multiple detectors may be used.
FIG. 4 is a perspective view of the way in which a device and meter of FIG. 3 can be used to obtain a sample S from a stuck finger tip. It is quite easy for the user to bring the disposable into contact with the finger, which is a big advantage for users that have impaired vision.
FIG. 5 is a cross section of part of distal section 32 of meter 30 and disposable 10, which illustrates the way indentations 20 and groove 34 positively locate meter 30 within disposable 10, leaving gap G. Note that gap G ensures that blood that penetrates through the membrane does not contaminate the meter. The gap dimension, while not critical, is preferably at least about 1/2 mm.
An advantage of the device of the invention, when used with a meter of the type shown in FIG. 3, is that the devices can be in a stack, nested conveniently in a container 42, as shown in FIG. 6. A device can then be secured simply by inserting the distal section 32 of meter 30 into container 42 and engaging groove 34 and indentations 20. After a test has been completed, a used disposable can be ejected into waste container W, as shown in FIG. 7, provided there is an optional push-button ejection mechanism.
Push-button ejection mechanisms of the type that are widely known and used are suitable for this invention (see e.g.; U.S. Pat. No. 3,991,617). One such mechanism is depicted in FIGS. 8 and 9, which show a push-button mechanism mounted in a meter of the type shown in FIG. 3. The elements of the mechanism include shaft 44, which joins ejector 46 and push button 48. Push button 48 works through shaft 44 to cause ejector 46 to disengage disposable 10 from the distal section 32 of meter 30. Spring 50 works to return the ejector 46 and push button 48 to their retracted position. Push-button ejection, by permitting the disposable to be removed without direct contact, helps to avoid contamination. Disposables to be used with push-button ejection mechanisms of the type shown in FIGS. 8 and 9 preferably have a flange 19.
FIG. 10 depicts an embodiment of a meter of this invention, which includes a display 50 for depicting the analyte concentration measured by the meter. The display can be a light-emitting diode (LED) display, a liquid crystal display (LCD), or similar display well known in the art.
Although the above description and Figs. contemplate a disposable having a circular cross section and meter having a distal section having a mating cross section, that geometry is not essential and, in fact, may not even be preferred. A primary consideration in selecting the geometry in a photometric system is the optical design. Generally, reflectometry dictates at least a minimum angular separation (typically 45°) between a detector and specularly reflected light. This, in turn requires at least a minimum vertex angle of the conical disposable. However, it is an advantage to a user to be able to view his/her finger for dosing, and a large vertex angle interferes with that view. Thus, a disposable having a rectangular cross section may be preferred, such as the hollow frustum of a rectangular pyramid 110 shown in FIG. 11. In that case, the angular separation between detector and specular-reflected light determines only the minimum feasible value of L, the longitudinal dimension of the larger open end. But the disposable could be smaller and provide less interference with a user's view of his/her finger. Furthermore, rectangular membranes can be fabricated from ribbons or sheets at less expense and with less waste of material. Nevertheless, a circular cross section is advantageous when an array of several sources and/or detectors is used in the optical system.
Since contamination is possible if excess sample were to drop from the disposable, it is desirable to accommodate large samples, without dripping. Various designs can serve to retain excess sample. One is shown in FIGS. 12,13, and 14. FIG. 12 depicts the disposable of FIG. 11 with indentations 124 on the small-end surface of the disposable. As shown in FIGS. 13 and 14, the indentations allow capillary flow to fill the resulting gap between the membrane and the top inside surface of the device. An alternative way of forming such gaps is to adhere the membrane to the disposable with thick adhesive, leaving gaps to accommodate the excess sample. Another way to absorb excess sample is to attach an absorbent pad 126 over the front surface of the membrane, as shown in FIG. 15.
FIG. 16 is an exploded perspective view of a meter and a disposable of the type shown in FIG. 11. The distal section 132 of meter 130 has an optional groove 134, which is similar to groove 34, for retaining the disposable. Elongated neck 130 facilitates pickup of disposables from the elongated containers 42 shown in FIG. 6. Display 150 depicts the measured analyte concentration.
FIG. 17 depicts an alternative embodiment of a meter adapted for use with the disposable of FIG. 11.
FIG. 18 depicts the distal portion of yet another embodiment of a disposable 210 and meter 230. Distal section 232 mates with disposable 210. Note that slots 234 are an alternative to groove 34 (or 134) for capturing indentations, such as 220, on the disposable.
FIG. 19 is a side view of the embodiment of FIG. 18.
In the method of this invention, a blood sample is picked up on the outward-facing surface of the membrane. Glucose in the sample interacts with a reagent in the membrane to cause a color change, which changes the reflectance of the inward-facing membrane surface. The light source in the meter illuminates the inward-facing membrane surface and measures the intensity of light reflected from that surface. Using the appropriate computation, the change in reflectance yields the glucose concentration in the sample.
A variety of combinations of membrane and reagent compositions are known for photometric determinations of blood glucose concentration. A preferred membrane/reagent composition is a polyamide matrix incorporating an oxidase enzyme, a peroxidase, and a dye or dye couple. The oxidase enzyme is preferably glucose oxidase. The peroxidase is preferably horseradish peroxidase. A preferred dye couple is 3-methyl-2 benzothiazolinone hydrazone hydrochloride plus 3,3-dimethylaminobenzoic acid. Details of that membrane/reagent combination and variations on it appear in U.S. Pat. No. 5,304,468, issued Apr. 19, 1994, to Phillips et al., incorporated herein by reference.
Another preferred membrane/reagent composition is an anisotropic polysulfone membrane (available from Memtec America Corp., Timonium, Md.) incorporating glucose oxidase, horseradish peroxidase, and the dye couple 3-methyl-2-benzothiazolinone hydrazone! N-sulfonyl benzenesulfonate monosodium combined with 8-anilino-1-naphthalene sulfonic acid ammonium. Details of that membrane/reagent combination and variations on it appear in U.S. patent application Ser. No. 08/302,575, filed Sep. 8, 1994, incorporated herein by reference.
It will be understood by those skilled in the art that the foregoing descriptions of embodiments of this invention are illustrative of practicing the present invention but are in no way limiting. Variations of the detail presented herein may be made without departing from the scope and spirit of the present invention. | A hollow, frustum-shaped disposable device is used in an apparatus for measuring the concentration of an analyte in a sample of a biological fluid. The smaller end of the frustum has a porous membrane, to which a sample of the fluid may be applied. Preferably, a reagent in the membrane reacts with the analyte to cause a color change. The device is mounted on a meter, which measures the color change and computes from the change the analyte concentration in the sample. The apparatus permits remote dosing of the device, which minimizes the likelihood of cross-contamination between the user and the meter. Devices can be mounted on the meter and released from the meter without touching them, to further protect against contamination. | 6 |
AREA OF INVENTION
[0001] The present invention relates to a method of operating an assembly of heat exchangers for subcritical and transcritical conditions, by initially arranging at least two heat exchangers in parallel for the subcritical condition, and to an assembly of heat exchangers.
BACKGROUND OF INVENTION
[0002] In a conventional refrigeration system, heat release from the refrigerant is based on condensation of the refrigerant. The temperature is a critical point, which being constant during condensation. Operating an assembly of heat exchangers below the critical point is defined as subcritical mode. It is previously known to arrange heat exchangers in parallel at such subcritical mode.
[0003] However, in heat pump and refrigeration applications using CO2 as refrigerant there is a need to operate in transcritical mode, i.e. above the critical point as well as below the critical point. Transcritical refrigeration systems with CO2 as a refrigerant are well known in the art. The critical temperature of CO2 is 31.0° C. and the critical pressure is 73.8 bar. At higher temperatures and pressures no clear distinction can be drawn between liquid and vapour, and CO2 is said to be in the so-called super-critical fluid region. The thermal conditions for these two operation modes are dramatically different. During transcritical mode the flow rates of the cold side, typically brine or water, are much lower than during subcritical mode. Thermally the process on the hot side of the refrigerant is also very different. In transcritical mode large temperature drops is required with close approach at pinch point and outlet. All together this calls for two different designs of the heat exchanger to be able to operate the system in an optimal way.
[0004] Considering the temperature difference needed in a heat exchanger, i.e. approximate 10° C., the upper limit for heat release based on condensation of CO2 will be around 20° C. ambient temperature. Below this temperature, the CO2 stays below the critical point and the refrigeration system operates in subcritical mode. For refrigeration systems used in supermarkets, the ambient temperature will exceed 20° C. during the summer in a large part of the world. At these temperatures, cooling of the CO2 is a single-phase cooling, namely a gas cooling. CO2 is above the critical point at the high pressure side of the system, and the refrigeration system operates in transcritical mode.
[0005] The efficiency and the cooling capacity of the refrigeration system are lower in transcritical operation than in subcritical operation. It is an important disadvantage of known CO2 refrigeration systems that they have a lowered performance at elevated ambient temperatures above approximately 20° C., i.e. when a high performance is actually desired. It is an object of the present invention to provide a transcritical refrigeration system with improved performance during transcritical operation.
DISCLOSURE OF INVENTION
[0006] It is an object of the present invention to constitute a solution to the problem, of the contradictory requirements for heat exchanger design for gas coolers and condensers. Instead of finding a design for a heat exchanger that typically is determined by subcritical conditions and then use it for transcritical operation one may use multiple heat exchangers in the system.
[0007] According to a first aspect of the present invention, these objects are achieved by arranging at least one heat exchanger at a transcritical condition in series with the other heat exchangers, and arranging an inlet and an outlet at opposite ends of the assembly, and switching the heat exchangers between being arranged in parallel to being arranged in series by closing a first conduit, connecting said inlet to a first duct of each heat exchanger, after the first heat exchanger and between every second heat exchanger, and a second conduit, connecting said outlet to a second duct of each heat exchanger, between the other heat exchangers.
[0008] The method include the use of multiple heat exchangers in parallel during condensation and then change to use them in serial or a combination serial and parallel during transcritical operation.
[0009] This improves system efficiency substantially in transcritical mode as the thermal length and heat transfer increases and thus the outlet temperature of the refrigerant can be lowered.
[0010] In addition, switching the heat exchangers between being arranged in parallel to being arranged in series by closing a first conduit, which connecting said inlet to a first duct of each heat exchanger, after the first heat exchanger and between every second heat exchanger, and a second conduit, which connecting said outlet to a second duct of each heat exchanger, between the other heat exchangers.
[0011] By providing said heat exchangers with a dual-circuit for heat transfer between two essentially liquid media, such as a refrigerant and brine, it is an advantage of switching each circuit between being arranged in parallel to being arranged in series.
[0012] By this the flexibility is increased and makes it possible to optimize the performance of the system both for subcritical as well as transcritical mode.
[0013] Another aspect of the invention is an assembly of heat exchangers having an inlet and an outlet at opposite ends of the assembly, a first conduit connected to said inlet and to a first duct of each heat exchanger and a second conduit connected to said outlet and a second duct of each heat exchanger, characterised in that a valve being located in the first conduit after the first heat exchanger and between every second heat exchanger and in the second conduit between the other heat exchangers, wherein the heat exchangers being arranged in parallel having all valves in open position and in series having all valves in closed position.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] This and other aspects of the present invention will now be described in more detail, with reference to the appended drawings showing a currently preferred embodiment of the invention.
[0015] FIG. 1 a shows a schematically view of an assembly of heat exchangers according to a first parallel arranged operating condition according to the present invention.
[0016] FIG. 1 b shows a temperature/position chart for the operating condition according to FIG. 1 a.
[0017] FIG. 2 a shows a schematically view of the assembly of heat exchangers according to a second serial arranged operating condition according to the present invention.
[0018] FIG. 2 b shows a temperature/position chart for the operating condition according to FIG. 2 a.
DETAILED DESCRIPTION OF EMBODIMENTS
[0019] FIGS. 1 a and 2 a shows an assembly 1 of heat exchangers 2 . The heat exchangers 2 each have a dual-circuit for heat transfer between two essential liquid media, such as a refrigerant and brine. However, the present invention is also applicable in heat exchangers with only one liquid media. The assembly 1 of heat exchangers 2 having an inlet A, e.g. from a compressor (not shown) in a refrigerant circuit, and an outlet B, e.g. to an expansion valve (not shown), at opposite ends of the assembly 1 . The assembly 1 having a corresponding inlet C and outlet D for the brine circuit at opposite ends of the assembly 1 . In addition, the assembly 1 having a first conduit 4 connected to said inlet A and to a first duct 5 of each heat exchanger 2 , and a second conduit 6 connected to said outlet B and a second duct 7 of each heat exchanger 2 . Further, a valve 3 being located in the first conduit 4 , after the first heat exchanger 2 and between every second heat exchanger 2 , and in the second conduit 6 between the other heat exchangers 2 , wherein the heat exchangers 2 being arranged in parallel having all valves 3 in open position, as shown in FIG. 1 a, and in series having all valves 3 in closed position, as shown in FIG. 2 a.
[0020] In FIG. 1 a the heat exchangers 2 are arranged in parallel for the subcritical condition, i.e. at a temperature below the condensing condition of the refrigerant. The heat transfer is shown in FIG. 1 b, wherein the upper curve corresponds to the temperature drop from inlet A to outlet B of the refrigerant, which during condensation having a more or less constant temperature, and the lower curve corresponds to the temperature rise from inlet C to outlet D of the brine. In FIG. 2 a the heat exchangers 2 are arranged in series with each other at a transcritical condition, i.e. at a temperature above condensing condition of the refrigerant. The heat transfer is shown in FIG. 2 b , wherein the upper curve corresponds to the temperature drop from inlet A to outlet B of the refrigerant, and the lower curve corresponds to the temperature rise from inlet C to outlet D of the brine. The heat exchangers 2 are switched between being arranged in parallel to being arranged in series by closing valves 3 arranged alternating in a first conduit 4 , connected to a first duct 5 of each heat exchanger 2 , between each second heat exchanger and in a second conduit 6 , connected to a second duct 7 of each heat exchanger 2 , between the other heat exchangers 2 .
[0021] The brine circuit (not shown) having a corresponding conduit 8 and a conduit 9 , communicating with the inlet C and the outlet D, respectively, and valves 10 . The brine circuit may likewise be switched between being arranged in parallel to being arranged in series. The valves 10 being located in the conduit 8 , after the first heat exchanger 2 referred to the inlet C and between every second heat exchanger 2 , and in the second conduit 9 between the other heat exchangers 2 , wherein the heat exchangers 2 being arranged in parallel having all valves 10 in open position, as shown in FIG. 1 a, and in series having all valves 10 in closed position, as shown in FIG. 2 a.
[0022] The person skilled in the art realizes that the present invention by no means is limited to the preferred embodiments described above. On the contrary, many modifications and variations are possible within the scope of the appended claims. For example only one circuit of the dual-circuit heat exchanger may be operated according to the present invention. | The present invention refers to a method of operating an assembly ( 1 ) of heat exchangers ( 2 ) for subcritical and transcritical conditions, by initially arranging at least two heat exchangers ( 2 ) in parallel for the subcritical condition. | 5 |
STATEMENT OF GOVERNMENT RIGHTS
This work was supported in part by Sandia National Laboratory under contract number BE-7471. The government may have certain rights in the invention.
BACKGROUND OF THE INVENTION
Micro-electro-mechanical system devices (MEMS) are usually made from inorganic materials using semiconductor technologies. Examples of commonly used inorganic material for MEMS devices include silicon, silicon oxide, silicon nitride, and aluminum. These inorganic materials possess high surface energy. As a result, the surfaces often stick together when they come into contact. This problem is particularly significant because the surface-area to volume ratio scales with the inverse of device dimension and this ratio is very large for MEMS devices with typical dimensions on the micrometer scale.
A well-known surface related problem in the fabrication and operation of MEMS devices is stiction, which occurs when the surface adhesion force overcomes the mechanical restoring force of microstructures. Stiction is one of the leading causes of device failure in the MEMS industry. One example of a MEMS device currently in commercial use is the digital mirror device (DMD) of Texas Instruments. The DMD consists of ˜1,000,000 micro-mirrors. During operation, each mirror is rotated ±10° to reflect light from a source to the screen; this rotation brings the mirror assembly (specifically, the tip of the yoke on which the mirror is mounted) into contact with the substrate and stiction can occur. Another example of a commercial product utilizing MEMS technology is the airbag sensor of Analog Devices. The airbag sensor, also called accelerometer, consists of a movable component which responses to changes in inertial during collision. However, the movable component may become stuck to other fixed component in its immediate environment resulting in device failure.
One approach to solve the stiction problem has been to apply a passivation, organic coating to the surfaces of MEMS devices. Organic coatings consisting of hydrocarbon or fluorocarbons are generally characterized by low surface energy. When surfaces with such low energy coatings come into contact, the adhesion energy is substantially reduced as compared to the uncoated, inorganic surfaces. The lowering of surface energy helps to alleviate the stiction problem.
Another approach to apply a passivating coating onto a MEMS devices involves the introduction of an organic material, phenyl-siloxane in particular. Still another approach has been to utilize a combination of an organic material and moisture with a MEMS device in a sealed package and heating the package to a high temperature to form a passivation coating on the surface of the MEMS device. This type of coating has been applied to accelerometers (airbag sensors) where contacts between different components on a MEMS device are infrequent. Thus emphasis of this method has been on thermal stability of the coating to be compatible with packaging temperature, rather than achieving the lowest possible surface energy or the highest mechanic stability.
Therefore, there remains a need in the art for improved methods and coatings applicable to a MEMS device that provide for robust coatings and the reduction or, preferably, elimination of stiction.
BRIEF SUMMARY OF THE INVENTION
This present invention provides methods of coating and coatings to modify surfaces of micro-electro-mechanical system (MEMS) devices. MEMS devices are sometimes referred to as micro-opto-electro-mechanical systems (MOEMS), micro-machines, micro-machined sensors and actuators, or microsystems, all of which are included within the scope of this invention. More particularly, the invention deals with forming robust and low energy surface coatings on MEMS devices.
In one aspect, the present invention provides methods for the formation of organic coatings, particularly low-energy coatings, on MEMS devices. Preferably, the methods can be used to form composite coatings, each consisting of at least two types of regions. A first region where the adsorbed molecules to the MEMS surface are extensively cross-linked (oligomeric or polymeric) and a second region, where each adsorbed molecule is covalently bonded to the surface. More particularly, the coatings are of monolayer nature. Such coatings are most desirable as anti-stiction coatings in MEMS devices where frequent mechanical contacts are required during operation.
The present invention focuses on treating a surface of a MEMS device with a coating material or materials in one or two reactive components. In either case, the coated MEMS device is subjected to heat to help facilitate the desired anti-stiction properties. For example, the MEMS device is treated with either SiX 3 R and/or SiX 2 R 2 (in gaseous form or as a solution) and then subjected to a heat treatment. In one aspect, SiX 3 R (gaseous or in solution) is coated onto the MEMS device and then subjected to elevated temperatures in the presence of SiXR 3 ″ (gaseous or in solution). In another aspect, SiX 2 R 2 (gaseous or as a solution) is coated onto the MEMS device and then subjected to elevated temperatures in the presence of SiXR 3 ″ (gaseous or in solution). Alternatively, both SiX 3 R and SiX 2 R 2 (gaseous or in solution) are coated onto the MEMS device and then subjected to elevated temperatures in the presence of SiXR 3 ″ (gaseous or in solution). The resultant coating can be a thin film or a self-assembled monolayer (SAM).
In one embodiment, the present invention provides methods for application of a composite coating to the surface of a MEMS device in two steps. First, a self assembled monolayer is formed from SiX 3 R (gaseous or in solution), wherein R is an organic group, e.g., R is a linear or branched, substituted or unsubstituted alkyl or aryl group, and each X, individually, is Cl or OR′, wherein R′ is an alkyl group (e.g., CH 3 — or C 2 H 5 —). A suitable example of SiX 3 R is 1H,1H,2H,2H-perfluorooctyl trimethoxysilane (PFOTMS), i.e., CF 3 (CF 2 ) 5 CH 2 CH 2 Si(OCH 3 ) 3 .
In a second step, the surface is exposed at elevated temperatures to SiXR″ 3 (gaseous or in solution) wherein each R″ is independently an organic group (R″ is a linear or branched, substituted or unsubstituted alkyl or aryl group) and X is Cl, H, or OR′ and R′ is an alkyl group (e.g., CH 3 — or C 2 H 5 —). A suitable example of SiXR″ 3 is 1H,1H,2H,2H-perfluorooctyl dimethyl methoxysilane (PFODMMS), CF 3 (CF 2 ) 5 CH 2 CH 2 Si(CH 3 ) 2 OCH 3 .
In another embodiment, the present invention provides for application of a composite coating to the surface of a MEMS device in a two step process. First, a coating is formed from SiX 3 R (gaseous or in solution), wherein R is an organic group (R is a linear or branched, substituted or unsubstituted alkyl or aryl group) and each X, independently of each other, is Cl or OR′, and R′ is an alkyl group (e.g., CH 3 — or C 2 H 5 —). In a second step, the surface is heated to elevated temperatures to enable formation of cross-linked and surface attached regions.
In still another embodiment, the present invention provides for application of a composite coating to the surface of a MEMS device in a two step process. First, an oligomeric or polymeric thin film is formed from SiX 3 R or SiX 2 R 2 (gaseous or in solution), wherein each R, independently, is an organic group (e.g., R is a linear or branched, substituted or unsubstituted alkyl or aryl group) and each X, independently, is Cl or OR′ and R′ is an alkyl group (e.g., CH 3 — or C 2 H 5 —). In a second step, the surface is exposed at elevated temperatures to SiXR″ 3 (gaseous or in solution) wherein each R″ is independently an organic group (e.g., R″ is a linear or branched, substituted or unsubstituted alkyl or aryl group) and X is Cl, H, or OR′.
While multiple embodiments are disclosed, still other embodiments of the present invention will become apparent to those skilled in the art from the following detailed description, which shows and describes illustrative embodiments of the invention. As will be realized, the invention is capable of modifications in various obvious aspects, all without departing from the spirit and scope of the present invention. Accordingly, the drawings and detailed description are to be regarded as illustrative in nature and not restrictive.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic illustration of a composite monolayer prepared by a method of the invention and consists of regions (A) where molecules are extensively cross-linked with a small number of anchoring bonds to the surface, and regions (B) where each molecule is individually anchored to the surface.
FIG. 2 compares tribological results between a composite monolayer prepared from 1H,1H,2H,2H-perfluorooctyl triethoxysilane (PFOTES) and 1H,1H,2H,2H-perfluorooctyl dimethyl methoxysilane (PFODMES) on a Si(111) surface and a one-component monolayer prepared from PFOTES on Si(111). The composite monolayer is labeled AB/Si(111) (upper panel) and the PFOTES monolayer as A/Si(111) (lower panel). The measurements were carried out on an Interfacial Force Microscope (IFM) at Sandia National Laboratory, with a gold coated tungsten tip of ˜5 micrometer diameter. The lines are normal force (in μN) and the dots are frictional force (μN, uncalibrated). The x-axis is tip-surface distance (d). The zero value is the equilibrium position when the normal force is most negative (adhesion force). The d<0 value corresponds to attractive region and the d>0 value corresponds to repulsive region.
FIG. 3 compares tribological results between a composite monolayer prepared from 1H,1H,2H,2H-perfluorooctyl triethoxysilane (PFOTES) and 1H,1H,2H,2H-perfluorooctyl dimethyl methoxysilane (PFODMES) on a Si(111) surface and a one-component monolayer prepared from PFODMES on Si(111). The composite monolayer is labeled AB/Si(111) (upper panel) and the PFODMES monolayer as B/Si(111) (lower panel). The measurements were carried out on an Interfacial Force Microscope (IFM) at Sandia National Laboratory, with tungsten tip of ˜3.8 micrometer diameter. The lines are normal force (in mN) and the dots are frictional force (μN, uncalibrated).
DETAILED DESCRIPTION
The present invention provides methods for the formation of organic coatings on MEMS devices. In one aspect, the methods can be used to form composite coatings. A composite coating is defined as one which consists of at least two types of regions: those where the adsorbed molecules are extensively cross-linked (oligomeric or polymeric) and those where each adsorbed molecule is covalently bonded to the surface. Oligomeric is defined as involving less than 10 cross-linked bonds and polymeric is defined as involving more than 10 cross linked bonds.
In another aspect of the invention, the coatings provided by the methods of the invention are monolayer films having substantially molecular thickness. The molecules forming the monolayer are chemically and thermally stable at room temperature (with vaporization temperatures preferably above room temperature, and more particularly below 400° C.), and are soluble in an organic solvent such as iso-octane in an amount of at least about 1×10 −6 mole/liter.
The composite coatings possess low energy surface characteristics. In this context, “low energy” means that the water contact angle of the surface is 90 degrees or larger. Such coatings also form passivation layers. In this context, a “passivation layer” is one that possesses generally low chemical reactivity towards the adsorption of or reaction with chemical species in ambient conditions and within a packaged environment. Thus, the coatings provided by the methods of the present invention are mechanically stable and can withstand more than 10 9 cycles of contacts, such as the operation of a DMD, without stiction. These coatings provided by the methods of the invention are thermally stable at temperatures as high as 200° C., and more preferable up to 400° C., for example.
The surfaces of various materials used in MEMS devices can be modified according to the present invention. These materials include metals, semiconductors, as well as various chemical variants of metals and semiconductors, such as alloys, oxides, nitrides, carbides, ceramics, and combinations thereof. More specifically, the materials include silicon, silicon oxide, silicon nitride, aluminum, aluminum alloys, aluminum oxide, aluminum nitride.
Each silane monomer (organic precusor) used in the coating processes of the invention contains two major portions: a functional group to provide low surface energy (e.g., a hydrocarbon or fluorocarbon group to provide “wax-like” or “Teflon-like” surfaces); and a second reactive group.
Suitable hydrocarbon groups include substituted and unsubstituted, branched and linear alkyl groups having from about 1 to about 20 carbon atoms. The term “alkyl” refers to the radical of saturated aliphatic groups, including straight-chain alkyl groups, branched-chain alkyl groups, cycloalkyl (alicyclic) groups, alkyl substituted cycloalkyl groups, and cycloalkyl substituted alkyl groups. In particular, cycloalkyls have from about 4–10 carbon atoms in their ring structure, and more particularly have 5, 6 or 7 carbons in the ring structure.
In another embodiment, hydrocarbon portion of the organic precursor could be an aryl group. The term “aryl” as used herein includes 5- and 6-membered single-ring aromatic groups that can include from zero to four heteroatoms, for example, benzene, pyrrole, furan, thiophene, imidazole, oxazole, thiazole, triazole, pyrazole, pyridine, pyrazine, pyridazine and pyrimidine, and the like. Aryl groups also include polycyclic fused aromatic groups such as naphthyl, quinolyl, indolyl, and the like. Those aryl groups having heteroatoms in the ring structure may also be referred to as “aryl heterocycles”, “heteroaryls” or “heteroaromatics”. Aryl groups can also be fused or bridged with alicyclic or heterocyclic rings, which are not aromatic so as to form a polycycle (e.g., tetralin). The aromatic ring can be substituted at one or more ring positions with substituents that are hydrophobic in nature as described below.
Substituents suitable for substitution on the aryl group or alkyl group, are for example, halogen, alkoxy, alkylcarbonyloxy, arylcarbonyloxy, alkoxycarbonyloxy, aryloxycarbonyloxy, perfluoroalkyl, trifluoromethyl, aralkyl, or an aromatic or heteroaromatic moiety.
In particular, fluorocarbon groups are within the scope of the invention and are included as both alkyl type groups and aryl type groups. The fluorocarbon group can include one or more positions of the alkyl or aryl group substituted with a fluorine group. Where more than one hydrogen atom has been replaced with a fluorine group, the resultant moiety is perfluorinated. Suitable examples of perfluorinated alkyls are those that include two methylenes (CH 2 ) groups adjacent to the Si moiety (the remainder of the alkyl chain being perfluorinated) or fully fluorinated.
The term “reactive group” of a silane is intended to mean those moieties that will react with a component of the MEMS device surface, such as a hydroxyl group or an oxide layer. Suitable reactive groups include, for example, halogen atoms (chloride, fluoride, iodide, bromide), hydride (H) and OR′, wherein OR′ is defined below.
There are two types of silane groups selected for the composite coating: those that selectively attach to the solid surface of interest and those that attach to each other for cross-linking as well as to the surface. An example for the first type of molecules is 1H,1H,2H,2H-perfluorooctyl dimethyl methoxysilane, i.e., CF 3 (CF 2 ) 5 CH 2 CH 2 Si(CH 3 ) 2 OCH 3 . An example for the second type of precursor molecule is 1H,1H,2H,2H-perfluorooctyl trimethoxysilane, i.e., CF 3 (CF 2 ) 5 CH 2 CH 2 Si(OCH 3 ) 3 . Both types include a perfluorinated group.
In particular, the silane groups that provide low surface energy are those, which contain straight chain alkyl groups, which are capable of forming a close-packed monolayer where each alkyl group is in van der Waals contacts with neighboring alkyl groups. These straight chain alkyl groups can be of any length desired for the particular application and are, in particular, fully fluorinated or partially fluorinated with CF 3 termination.
The present invention provides anti-stiction and passivation coatings for MEMS devices, in part, because the coating is sufficiently thin, particularly on the order of a few nanometers and more specifically a monolayer. A monolayer corresponds to a closely packed molecular film with thickness no more than one of the dimensions (typically the length) of the film forming molecule. Such nanometer thickness ensures that the presence of the coating does not appreciably affect the mechanical properties of the MEMS structure and does not result in electrostatic charging within the organic coating. Surprisingly, there have been no demonstrations of covalently bonded organic coatings with nanometer scale thickness that can survive the large number (>10 9 ) of mechanical contacts required for some MEMS devices until the present methods and coatings provided by this invention.
In contrast to the present invention, siloxane self-assembled monolayers (SAMs) formed from alkyltrichlorosilane or alkyltrialkoxylsilanes as passivation coatings for MEMS, fail as anti-stiction coatings after repeated contacts, particularly in the presence of high humidity. Not to be limited by theory, it is believed that the mechanism of SAM formation from alkyltrichlorosilane or alkyltrialkoxylsilanes proceeds by the initial conversion of Si—X (X═Cl, or —OR, where R is a methyl or ethyl group) groups on the silane molecule to Si—OH groups. Under ideal conditions, a Langmuir like monolayer is formed on the hydrophilic surface with the presence of a thin water film. A cross-linked surface assembly is then formed by condensation reactions between the —OH groups on the silane molecules with those on the oxide surface or on neighboring silanes. Complications arise because close-packing of alkyl groups is incompatible with cross-linking between neighboring Si—OH groups within the monolayer and there is competition between cross linking and surface attachment. As a result, the siloxane SAM may consist of extensively cross-linked molecules, but with few covalent bonds to the surface. Such a monolayer is poorly attached to the substrate surface and, under repeated mechanical contacts, may roll-up and form clumps on the surface. This is a generally accepted mechanism for the failure of anti-stiction properties. The availability of three reactive groups on each silane molecule also leads to the easy formation of polymeric and other microstructures that are not desirable for MEMS devices. The present invention circumvents many of these issues.
Digital mirror devices (DMDs) require stringent application, where components on a MEMS structure come into frequent contact, e.g., tens or hundreds of billion (10 10-11 ) cycles during the lifetime of the device. It is of critical importance that the organic passivation coating not only provides low surface energy, but also possesses sufficient mechanical stability to survive the large number of contacts. The present invention affords such protection. In contrast, a method currently employed in DMD production is to form a low energy coating involving an oriented monolayer that includes —COOH and —CF 3 end groups, e.g., a perfluorodecanoic acid (PFDA) molecule, attached to the surface of a MEMS device during the packaging stage. An excess amount of these molecules is added to the package to provide a background pressure of PFDA; the reversible adsorption/desorption of these molecules from the surfaces provides a self-repair mechanism, thus allowing the operation of the device for 10 11 cycles without stiction failure. However, due to the weak bonding between the —COOH group and the surface, the monolayer is susceptible to moisture attack, thermal decomposition, and evaporation. These necessitate the use of hermetically sealed packages and relatively low operating temperatures. The perfluorodecanoic acid molecule is also corrosive towards some materials commonly used in MEMS devices. Thus, the use of such compounds during the packaging process to coat the surfaces is undesirable for some MEMS products. Advantageously, the present invention circumvents many of the disadvantages of the current known methods and coatings.
In one embodiment, the present invention provides methods of applying a coating to the surface of a MEMS device that includes a first step of contacting the surface of the MEMS device with a silane of the formula SiX 3 R. The silane can be applied to the surface as a gas, a liquid, or in solution.
In a second step, the coated surface is then heated at an elevated temperature. This method provides improved anti-stiction properties to the coated surface. In one aspect, a thin film can be formed on the surface of the MEMS device. In another aspect, a self-assembled monolayer (SAM) can be formed on the surface of the MEMS device as described below.
For SiX 3 R, R is a linear or branched, substituted or unsubstituted alkyl or aryl group and each X, independently, is a halogen atom, hydrogen, or OR′. R′ is a linear or branched, substituted or unsubstituted alkyl or aryl group. A suitable example of SiX 3 R is 1H,1H,2H,2H-perfluorooctyl trimethoxysilane (PFOTMS), i.e., CF 3 (CF 2 ) 5 CH 2 CH 2 Si(OCH 3 ) 3 .
The temperature of the reaction in the first step is one that can be appropriate for the formation of a self-assembled monolayer on the surface of the MEMS device(s). The temperature of this reaction is generally from about 0° C. to about 40° C., and more particularly from about 10° C. to about 25° C. The partial pressure of the silane at the reaction temperature is at least about 1×10 −6 atmospheres (atm), and more particularly at least about 1×10 −3 atm.
This process is known to be able to form a self-assembled monolayer (SAM) of RSi(OH) 3 , with limited number of intermolecular cross-linking (Si—O—Si) or bonding to the surface (—Si—O-Surface) (see., e.g., A. Y. Fadeev, T. J. McCarthy, Langmuir 2000, 16, 7266–7274; J. Genzer, K. Efimenko, D. A. Fischer, Langmuir 2002, 19, 9307–9311). The SAM usually forms via an island growth mechanism, leading to incomplete monolayers with patchy structures and a large number of vacancies (see, e.g., J. Y. Huang et al. Langmuir 1997, 13, 58; D. H. Flinn, D. A. Guzonas, R.-H. Yoon, Colloids Surf. 1994, 87, 163; R. Banga, et al. Langmuir 1997, 13, 58; A. G. Richer et al. Langmuir 1998, 14, 5980; C. Carraro, O. W. Yauw, M. M. Sung, R. Maboudian, J. Phys. Chem. 1998, 102, 4441).
Alternatively, the temperature of the reaction in the first step is one that can be appropriate for the formation of a thin film on the surface of the MEMS device(s). The temperature of this reaction is generally from about 0° C. to about 300° C. The partial pressure of the silane at the reaction temperature is at least about 1×10 −6 atmospheres (atm), and more particularly at least about 1×10 −3 atm. For some R groups, such as alkyls shorter than n-decyl, this process is known to be able to form oligomeric siloxane thin films on the surface (see., e.g., A. Y. Fadeev, T. J. McCarthy, Langmuir 2000, 16, 7266–7274).
The temperature of the second step is generally from about 50° C. to about 350° C., more particularly from about 80° C. to about 250° C., and even more specifically from about 100° C. to about 200° C., e.g. about 150° C. The pressure of the silane at the reaction temperature is generally at least about 1×10 −6 atmospheres (atm), more particularly at least about 1×10 −3 atm, even more specifically about 1 atm.
The afore-mentioned methods with SiX 3 R can further include in the second step, the heating step, an environment that contains at least one compound having the formula SiXR″ 3 . Each R″, independently, is a linear or branched, substituted or unsubstituted alkyl or aryl group and X is a halogen atom, H, or OR′. R′ is as defined above. A suitable example of SiXR″ 3 is 1H,1H,2H,2H-perfluorooctyl dimethyl methoxysilane (PFODMMS), CF 3 (CF 2 ) 5 CH 2 CH 2 Si(CH 3 ) 2 OCH 3 . The silane can be added as a gas, a liquid, or in solution.
Contact of the surface of the above siloxane coated MEMS device at elevated temperatures with one or more compounds of the formula SiXR″ 3 provides extensive cross-linking (Si—O—Si) and bonding to the surface (—Si—O-Surface) within islands of the siloxane oligomers. SiXR″3 reacts with surface vacancy sites to form surface anchored R″ 3 Si—O-surface species. SiXR″3 also reacts with un-reacted Si—OH groups within islands of oligomeric siloxane.
The result of the two steps described above for SAMs (treated with both SiX 3 R and SiXR″ 3 ) is a composite monolayer, illustrated in FIG. 1 , consisting of two types of regions: (A) cross-linked regions with a small number of anchoring bonds to the surface, and (B) strongly anchored regions where each molecule is individually bonded to the surface. The composite nature of the monolayer provides much enhanced mechanical stability, as compared to coatings of pure (A) or (B).
Alternatively, the result of the two steps described above for a thin film (treated with both SiX 3 R and SiXR″ 3 ) is a thin film composite coating consisting of regions of oligomeric siloxane from SiX 3 R and regions of R″ 3 Si—O— bonded to the surface or oligomeric siloxane.
In another embodiment, the present invention provides methods of applying a coating to the surface of a MEMS device that includes a first step of contacting the surface of the MEMS device with a silane of the formula SiX 2 R 2 . The silane can be applied to the surface as a gas, a liquid, or in solution.
In a second step, the coated surface is then heated at an elevated temperature. This method provides improved anti-stiction properties to the coated surface. In one aspect, a thin film can be formed on the surface of the MEMS device. In another aspect, a self-assembled monolayer (SAM) can be formed on the surface of the MEMS device as described below.
For SiX 2 R 2 , each R, independently, is a linear or branched, substituted or unsubstituted alkyl or aryl group and each X, independently, is a halogen atom, hydrogen, or OR′. R′ is a linear or branched, substituted or unsubstituted alkyl or aryl group.
The temperature of the reaction in the first step is one that can be appropriate for the formation of a self-assembled monolayer on the surface of the MEMS device(s). The temperature of this reaction is generally from about 0° C. to about 40° C., and more particularly from about 10° C. to about 25° C. The partial pressure of the silane at the reaction temperature is at least about 1×10 −6 atmospheres (atm), and more particularly at least about 1×10 −3 atm.
This process, as described above, is known to be able to form a self-assembled monolayer (SAM) of RSi(OH) 3 , with limited number of intermolecular cross-linking (Si—O—Si) or bonding to the surface (—Si—O-Surface) (see., e.g., A. Y. Fadeev, T. J. McCarthy, Langmuir 2000, 16, 7266–7274; J. Genzer, K. Efimenko, D. A. Fischer, Langmuir 2002, 19, 9307–9311). The SAM usually forms via an island growth mechanism, leading to incomplete monolayers with patchy structures and a large number of vacancies (see, e.g., J. Y. Huang et al. Langmuir 1997, 13, 58; D. H. Flinn, D. A. Guzonas, R.-H. Yoon, Colloids Surf. 1994, 87, 163; R. Banga, et al. Langmuir 1997, 13, 58; A. G. Richer et al. Langmuir 1998, 14, 5980; C. Carraro, O. W. Yauw, M. M. Sung, R. Maboudian, J. Phys. Chem. 1998, 102, 4441).
Alternatively, the temperature of the reaction in the first step is one that can be appropriate for the formation of a thin film on the surface of the MEMS device(s). The temperature of this reaction is generally from about 0° C. to about 300° C. The partial pressure of the silane at the reaction temperature is at least about 1×10 −6 atmospheres (atm), and more particularly at least about 1×10 −3 atm. For some R groups, such as alkyls shorter than n-decyl, this process is known to be able to form oligomeric siloxane thin films on the surface (see., e.g., A. Y. Fadeev, T. J. McCarthy, Langmuir 2000, 16, 7266–7274).
The temperature of second step is generally from about 50° C. to about 350° C., more particularly from about 80° C. to about 250° C., and even more specifically from about 100° C. to about 200° C., e.g. about 150° C. The pressure of the silane at the reaction temperature is generally at least about 1× 10 −6 atmospheres (atm), more particularly at least about 1×10 −3 atm, even more specifically about 1 atm.
The afore-mentioned methods with SiX 2 R 2 can further include in the second step, the heating step, an environment that contains at least one compound having the formula SiXR″ 3 . Each R″, independently, is a linear or branched, substituted or unsubstituted alkyl or aryl group and X is a halogen atom, H, or OR′. R′ is as defined above. A suitable example of SiXR″ 3 is 1H,1H,2H,2H-perfluorooctyl dimethyl methoxysilane (PFODMMS), CF 3 (CF 2 ) 5 CH 2 CH 2 Si(CH 3 ) 2 OCH 3 . The silane can be added as a gas, a liquid, or in solution.
Contact of the surface of the above siloxane coated MEMS device at elevated temperatures with one or more compounds of the formula SiXR″ 3 provides extensive cross-linking (Si—O—Si) and bonding to the surface (—Si—O-Surface) within islands of the siloxane oligomers. SiXR″3 reacts with surface vacancy sites to form surface anchored R″ 3 Si—O-surface species. SiXR″3 also reacts with un-reacted Si—OH groups within islands of oligomeric siloxane.
The result of the two steps described above for SAMs (treated with both SiX 2 R 2 and SiXR″ 3 ) is a composite monolayer, illustrated in FIG. 1 , consisting of two types of regions: (A) cross-linked regions with a small number of anchoring bonds to the surface, and (B) strongly anchored regions where each molecule is individually bonded to the surface. The composite nature of the monolayer provides much enhanced mechanical stability, as compared to coatings of pure (A) or (B).
Alternatively, the result of the two steps described above for a thin film (treated with both SiX 2 R 2 and SiXR″ 3 ) is a thin film composite coating consisting of regions of oligomeric siloxane from SiX 3 R and regions of R″ 3 Si—O— bonded to the surface or oligomeric siloxane.
In still another embodiment, the present invention provides methods of applying a coating to the surface of a MEMS device that includes a first step of contacting the surface of the MEMS device with a combination of silanes having the formulae SiX 3 R and SiX 2 R 2 , wherein SiX 3 R and SiX 2 R 2 are as defined above. The silanes can be applied to the surface in a gaseous state, as a liquid, or in solution.
In a second step, the coated surface is then heated at an elevated temperature. This method provides improved anti-stiction properties to the coated surface. In one aspect, a thin film can be formed on the surface of the MEMS device. In another aspect, a self-assembled monolayer (SAM) can be formed on the surface of the MEMS device as described below.
The temperature of the reaction in the first step is one that can be appropriate for the formation of a self-assembled monolayer on the surface of the MEMS device(s) as described above. The temperature of this reaction is generally from about 0° C. to about 40° C., and more particularly from about 10° C. to about 25° C. The partial pressure of the silane at the reaction temperature is at least about 1×10 −6 atmospheres (atm), and more particularly at least about 1×10 −3 atm.
Alternatively, the temperature of the reaction in the first step is one that can be appropriate for the formation of a thin film on the surface of the MEMS device(s) as described above. The temperature of this reaction is generally from about 0° C. to about 300° C. The partial pressure of the silanes at the reaction temperature is at least about 1×10 −6 atmospheres (atm), and more particularly at least about 1×10 −3 atm.
The temperature of second step is generally from about 50° C. to about 350° C., more particularly from about 80° C. to about 250° C., and even more specifically from about 100° C. to about 200° C., e.g. about 150° C. The pressure of the silanes at the reaction temperature is generally at least about 1×10 −6 atmospheres (atm), more particularly at least about 1×10 −3 atm, even more specifically about 1 atm.
The afore-mentioned methods with SiX 3 R and SiX 2 R 2 can further include in the second step, the heating step, an environment that contains at least one compound having the formula SiXR″ 3 , wherein SiXR″ 3 is as described above. A suitable example of SiXR″ 3 is 1H,1H,2H,2H-perfluorooctyl dimethyl methoxysilane (PFODMMS), CF 3 (CF 2 ) 5 CH 2 CH 2 Si(CH 3 ) 2 OCH 3 . The silane can be added as a gas, a liquid, or in solution.
Contact of the surface of the above siloxane coated MEMS device at elevated temperatures with one or more compounds of the formula SiXR″ 3 provides extensive cross-linking (Si—O—Si) and bonding to the surface (—Si—O-Surface) within islands of the siloxane oligomers. SiXR″3 reacts with surface vacancy sites to form surface anchored R″ 3 Si—O-surface species. SiXR″3 also reacts with un-reacted Si—OH groups within islands of oligomeric siloxane.
The result of the two steps described above for SAMs (treated with both SiX 3 R and SiX 2 R 2 and SiXR″ 3 ) is a composite monolayer, illustrated in FIG. 1 , consisting of two types of regions: (A) cross-linked regions with a small number of anchoring bonds to the surface, and (B) strongly anchored regions where each molecule is individually bonded to the surface. The composite nature of the monolayer provides much enhanced mechanical stability, as compared to coatings of pure (A) or (B).
Alternatively, the result of the two steps described above for a thin film (treated with both SiXR 3 and SiX 2 R 2 and SiXR″ 3 ) is a thin film composite coating consisting of regions of oligomeric siloxane from SiX 3 R and regions of R″ 3 Si—O— bonded to the surface or oligomeric siloxane.
When a silane solution is utilized in any of the above-identified methods, the concentration of the silane in the solution is generally at least about 1×10 −6 mole/l (M), more particularly from about 1×10 −4 M to about 1×10 −2 M. Alternatively, the silane can be applied in the absence of a solvent.
Suitable solvents to prepare the solution include, for example, iso-octane, hexadecane, THF, DMSO, and alcohols.
Heating of the treated surfaces in the second step for any of the above methods, can be conducted under, vacuum, under an inert gas environment (argon or nitrogen, for example) or in air.
In certain embodiments, R′ can be a linear alkyl group, such as methyl or ethyl.
In certain embodiments R can be a perfluorinated alkyl group, having a carbon chain length of about 6 to about 12 carbon atoms. In certain embodiments, one “terminal” portion of the perfluorinated alkyl group remains unfluorinated, such that two unfluorinated methylenes exist (e.g., 1H,1H,2H,2H-perfluoroalkyl). The unfluorinated methylene chain is generally attached to the Si of the reactive moiety. For example, 1H,1H,2H,2H-perfluorooctane is a suitable R group.
In certain embodiments of the invention, R″ can be a perfluorinated alkyl group, having a carbon chain length of about 6 to about 12 carbon atoms. In certain embodiments, one “terminal” portion of the perfluorinated alkyl group remains unfluorinated, such that two unfluorinated methylenes exist (e.g., 1H,1H,2H, 2H-perfluoroalkyl). The unfluorinated methylene chain is generally attached to the Si of the reactive moiety. For example, 1H,1H,2H,2H-perfluorooctyl dimethyl methoxysilane (PFODMMS), CF 3 (CF 2 ) 5 CH 2 CH 2 Si(CH 3 ) 2 OCH 3 is a suitable example where R″ is 1H,1H,2H,2H-perfluorooctyl.
In a particular embodiment, a microelectromechanical system is formed that includes the surface of the present invention. There are many types of MEMS devices. They can include, for example, optical routing devices, digital mirror devices, microvalves, pressure sensors, and the like. Examples of MEMS devices are disclosed in U.S. Pat. No. 5,694,740 (Martin et al.) and U.S. Pat. No. 5,602,671 (Hornbeck) and can generically found in Proceeding of the 7 th International Conference on the Commercialization of Micro and Nano Systems; Hsu, Tai-Ran—MEMS and Microsystems: design and manufacture (McGraw-Hill, 2002.); and W. Menz, J. Mohr, O. Paul, Microsystem technology (Wiley-VCH, New York, 2001).
EXPERIMENTALS
Si(111) samples were slices of polished Si(111) wafers (Wafernet). They were cleaned in oxygen plasma (250 mtorr O 2 , 200 watts, 2 min.). Immediately after plasma cleaning, each sample was placed in a clean plastic box (Fluoroware). One drop (3.5 microlieter liquid) of 1H,1H,2H,2H-perfluorooctyl triethoxysilane (PFOTES) was added into the box (not touching the sample). Each box was sealed at room temperature (20° C.) and ambient pressure (760 torr) and the Si samples were coated by PFOTES vapor. After three hours, the box was opened and the samples were removed from the plastic box for further processing or testing. This vapor exposure leads to the formation of a self-assembled monolayer of PFOTES on Si(111) and each was referred to as A/Si(111).
To form the composite coating, the A/Si(111) samples were placed in a stainless steel reactor (a 2 inch diameter tube with NW40 flanges on both ends) with approximate volume of 300 ml. A drop (10 microliter, liquid) of 1H,1H,2H,2H-perfluorooctyl dimethyl ethoxysilane (PFODMES) was added to the reactor (not touching the sample) at room temperature and ambient pressure. The reactor was subsequently sealed and placed in an oven set at 125° C. After ˜12 hours, the reactor was removed from the oven and opened immediately. The samples were removed from the reactor for further testing. This process lead to the composite monolayer on Si(111) and each sample was referred to as AB/Si(111).
Table 1 lists the values of water contact angle on the three surfaces: AB/Si(111), A/Si(111), B/Si(111). The AB/Si(111) surface shows the highest value of static water contact angle (qs) and the lowest value of hysteresis between advancing and receding water contact angles (qa-qr). Both results indicated that, among the three surfaces, the one with composite coating gave the most complete coverage of surface attached 1H,1H,2H,2H-perfluorooctyl groups with —CF 3 termination.
TABLE 1
Water contact angles in degrees. Error: ±2°
θ s : static; θ a : advancing; θ r : receding
θ a :
θ r :
Sample
θ s : Static
Advancing
Receding
AB/Si(111)
120 0
125 0
110 0
A/Si(111)
115 0
125 0
95 0
B/Si(111)
100 0
110 0
90 0
Quantitative comparisons between these surfaces are shown by interfacial force microscopy measurements. This technique allows the direct measurement of adhesion and friction forces between a probe tip and a solid surface on the microscopic scale. In each measurement, both the normal force (FN) and the friction force (FR) are zero when the tip is at long distance from the surface. As the tip moves closer to the surface, FN becomes negative, indicating attractive interaction between the tip and the surface. The absolute value of FN when it is minimum corresponds to the adhesion force, FA. As the tip moves further towards the surface, the normal force rises rapidly, indicting repulsion between the tip and the solid substrate. The simultaneously measured friction force rises when the tip and the surface interacts, particularly in the repulsive region.
FIG. 2 compares the composite AB/Si(111) surface with the A/Si(111) surface. These experiments were done with the same tip, thus allowing a direct, quantitative comparison. Compared to the AB/Si(111) surface, the A/Si(111) shows 25% more surface adhesion force, in agreement with water contact angle measurements in Table 1. Thus, the AB/Si(111) is more completely covered by 1H,1H,2H,2H-perfluorooctyl groups with —CF 3 termination to give a lower surface adhesion force. The A/Si(111) surface also shows similar increase in friction force. It is known from previous IFM studies (see, e.g., Major, R. C.; Kim, H. I.; Houston, J. E.; Zhu, X.-Y. Tribol. Lett. 2003, 14, 237–244. Houston, J. E.; Kim, H. I. Acct. Chem. Res, 2002, 35, 547–553.) that the friction force is sensitive to the presence of disorder, such as vacancies and domain boundaries, in a monolayer film. Thus, it appears that less defects are within the composite AB/Si(111) monolayer than those in the single component A/Si(111) monolayer. Defects within the film are believed to be the origins of film degradation.
FIG. 3 compares the composite AB/Si(111) surface with the B/Si(111) surface. These experiments were done with the same tip, but different from the tip used in FIG. 2 . Compared to the AB/Si(111) surface, the B/Si(111) shows 80% more surface adhesion force. Thus, the surface coverage of —CF 3 terminal groups decreases in the order of AB/Si(111)>A/Si(111)>B/Si(111). The B/Si(111) surface also shows much higher friction force than that on AB/Si(111).
Although the present invention has been described with reference to preferred embodiments, persons skilled in the art will recognize that changes may be made in form and detail without departing from the spirit and scope of the invention. The teachings of any reference cited throughout this specification are incorporated herein in their entirety. | The present invention provides unique methods of coating and novel coatings for MEMS devices. In general a two step process includes the coating of a first silane onto a substrate surface followed by a second treatment with or without a second silane and elevated temperatures. | 1 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method 1 for controlling a fluid compression system. The invention also concerns a control system suited for controlling a fluid compression system.
2. Description of the Prior Art
In conventional compression systems of a fluid medium, particularly compressed-air systems, the outlet pressure of the compressor is sensed, and this information is used to control the compressor operation with the help of a pressostat placed immediately at the compressor outlet. In compressor models equipped with a no-load unloading facility, the duration of the unloaded no-load running mode can be controlled by an adjustable timer. The set time is always constant until changed manually. Such control schemes are not capable of taking into account pressure losses caused by air consuming equipment attached to the system and variations in compressed air demand. Pressure loss occurring in the equipment is entirely dependent on instantaneous air flow rate and pressure. These variables may change by a large amount within a short interval of time. Moreover, the pressure loss caused by filters on the compressed-air line is dependent on the degree of clogging of the filters. When new, the filter causes a small pressure loss which increases with the clogging of the filter when it binds impurities from the through-flowing air. When sufficiently clogged, the filter element is replaced, whereby the pressure loss is again reduced to a low level.
To the user of the compressed-air system, it is extremely important that proper pressure level for the compressed-air operated equipment is ensured at the point of demand.
A disadvantage of prior-art equipment is that they require the compressor working pressure to be set to an unnecessarily high level due to the incapability of such equipment to compensate for the pressure losses caused by the above-mentioned accessories or devices. Resultingly, the energy consumption of the compressed-air system is unnecessarily high. Moreover, for compressors operated with period of unloaded postrunning mode, the duration of the postrunning mode is set according to the rule that the frequency of compressor starts may not exceed the maximum frequency of starts specified for the drive motor. This duration of the postrunning mode is fixed and unrelated to variations in compressed-air demand, thus permitting the compressor to run unloaded for the preset duration of the postrunning mode even during times of no compressed air demand. In this case, unnecessary energy losses occur.
Also in conjunction with compressed-air systems having two or more compressors, control systems based on conventional techniques cause superfluous energy consumption. Very commonly a pressure swing of small amplitude or short duration starts the second or the other compressors even when no extra air would actually be required. Further, if the compressor is operated using an unloaded no-load running mode, the proportion of useless energy consumption may rise up to about 40% of the nominal electrical input rating of the compressor yet producing no air to the compressed-air network.
Energy consumption in conventional compressed-air systems is on the average more than 30% greater than the theoretical minimum due to the following reasons:
To fulfill the pressure requirements of the user equipment under varying conditions of air demand, the compressor working pressure must be set significantly higher than the average pressure demand;
The compressor operating control system by no means takes into account the effect of the amount of air demand and the degree of filter contamination on pressure losses occurring in the compressed-air circuit;
The duration of the postrunning mode of the compressor intended to protect the drive motor is constant, thus failing to adjust the actually needed duration of the postrunning mode according to the variations in air demand; and
Multiple compressor systems are unnecessarily sensitive, and entirely useless compressor starts are triggered which are caused by the delay from the compressor start to the instant of effective compressed air production.
SUMMARY OF THE INVENTION
It is an object of the present invention to achieve an entirely novel control method and control system for a fluid compression system, whereby the drawbacks of the prior art are overcome.
The embodiment disclosed herein provides several significant benefits. Savings in excess of 30% over conventional techniques will be achieved in the energy consumption of compressed-air production. The control scheme according to the invention provides continuous and automatic control of compressor operation in a manner that minimizes energy consumption. In multiple compressor systems the control scheme according to the invention stops and starts the compressors automatically and in an anticipatory manner so as to keep the pressure level at the point of air demand within predetermined limits and to prevent exceeding the maximum starting frequency permitted for the drive motors of the compressors. The user line pressure can be maintained within predetermined limits also under varying rates of air demand, while unnecessary running of the compressors is avoided. The control scheme according to the invention is easily adjustable to comply with local operating conditions. The system reacts immediately to changes in compressed air demand. The control system according to the invention is also capable of compensating for slow changes in pressure losses due to clogging of filters, for example.
The invention is well suited for use in different environments. It can be adapted to single as well as multiple compressor systems. In can be used in conjunction with the most common air compressor types and other fluid compression means. Further, it may be installed in both new and old compressed-air systems. The control system according to the invention comprises a modest number of components and its installation is straightforward. Connections to the compressed-air system are limited to two pressure sensors and an electrical connection to the existing control system of the compressor(s).
Further scope of applicability of the present invention will become apparent from the detailed description given hereinafter. However, it should be understood that the detailed description and specific examples, while indicating preferred embodiments of the invention, are given by way of illustration only, since various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will become more fully understood from the detailed description given hereinbelow and the accompanying drawings which are given by way of illustration only, and thus are not limitative of the present invention, and wherein:
FIG. 1 is a schematic representation of the system configuration according to the invention;
FIG. 2 is a graph illustrating the working pressure of the compressor measured at air receiver 3 of FIG. 1; and
FIG. 3 is a graph illustrating the user site pressure measured at air receiver 8 of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference to FIG. 1, a compressed-air system equipped with the control system according to the invention is shown. Connected to a compressor 1 in the system is a cooler 2 and an air receiver 3, or alternatively, an expanded section of the pressure line or equivalent air storage. These elements are followed by a post-conditioning outfit 4, 5, 6, 7. Depending on the system configuration, the post-conditioning outfit includes different kinds of accessories. With reference to FIG. 1, the post-conditioning accessories include filters 4, 5 equipped with water separators, a dryer 6 and a filter 7. The post-conditioning outfit in the piping is followed by a second air receiver 8 from which air is taken to a point of demand 9.
The control system of the compressor 1 comprises a control unit 12 and two pressure sensors 15, 16, of which the first pressure sensor 15 is placed on the first air receiver 3 preceding the post-conditioning outfit 4, 5, 6, 7 and the second pressure sensor 16 is placed on the second air receiver 8 following the post-conditioning outfit. Additionally, the control system includes cabling 10, 11 connecting the control unit 12 to the pressure sensors 15, 16 as well as cabling 13 connecting the control unit 12 to the local operating control system 14 of the compressor 1. Obviously, such cabling may be replaced by any suitable signal transmission means.
The control unit 12 advantageously comprises a programmable logic controller or similar centralized control means with required accessories and connectors, as well as compressor selector switches implemented in a conventional manner for the manual operation and operating status monitoring of the compressors, indicator lamps, pushbuttons, connections for remote supervision and external display panels, etc. The programming of the logic controller in the control unit 12 is most appropriately performed using a separate programming device suited for storing in the programmable logic controller the basic data of the compressed air system such as the total volume of air receivers in the circuit, desired pressure level P 3 after the post-conditioning outfit, maximum permissible starting frequency for the drive motor, permissible pressure limits and other information necessary for the function of the control system.
In the method according to the invention, the pressure of compressed air delivered to the point of demand 9 is allowed to vary between a permissible minimum pressure P 3min and a permissible maximum pressure P 3max (whereby the maximum pressure P 3max =minimum permissible pressure P 3min maximum permissible pressure deviation). The pressure P 3 delivered to the point of demand is monitored by means of the pressure sensor 16. The pressure loss between the first air receiver 3 and the second air receiver 8 due to the outfit 4, 5, 6, 7 connected between them is dependent on the air flow rate, degree of filter clogging and the pressure prevailing in these elements. In practice, the pressure measured by means of the pressure sensor 15 is equal to the working pressure P 2 of the compressor. This pressure may be any level between the minimum pressure P 2min and a maximum pressure P 2max permitted for the operation of the compressor.
When the pressure P 3 measured by means of the pressure sensor 16 reaches either the preset minimum pressure P 3min or the preset maximum pressure P 3max , the control unit 12 controls the working pressure P 2 of the compressor according to rules expressed below in preset pressure steps either higher or lower depending on which pressure limit is reached and how the post-conditioning accessories between the receivers 3 and 8 affect the pressure level.
The rate-of-change (rate-of-rise or rate-of-fall) of compressed air pressure delivered to the point of demand 9 is monitored continuously. The signal for the rate-of-change monitoring is most conveniently obtained from the pressure sensor 15, whereby also the effect of the post-conditioning outfit placed on the pipe between the receivers 3 and 8 is taken into account.
When the compressor 1 is running in the unloaded mode and the pressure rate-of-fall is slow, or alternatively, when the pressure is rising and the permissible starting frequency of the compressor drive motor is not exceeded, compressor 1 is stopped immediately.
Fast rate-of-fall of the pressure P 3 causes removal of unloading or start of a compressor before the preset lower pressure limit P 3min is attained.
Compressor unloading/stop/start steps are predictively controlled on the basis of pressure rate-of-rise or rate-of-fall.
In systems of two or more compressors, only a single permissible pressure range from P 3min to P 3max need to be preset from the point of demand 9, after which the start/unloading/unloaded postrunning/stop modes of the compressors are controlled on the basis of the pressure rate-of-rise or rate-of-fall detected with the help of the pressure sensor 15.
The control scheme according to the invention avoids exceeding the maximum permissible start frequency specified for the drive motors of the compressors. At the onset of a possible equipment malfunction, the local control system 14 of any compressor 1 can overtake the control. The working pressure P 2 of the compressor is always kept at the lowest possible level which can maintain the pressure P 3 at the point of demand within the preset limits. In compressed air systems of multiple compressors, only the minimum number of compressors is run loaded. The method according to the invention optimizes energy consumption in a system of on arbitrary number of compressors. The system energy consumption will be the lowest possible under varying conditions of compressed air demand.
In the following the details of the invention are elucidated with reference to FIGS. 2 and 3. Pressure P 3 at the point of demand 9 and its permissible limits P 3max and P 3min are shown in FIG. 3. The working pressure P 2 of the compressor 1 is dependent on the instantaneous air demand situation due to the fact that the accessories 4-7 cause a pressure loss which further is dependent on the dimensioning of the accessories, instantaneous air flow rate, degree of contamination, pressure and temperature prevailing in the accessories and possible internal air consumption (particularly in adsorption dryers). Consequently, the compressor working pressure P 2 varies continuously. The level of the compressor working pressure P 2 may be affected by increasing or decreasing the compressed air delivery rate. Such changes of delivery capacity can be effected by unloading the compressor(s), stopping the compressor(s) or removing compressor unloading and starting a compressor. The working pressure P 2 of the compressor is not constant herein, but rather, always as low as possible, whereby the lowest possible energy consumption is achieved. The control unit 12 does not primarily monitor the absolute value of the pressure P 2 , but only the changes of the pressure level.
With reference to FIGS. 2 and 3, a graph is shown illustrating the different operating situations and the function of the invention under different pressure change situations.
When air consumption at the point of demand 9 begins to increase, a pressure fall P 32 OCCURS in the line pressure. The pressure sensor 16 signals the pressure fall to the control unit 12 and the control unit aims to control an increase in the working pressure P 2 . Simultaneously, the resulting increase in the flow rate through the accessories 4-7 causes a higher pressure drop which requires a further increase in the working pressure P 2 . If no increase is detected in the working pressure P 2 , the control unit 12 finds the air delivery capacity insufficient and removes unloading of the compressor 1 or starts the next compressor to increase the delivery capacity.
An increase in air delivery capacity results in an increase in the working pressure P 2 (indicated by pressure phase P 21 in FIG. 2). With the increase in the flow rate, also the pressure drop through the accessories 4-7 increases. In maintaining a balance between the delivery and demand of compressed air, the line pressure P 3 (indicated by pressure phase P 31 in FIG. 3) varies between the limits P 3min and P 3max . Then, the compressors are run under steady-state conditions.
At a very rapid fall of the line pressure P 3 (indicated by pressure phase P 32 in FIG. 3), the control unit 12 computes from the rate-of-change of the working pressure P 2 (indicated by pressure phase P 22 in FIG. 2) the instant when line pressure will fall below the minimum permissible pressure P 3min , and to anticipate this, removes unloading of the compressor 1 or starts the next compressor in advance so that the starting delays of the compressors or removal delays of unloading will not result in line pressure drop below the lower limit P 3min . The control unit contains data of starting and unloading removal delays of the compressors, and the stored compressor delivery capacity data can be complemented with information on receiver capacity.
When air consumption at the point of demand 9 begins to decrease and the compressor(s) is/are still running, the line pressure P 3 (indicated by pressure rise P 33 in FIG. 3) begins to rise. The pressure sensor 16 signals the rise of the pressure P 3 to the control unit, and as the line pressure tends to approach the preset permissible upper limit P 3max , the control unit 12 aims to control a decrease in the working pressure P 2 (resulting in a pressure fall P 23 in FIG. 2). To accomplish this, the control unit controls the compressor to run unloaded or stops the compressor(s) in a preset sequence until such an equilibrium state is attained that keeps the line pressure P 3 within the preset limits (indicated by pressure P 31 in FIG. 3).
If the air consumption at the point of demand 9 is very small and the line pressure P 3 has already reached the upper limit P 3max and the compressor(s) has/have controlled to run unloaded, the control program computes on the basis of the stored basic data the instant at which the line pressure P 3 (P 34 in FIG. 3) or the compressor working pressure P 2 (P 24 in FIG. 2) will fall to the permissible minimum pressure P 3min . If this pressure fall time is found to become longer than the minimum stop time permitted by the highest permissible starting frequency of the compressor drive motor, the control unit 12 stops the compressor immediately and thus saves energy by avoiding unnecessary no-load running of the compressor.
If the compressor working pressure P 2 monitored with the help of the pressure sensor 15 rises up to its upper permissible limit P 2max , no more compressor(s) will be started by the control unit 12 notwithstanding the possibility that the user line pressure P 3 would be at its lower permissible limit, but instead the control unit issues an alarm of working pressure upper limit violation and/or simultaneously stops/unloads the compressor(s) presently running. This function is a safety measure protecting the compressor(s) from overload.
In the case where the compressor working pressure P 2 monitored with the help of the pressure sensor 15 falls to its lower permissible limit P 2min , depending on the conditions the control unit 12 may issue an alarm of exceeded capacity of the compressor(s).
In the case where a malfunction of the control unit 12 occurs and the compressor working pressure P 2 exceeds its upper permissible limit P 2max , system control will be directly transferred to the local control unit 14 of the compressor 1 which is adjusted to keep the working pressure of the compressor marginally above P 2max . Also this function is a safety measure.
All the foregoing functions occur automatically in the above-described or any arbitrary sequence as required by the air consumption at the point of demand 9 and the compressor working pressure P 2 which directly control the functions. Because the air consumption at the point of demand 9 and the running status of the compressor 1 directly affect the user line pressure which is monitored immediately after the post-conditioning accessories 4-7 with the help of the pressure sensor 16, the above-described control method makes it possible to minimize energy consumption by keeping the user line pressure P 3 close to its permissible minimum value and by anticipating the required unloadings and starts/stops of the compressors and by allowing the compressor working pressure P 2 to freely float at the level required by the instantaneous demand of compressed air and prevailing operational conditions of the equipment.
The control unit 12 can be linked by conventional means to a remote supervisory system of the compressor station.
Further, the control system can be integrated as a part of the local control equipment of the compressor, or alternatively, it can be designed to replace conventionally employed control systems of compressors.
In compressor installations of two or more compressors, the control unit can be programmed to automatically select the compressor optimally suited to produce compressed air under the instantaneous operating situation.
To those versed in the art it is obvious that the invention is not limited by the exemplifying embodiments described above, but rather, can be varied within the scope of the invention defined in the appended claims. | A method of controlling a fluid compression system having at least one compressor for compressing a fluid medium includes defining the permissible minimum and maximum values of the user line pressure at the point of demand. The user line pressure is continuously monitored using a pressure sensor, and the working pressure of the compressor is monitored. The pressure difference between the working pressure of the compressor and the user line pressure at the point of demand is monitored. The pressure rate-of-change of the fluid medium delivered to the point of demand is monitored, and at least one of the compressors is controlled by a control unit on the basis of at least one of the monitored parameters defined in the foregoing steps of the method. A control system for controlling the operation of at least one compressor uses a plurality of sensors for sensing the status of the flowing medium. | 5 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a security fence of the type employing a fiber optic cable to detect intrusion or tampering. Further, the present invention relates to a method and apparatus for calibrating and initializing such a system, so that the system accurately approximates an intrusion or tampering location along the security fence.
2. Discussion of the Related Art
Security fences are widely used today. For example, security fences usually surround the perimeters of military facilities, some government agencies, airports, residences of celebrities and politicians, and other such areas. Simple fences are effective in alerting an innocent passerby that a certain area is restricted. Deterrent fences, such as fences with barbed wire, razor wire, or electrical currents therein, can also be effective at deterring less determined persons, such as children and vagabonds, from crossing into the restricted area. However, determined individuals, such as criminals and terrorists, may easily bypass deterrent fences by using common tools, such as wire or bolt cutters to simply make a passageway therethrough.
A first attempt to address the concern of determined individuals entering a restricted, fenced area was the employment of monitoring schemes. Security guards, cameras, and watch dogs, to name a few, were used to monitor the fence perimeter. However, such conventional monitoring systems are far from foolproof, as humans and animals can be distracted and often do not monitor closely due to boredom.
An improvement in the art came with the advent of employing fiber optic cable in conjunction with a security fence. FIG. 1 shows a section of a security fence 1 , in accordance with the background art. The security fence extends from a first end 3 to a second end 5 . Such a security fence is formed by interlocked galvanized metal wires attached to support posts 2 , and is commonly referred to as a “chain-link” fence. Of course, a protected area would be surrounded by a plurality of such fence sections, which abut, or are closely adjacent to, one another.
A fiber optic cable 7 is woven into an overall pattern and attached to each section of the security fence 1 at a plurality of locations along the section of the security fence 1 . FIG. 2 is close-up view of fiber optic cable 7 of the security fence 1 . FIG. 2 illustrates the overall weave pattern of the fiber optic cable 7 . Six columns and five rows of the weave pattern are illustrated, however in practice, there could be thousands of columns and dozens of rows in a weave pattern covering a complete security fence section 1 . The galvanized wires have been removed to simplify the illustration. The fiber optic cable 7 is attached to the security fence 1 by a plurality of clips 9 . As illustrated in FIG. 3 , the clips 9 connect one portion of the fiber optic cable 7 to another portion of the fiber optic cable 7 , and also attach the fiber optic cable 7 to galvanized wires 6 of the security fence 1 .
As illustrated in FIG. 2 , a light is piped into one end 12 of the fiber optic cable 7 via a source/receiver, known as a transceiver 10 or ODTR. The light passes through the fiber optic cable 7 until it reaches the other end 14 of the fiber optic cable 7 . At the other end, the light is reflected off of a termination and returns back to the transceiver 10 . In practice, the weave pattern of FIG. 2 would be continuous all over the security fence 1 , and the one end 12 of the fiber optic cable 7 would reside at the first end 3 of the security fence 1 . Likewise, the other end 14 of the fiber optic cable 7 would reside at the second end 5 of the security fence 1 .
The time delay between the transmission of the light and the return of the reflected light is indicative of the length of the fiber optic cable 7 . A typical length of the fiber optic cable 7 might be 5,000, 10,000 or even 20,000 meters (m). If the cable is disturbed (e.g. cut by a tool or bent sharply as by climbing), the transmission of light therethrough is interrupted. The interruption causes the transmitted light to be partially or completely stopped before reaching the other end 14 of the fiber optic cable 7 , and instead causes the transmitted light to be reflected back to the transceiver 10 from the point of the cut or sharp bend.
The transceiver 10 constantly monitors the time delay between transmitting light and receiving reflected light back. If the measured time delay remains within a threshold value of a standard time delay, indicative of the light reaching the other end 14 of the cable, the transceiver 10 knows that the fiber optic cable 7 remains unmolested (e.g. uncut and unbent). If the time delay varies outside of the threshold value, e.g. less than the standard time delay, the transceiver 10 assumes that an uncommon event has occurred, and an alarm is raised.
Because of the nature of the speed of light and electronic circuits, the alarm is raised at almost the same instant as the breaching of, or tampering with, the fence. However, it should be noted that the length of fence being monitored by the system is usually quite long. For example, one transceiver 10 can monitor a fence up to and perhaps exceeding one mile (1.6 kilometers) in length. In most circumstances, such a fence is too long to be monitored by a person or camera from a single vantage point.
Initially, it is important to gain at least a general idea of the potential breach (PB) point along the fence from the transceiver 10 . By knowing the general area of the PB, it is possible to have a quick response by personnel to the area of a PB. Further, it is possible to quickly activate and/or aim a camera to the general area of the PB.
Later, it is also very important to have a more specific idea of the PB point in order to facilitate inspection and servicing of the fiber optic cable 7 to ensure/restore its operability. If the fiber optic cable 7 has been cut, it is important to “know” a location of the cut with some precision, so as to facilitate its timely repair. If a general location of the cut in the fiber optic cable is only known to within plus or minus 30 meters, it can take several people a long time to trace or follow the weave pattern and try to discern the cut or damaged portion of the fiber optic cable 7 , so that the cable can be repaired.
To locate a PB, the background art employs an arithmetic approach, as will now be explained. A signal is introduced into the first end 12 of the fiber optic cable 7 and initially travels along the security fence 1 toward a termination at the second end 14 of the fiber optic cable 7 . The initial travel direction has been indicated by arrows in FIG. 2 . After reaching the termination, the light is reflected at the second end 14 , and travels back to the transceiver 10 . No arrows for the reflected light are included in FIG. 2 , in order to simplify the illustration.
The transceiver 10 monitors the time delay between the transmission of a light signal and the reception of the reflected light signal. The time delay can be converted into a length measurement by multiplying the time delay by the speed of the light transmitted through the fiber optic cable 7 (which is a known value), and dividing that product by two. Under normal circumstances (e.g. no cut or bending stress in the fiber optic cable 7 ), the distance calculated by the transceiver 10 will be the cable's total length (TL), otherwise the length will be a shorter value and will indicate a length of cable prior to the PB point in the fiber optic cable 7 . This length will be referred to as the cut length (CL).
To locate the ground distance (GD) from the first end 3 of the security fence 1 to the potential breach/bend (PB) in the fiber optic cable 7 , the transceiver 10 starts with the measured CL, and then subtracts a dummy cable length (DCL), which extends between the transceiver 10 and the start of the security fence 1 . Next, the outcome is divided by the cable length used per meter of ground length (CLM). The CLM is an average value, which is highly dependent upon such factors as the shape of the weave pattern selected (which is diamond shaped in FIG. 2 ), the closeness or density of the pattern, and the height of the security fence 1 . In some instances, CLM could equal 25 meters of cable per one meter of ground distance. The equation to estimate the ground distance (GD) from the start of the fence to the potential breach (PB) in the fiber optic cable 3 is: GD=(CL−DCL)/CLM.
Authorized personnel use the ground distance (GD) as a general guide to quickly respond to a potential breach (PB). For example, a security guard would be alerted to a potential break-in at 1,113 meters from the start point of the fence. The guard would then quickly proceed to a point in the neighborhood of 1,113 meters from the start of the fence in an attempt to intercept the breaching party. Later, the service personnel would attempt to exactly locate a point along the fence, which is approximately 1,113 meters from the start point of the fence, so that the fiber optic cable 3 could be inspected and repaired, as needed.
The background art, described above, suffers several drawbacks. First, it is difficult to locate points along a fence line based upon a known distance from a start point of the fence. If the distance is long, it is tedious to measure such a distance, and the measurement is prone to error. Further, obstacles along the fence line can further hinder a measurement from the start of the fence.
Second, the value CLM, which represents an average cable length used per meter of ground length, is a very troublesome value. In order for the ground distance (GD) to be accurately calculated, the CLM must remain relatively constant along the length of the fence. In other words, the actual CLM at any point along the fence should remain at, or very near to, the value of the average CLM for the entire fence, which is used in the equation to calculate the ground distance (GD).
In reality, it is very difficult to maintain a relatively constant CLM along the entire length of the fence line. For example, the height of the fence may vary to accommodate terrain changes. Further, it is difficult, and hence time consuming and expensive, to maintain a constant weave density for the weave pattern of the fiber optic cable 3 . Therefore, there exists a need in the art for an improved system and method of calculating a ground distance (GD) to a potential breach (PB) point in a fiber optic cable enhanced, security fence, such as the security fence 1 illustrated in FIG. 1 .
SUMMARY OF THE INVENTION
It is an object of the present invention to address one or more of the drawbacks associated with the background art.
The present invention offers an improved system and method for locating a potential breach in a fiber optic cable enhanced, security fence. The present invention discloses an improved system and method, which allows security personal to more quickly appreciate a general location of a potential breach (PB) in the security fence, and to more accurately locate the PB for later inspection, service and repair.
Further, the present invention offers a system and method to initialize and calibrate a system for detecting a location of a potential breach along a security fence.
These and other objects are accomplished by a system and method for establishing a look-up table to be used by a monitoring system for monitoring a security fence. The monitoring system evaluates the integrity of a fiber optic cable, having a weave pattern and attached to a security fence. Any breakage in, bending of, or stress on the fiber optic cable is noted by the monitoring system, and a length of cable between the monitoring system and the affected portion of the fiber optic cable is determined. The look-up table is indexed to determine a zone of potential breach. Further, an average weave density of the affected zone is computed, so that an approximate location of the potential breach within affected zone, in terms of ground distance, can be accurately determined and displayed.
Further scope of applicability of the present invention will become apparent from the detailed description given hereinafter. However, it should be understood that the detailed description and specific examples, while indicating preferred embodiments of the invention, are given by way of illustration only, since various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will become more fully understood from the detailed description given hereinbelow and the accompanying drawings which are given by way of illustration only, and thus, are not limits of the present invention, and wherein:
FIG. 1 is a perspective view of a chain-link security fence, in accordance with the background art;
FIG. 2 is a close-up view of a fiber optic cable having a diamond-shaped weave pattern for attachment to the security fence of FIG. 1 , in accordance with the background art;
FIG. 3 is a close-up view of a connector used to hold the fiber optic cable in the diamond-shaped weave pattern and connected to the security fence, in accordance with the background art;
FIG. 4 is a perspective view of a chain-link security fence, in accordance with the present invention;
FIG. 5 is a block diagram of a system for building a look-Lip table to establish a monitoring system, in accordance with the present invention;
FIG. 6 is a block diagram of an alternative system for building the look-up table to establish the monitoring system; and
FIG. 7 is a flow chart illustrating a manner of operating the monitoring system of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The present invention provides an improved system and method for more accurately detecting the location of a potential breach (PB) point in a fiber optic cable enhanced, security fence, such as the fence 1 illustrated in FIGS. 1–3 . Reference will be made to FIGS. 4–7 to describe the system and method of the present invention.
As illustrated in FIG. 4 , the security fence 1 , in accordance with the present invention, is divided into a plurality of zones Z 1 , Z 2 , Z 3 , Z 4 , . . . Zn. Each zone can be defined between posts 2 of the security fence 1 , or between installed signals, such as light signals 4 , or between natural objects, such as trees, streams, or rocks 6 . As illustrated in FIG. 4 , Zone Z 1 is 30 meters in length and extends between two posts 2 of the security fence 1 . Of course, there would most likely be several posts 2 residing within zone Z 1 , but for clarity's sake only the start and end posts 2 are illustrated. Zone 2 is 50 meters in length and extends between a fence post 2 and an installed light signal 4 . Zone Z 4 is also 50 meters in length and extends between a natural landmark, such as the rock 6 and a fence post 2 .
Next with reference to FIG. 5 , a system and method of initializing a system for monitoring the security fence 1 will be described. A first person 21 is provided with a first wireless communications device 23 , such as a cellular phone, or walkie-talkie radio. The first person 21 walks along the security fence 1 . At the zone boundaries, the first person pinches, bends or stresses the fiber optic cable 7 .
A second person 25 is located in a control center and is provided with a second wireless communications device 27 . The first person 21 informs the second person 25 when the fiber optic cable 7 is bent and the particular zone boundary at which the bend is made. For example, the first person may state that the bend is being made at 160 meters from the start of the security fence 1 , and that this location should be known as the start of zone 5 . As another example, the first person may state that the bend is being made at 377 meters from the start of the fence, and that this location should be know as the start of zone 13 , and is adjacent to a red and yellow marker staff.
The second person 25 views a display 29 connected to a controller 31 . The controller 31 is connected to the transceiver 10 . Because the fiber optic cable 7 is bent, the transceiver 10 will provide the second person 25 with the cable length to the bend, via an output of the display 29 . The second person 25 enters data via a keyboard 33 . The data may include the cable length determined by the transceiver 10 , the ground distance provided by the first person 21 and an identifier for the zone boundary.
By repeating the process for each zone boundary, the second person 25 may enter data into a table format, which is retained in a memory 35 connected to the controller 31 . The table establishes the zone boundaries as to: (1) their ground distance from the start of the fence; (2) the corresponding cable length from the transceiver to the start of the zone; and (3) any other relevant data, such as a marker identification or natural landmark which indicates the start of the zone. Table 1, set forth below, shows data entries for a security fence 1 covering an overall ground distance of 500 meters, and having ten zones. Of course, in practice the security fence could cover a much longer ground distance, have more zones, have zones of greater or shorter lengths, and have zones with varying lengths or uniform lengths.
TABLE 1
Look-Up Table for Zone Boundaries
Zone
Starts at
Starts at
Number
Ground Distance (GD)
Cable Length (CL)
1
0 meters (m)
325 m
2
50 m
840 m
3
100 m
1370 m
4
130 m
1805 m
5
180 m
2290 m
6
230 m
2800 m
7
270 m
3335 m
8
300 m
3825 m
9
400 m
4305 m
10
450 m
4750 m
The data table may be assembled in other manners, which would not require two persons. For example, as illustrated in FIG. 6 , the second wireless communications device 27 may be directly or indirectly connected to the controller 31 , and provide the first person 21 with direct access to the controller operations. In this instance, the second wireless communications device 27 would function in a manner similar to a wireless network router, and the first wireless communications device 23 would act as a linked device and would be capable of displaying data output to, and receiving data input from, the first person 21 . For example, the first wireless communications device 23 could be a laptop computer or personal digital assistant (PDA), networked to the second wireless communications device 27 . With the arrangement of FIG. 6 , the first person 21 could build and store the data table in the memory 35 using the first wireless communications device 23 . Also, the table could be completely built and initially stored in a memory within the first wireless communications device 23 , to be later downloaded into the memory 35 connected to the controller 31 . FIG. 6 also illustrates that a global positioning system (GPS) unit 40 may be included in the first wireless device 23 . The GPS unit 40 could provide an accurate display or input of the ground distance from the reference point or start of the security fence 1 , and hence relieve the first person 21 from making ground distance measurements using such devices as measuring roller wheels or range finders.
Once the data table has been built, the system is ready to operate. Next, an operating method for the security fence monitoring system will be described in connection with FIG. 7 . FIG. 7 is a flow chart illustrating a method of operation for the controller 31 of FIGS. 5 and/or 6 .
In step S 51 , the controller 31 is in a monitoring state. In the monitoring state, the controller 31 is constantly monitoring the output of the transceiver 10 . The normal output of the transceiver 10 is an indication of the condition where a light signal has traveled to the end 14 of the fiber optic cable 7 , reflected and returned to the transceiver 10 . Hence, the normal output of the transceiver 10 is a time delay value indicative of this condition.
Once the transceiver 10 outputs a shorter time delay signal to the controller 31 , an alarm is raised in step S 53 . The alarm may be given by a visual or audible alarm device 32 connected to the controller 31 . Alternatively, the alarm may be a signal provided to a remote monitoring station, wherein the remote monitoring station will process the alarm signal, such as alerting onsite security personnel, activating cameras, automatically calling the police and property owner/manager, etc.
Next, in step S 55 , the controller converts the time delay signal provided by the transceiver 10 into a cable length value, in other words the cable length (CL) existing between the transceiver 10 and the point of potential breach (PB) in the fiber optic cable 7 . The time delay can be converted into a cable length (CL) measurement by multiplying the time delay by the speed of the light transmitted through the fiber optic cable 7 (which is a known value), and dividing that product by two.
Next, in step S 57 , the CL value is compared to the lookup table stored in memory 35 to determine the zone of the PB point. For example, if the CL=2435 meters and table 1, above, is stored in the memory 35 , the point of PB resides in zone 5 . The identification of zone 5 can be made on display 29 and/or transmitted to the remote monitoring station.
Next, in step S 59 , an approximate location within zone 5 of the PB point is calculated. The approximate location of the PB point can be found using the following equations. First, the ground distance along the fence line within zone 5 is calculated by subtracting the ground distance to the start of zone 5 from the ground distance to the start of zone 6 . In this case, 230 m−180 m=50 m.
Next, the cable length consumed in the weave pattern residing in zone 5 is calculated by subtracting the cable length at the start of zone 5 from the cable length at the start of zone 6 . In this case, 2800 m−2290 m=510 m.
Next, the cable length within zone 5 from the start of zone 5 to the PB point is calculated by subtracting the cable length to the start of zone 5 from the CL to the PB point. In this case, 2435 m−2290 m=145 m.
Next, two ratios are equated and solved in order to calculate the ground distance of the PB point from the start of zone 5 . In other words, the ratio of total cable length within a particular zone divided by total ground distance of that zone, is equated to the ratio of cable from the start of the zone to the PB point divided by ground distance from the start of the zone to the PB point, the last variable is the unknown variable to be determined. In this case, 510 m/50 m=145 m/X, where X is the approximate ground distance of the PB point from the start of zone 5 . Here X=14.2 m, meaning that the PB point is located about 14.2 meters in ground distance from the start of zone 5 , or alternately stated about 194.2 meters from the first end 3 of the security fence 1 .
The method of determining the PB point along a security fence, in accordance with the above description offers many advantages over the background art. Primarily, the accuracy of the monitoring system is greatly enhanced, because there is no longer a reliance on an assumption that the fiber optic cable's weave pattern remains constant along the various portions of the security fence.
In practice, it is very difficult and time-consuming to ensure a consistent weave pattern density (cable length/ground distance covered) when installing a fiber optic cable along a security fence. Different persons may be installing the fiber optic cable at different portions of the security fence, the height of the security fence may change at various locations, natural or man-made objects may require alteration of the weave pattern (e.g. a 3 foot diameter drainage pipe passing through a security fence will prevent any fiber optic weave pattern within the cross sectional area it occupies). Hence, in the background art, the weave pattern density at any one point or portion of the fence section could vary greatly from the average value determined for that fence section.
Because of this variation, the background art's monitoring system could inaccurately predict the ground distance to the PB point. More importantly, when the fiber optic cable needed to be inspected or repaired, it took extended periods of time to locate the PB point.
The present invention has addressed the drawbacks of the background art's system. By the present invention, the location of a PB point will always certainly be known to within a certain zone. This is because the actual cable lengths to the zone boundaries are stored in a lookup table within a memory. The zone boundaries can be set very close together for enhanced accuracy. For example, when establishing the monitoring system for a 1000 meter section of fence, the first person 21 could “create” zone boundaries at 10 m intervals to establish approximately 100 zones, or at 20 meter intervals to establish approximately 50 zones, at the discretion of the user.
Moreover, by the present invention, the approximate location of a PB point within a zone is more accurately predicted, because there is a reliance upon an average weave pattern density for the zone having the PB point, rather than a reliance upon an average weave pattern density for the entire fence section. It is much more likely that the weave pattern density will be more uniform in any one particular zone, rather that the entire fence section.
The invention being thus described, it will be obvious that the same may be varied in many ways. For example, although the above description has referred to a transceiver 10 as a single device, it should be readily apparent that a distinct transmitter and a distinct receiver could be employed, in accordance with the present invention. As such, the term “light transmission and reception device,” as used in the claims, is meant to encompass the arrangement of an integrally formed transceiver and the arrangement of distinct components, which accomplish an equivalent function. Such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such modifications as would be obvious to one skilled in the art are to be included within the scope of the following claims. | A monitoring system evaluates the integrity of a fiber optic cable, having a weave pattern and being attached to a security fence. To establish and calibrate the monitoring system, the present invention provides a system and method for establishing a look-up table to be stored in a memory. Any breakage in, bending of, or stress on the fiber optic cable is noted by the monitoring system by an alarm, and a length of cable between the monitoring system and the affected portion of the fiber optic cable is determined. The look-up table is indexed to determine a zone of potential breach. Further, an average weave density of the affected zone is computed, so that an approximate location of the potential breach within the affected zone, in terms of ground distance, can be accurately determined and displayed. | 6 |
This is a continuation of co-pending application Ser. No. 07/270,454 filed on Nov. 7, 1988, which is a continuation of Ser. No. 06/800,330, filed on Nov. 21, 1985 (abandoned).
BACKGROUND OF THE INVENTION
The present invention relates generally to a solid-state still image recording apparatus for picking up and recording still images, which apparatus is also capable of recording audio signals. More specifically, the invention relates to control of the solid-state still image recording apparatus with audio recording feature, for controlling recording of still images and of audio signals at a given timing.
Recently, electronic or solid-state cameras for picking up still images have been developed and put into the market. Such electronic cameras employ magnetic media or the like as a replacement for photographic film in recording still images. Hereafter, the word "video recording" will be used to represent picking-up and recording still images on magnetic or equivalent recording media.
In order to make such solid-state still camera more attractive, it has been proposed to add audio recording features to the camera. In such cameras, it is possible to record audio sound related to the video recording, which is hereafter referred to as "audio recording", for a given period of time, e.g. 10 sec. Specifically, such cameras allow audio recording at a certain timing relative to the timing of video recording. The ability to record not only still images but also audio sound, such as voice, would make these cameras more attractive.
However, in cameras with both video and audio recording capability, it is difficult to properly set audio recording timing relative to video recording timing. This is inconvenient to the user since on different occasions, the user may want to perform video recording and audio recording at different times. Therefore, it would be beneficial to provide some flexibility in selecting the timing relationship between video recording and audio recording so that the user can use this type of camera more conveniently.
On the other hand, the camera can be equipped with a self-timing feature for performing video recording and audio recording in a manner similar to that of conventional film-type cameras. In this case, the timing relationship between video recording and audio recording becomes more critical. As is well known, such self-timers are generally used when the user of the camera wants to take his or her own picture. In such case, the user has to run to a predetermined position toward which the camera is directed after setting the self-timer. If the audio recording timing is set to start recording in response to onset of the self-timer, the user's voice will not be recorded until the user has run into the directional reception range of a microphone built into in the camera. On the other hand, if the audio recording timing is set for a certain delay after onset of the self-timer, the above problem is avoided, but the selection of an appropriate delay time is very difficult, since the timing would be different for each individual user.
SUMMARY OF THE INVENTION
Therefore, it is a principle object of the invention to provide an electronic still camera with an audio recording feature which can control video recording timing and audio recording timing in accordance with the user's desires.
Another, object of the invention is to provide a remote control system for the electronic still camera which can control video recording timing and audio recording timing in a mutually variable timing relationship.
A further object of the invention is to provide an electronic video recording and audio recording camera which can control video recording timing and audio recording timing independently.
In order to accomplish the aforementioned and other objects, an electronic still camera, according to the invention, comprises a video recording system and an audio recording system built into the camera, a data recording system including a recording medium for receiving video data from the video recording system and audio data from the audio recording system for recording and reproduction, and a remote control system associated with the video recording system and audio recording system for operating the video recording system and audio recording system. The remote control system can be used to adjust the video recording timing and audio recording timing relative to each other.
In the preferred construction, the remote control system includes manually operable means for operating the video recording system and the audio recording system at different timings. More preferably, the manually operable means comprises a remote controller including independent video recording and audio recording switches.
In accordance with one aspect of the invention, an electronic still camera with an audio recording feature comprises an image pick-up means for picking up video data, an audio recording means for receiving audio data, a magnetic disk drive mechanism including a magnetic disk for storing the video data and the audio data, and a remote controller for remotely controlling the image pick-up means to pick up video data and the audio recording means and to record audio data at a given timing.
The remote controller operates the image pick-up means and the audio recording means at mutually independent timings. The remote controller is operable in an AUTO mode in which the operation timings of the image pick-up means and the audio recording means are determined according to a preset timing, and in a MANUAL mode in which the operation timings of the image pick-up means and the audio recording means are controlled independently of each other.
According to another aspect of the invention, a combination of an image pick-up apparatus and an audio recording apparatus, comprises the image pick-up apparatus adapted to pick-up video data for a still image, the audio recording apparatus receiving audible sound and recording corresponding audio data, a medium adapted to store the video data and audio data, a recording and reproduction apparatus associated with the medium for recording video and audio data on the medium and reproducing the recorded video and audio data, a manually operable remote controller for producing a remote control signal including a first component representative of an image pick-up demand and a second component representative of an audio recording demand, first means associated with the image pick-up apparatus and responsive to the first component of the remote control signal for ordering the image pick-up apparatus to pick up video data, and second means associated with the audio recording apparatus and responsive to the second component of the remote control signal for ordering the audio recording apparatus to record audio data.
The remote controller comprises a first switch means for producing the remote control signal containing the first component when actuated, and a second switch means for producing the remote control signal containing the second component when actuated.
The first and second switch means are manually operable at mutually independent times. One of the first and second switch means is manually operable and the other of the first and second switch means is automatically operable at a preset time after manual operation of the one of the first and second switch means. The preset time is variable.
The remote controller comprises a timing setting means allowing manual adjustment of the preset time.
The image pick-up apparatus includes a first memory for temporarily storing the video data and transferring the data to the recording and reproduction apparatus for recording the video data on the medium at a first transfer timing, and the audio recording apparatus includes a second memory for temporarily storing the audio data and transferring the audio data to the recording and reproduction apparatus for recording the audio data on the medium at a second transfer timing. The image pick-up apparatus includes a shutter and the first memory comprises photo-sensitive elements, and the shutter becomes operative in response to the first component of the remote control signal for controlling exposure of the first memory, thereby causing the first memory to pick up and store video data.
On the other hand, the audio recording apparatus includes a microphone for receiving audible sound, means for converting the output of the microphone into a PCM signal and the second memory comprising a digital memory, and the second memory being responsive to the second component of the remote control signal for recording the PCM signal for a predetermined period of time.
The medium comprises a magnetic disk and the recording and reproduction apparatus comprises a disk drive accommodating the magnetic disk, the disk drive including an electric motor for driving the magnetic disk to rotate, which electric motor is driven in response to the first component of the remote control signal prior to operation of the shutter. The shutter is operated to expose the first memory after a given delay time after the first component of the remote control signal, which delay time is long enough to allow the electric motor to attain a proper operating speed after starting to rotate. The first and second means is responsive to termination of exposure of the first memory by the shutter to record the video and audio data on the magnetic disk. The second means is disabled while the second memory is receiving the PCM signal. The second memory is adapted to record the PCM signal in the form of a compressed-time-base PCM signal. The first memory comprises a charge transfer device.
The remote controller comprises a radio control unit. In the preferred embodiment, the radio control unit is adapted to transmit infrared rays as the remote control signal.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be understood more fully from the detailed description given herebelow and from the accompanying drawings of the preferred embodiment of the invention, which, however, should not be taken to limit the invention to the specific embodiments but are for explanation and understanding only.
In the drawings:
FIG. 1 is a block diagram of the preferred embodiment of a video and audio recording circuit according to the invention;
FIG. 2 is a perspective view of the preferred embodiment of a video and audio recording electronic still camera according to the invention; and
FIGS. 3(A-G), 4(A-G) and 5(A-F) are timing charts showing operation of the video and audio recording circuit of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings, particularly to FIGS. 1 and 2, the preferred embodiment of a still camera 10 has an image pick-up system 100 and an audio receiver system 200. The image pick-up system 100 includes a lens assembly 102 which focuses an image on an image receptacle comprising a charge transfer device, such as a charge-coupled device (CCD) 108, through a shutter mechanism 104. The shutter mechanism 104 controls exposure of the CCD 108 and therefore, is controlled by a shutter drive circuit 106 to be opened and closed. On the other hand, the audio receiving system 200 includes a microphone 202 and a memory 206. The memory 206 comprises a digital memory for receiving pulse-code-modulated (PCM) audio signals. In order to derive PCM signals from the output of the microphone 202, an analog-to-digital (A/D) converter 204 is interposed between the microphone and the memory.
The camera 10 also has a disk drive unit 300 with a magnetic disk 302 serving as a video and audio recording medium. The image received by the CCD 108 and the PCM audio signals written in the memory 206 are transferred to and stored on the magnetic disk 302 by means of a video head 304 and an audio head 306 respectively. A recording controller 400 controls transfer of the image data from CCD 108 and PCM signals from the memory 206. The recording controller 400 generally comprises a video processor 402 and an audio recording circuit 404. The video processor 402 is connected for input from CCD 108 via an amplifier 406 and is connected for output to the video head 304 via another amplifier 408.
It should be noted that a system for picking up an image and recording video data for the picked-up image on the magnetic disk, similar to the shown embodiment, has been disclosed in the British Patent First Publication No. 2,112,603A, published on July 20, 1983. The contents of this British Patent First Publication are hereby incorporated by reference for the sake of disclosure.
The video processor 402 and the audio recording circuit 404 cooperate in order to synchronize storage of video data and the PCM signals to the magnetic disk 302 in the disk drive.
The camera 10 also has a controller 500 for controlling operation of the image pick-up system 100, the audio receiving system 200, and the disk drive unit 300. The controller 500 includes a remote control sensor 502 which receives remote control signals from a remote controller 600.
In the shown embodiment, the remote controller 600 transmits infrared rays which serve as the remote control signal. The infrared rays emitted by the remote controller 600 may be modulated to represent a video recording demand and/or an audio recording demand. Toward this end, the remote controller 600 may emit different frequencies or different amplitudes of infrared light for controlling video recording and audio recording independently.
The controller 500 has a pair of detectors 504 and 506 connected for input from the remote control sensor 502 via an amplifier 508. The detector 504 responds to the output of the remote control sensor 502 indicative of the video recording demand by outputting a detector signal to a video recording controller 510. The video recording controller 510 controls the shutter drive circuit 106 which controls exposure timing and duration. Also, the video recording controller 510 controls the read-out timing of the video data from CCD 108 and the operation of a disk drive motor 308 in the disk drive unit 300. The video recording controller 510 further controls read-out timing of PCM signals from the memory 206 of the audio receiving system 200.
Hereafter, the control signal output from the video recording controller 510 for controlling the shutter drive circuit 106 will be referred to as "shutter control signal Sc 1 ", that for controlling read-out timing of video data from the CCD will be referred to as "video data read-out control signal Sc 2 ", that for controlling the disk drive motor will be referred to as "disk drive control signal Sc 3 ", and that for controlling read-out timing of the PCM signals from memory 206 will be referred to as "PCM signal read-out control signal Sc 4 ".
The detector 506 responds to a sensor output indicative of an audio recording demand by outputting a detector signal to a gate 512. The gate 512 is connected to a clock generator 514 in order to receive a clock signal S t . The gate 512 responds to the detector signal 506 by sending write-enable signal Sc 5 to the memory 206 in order to allow storage of audio data in the form of PCM signals for a predetermined period of time, e.g. 10 sec. The clock generator 514 also sends the clock signal to another gate 516. The gate 516 is connected to the video recording controller 510 to receive the PCM signal read-out control signal Sc 4 , whereupon it sends a read-enable signal Sc 6 to the memory 206. In response to this read-enable signal Sc 6 , the stored audio data is transmitted to the audio recording circuit 404.
Although it has not been illustrated in the drawings, the video recording controller 510 may be associated with a shutter release button 16 built into the camera 10 and serving as a shutter button. The video recording controller 510 may be responsive to depression of the shutter release button 16 to output the control signals Sc 1 to Sc 4 in substantially the same manner as when activated by the video recording controlling remote control signal from the remote controller. Furthermore, although not shown in the drawings, the camera may have an audio recording control button serving to trigger the gate 512 to enable storage of audio data for the predetermined period of time. Alternatively, the gate 512 can be triggered by depression of the shutter release button 12. In this case, the shutter control signal Sc 1 will be sent to the shutter drive circuit 106 after a given delay after issuance of the write-enable signal Sc 5 . This delay time may be adjusted by means of a manually operable video-audio recording timing adjuster which may also be built into the camera 10.
As shown in FIG. 2, the remote controller 600 is provided with an audio recording control button 602 and a video recording control button 604. The remote controller 600 is also provided with a mode selector switch 606 for switching operation mode between a MANUAL mode and an AUTO mode. In MANUAL mode, the audio recording control button 602 and the video recording control button 604 can be operated independently of each other. Therefore, in the MANUAL mode, the audio recording timing and the video recording timing can be set as desired. On the other hand, in the AUTO mode, the audio recording control button 602 is disabled and only the video recording control button 604 is manually operable. In this case, audio recording timing and video recording timing are automatically controlled by providing a delay between the remote audio recording demand signal and the remote video recording demand signal. Preferably, an adjuster (not shown) in the remote controller 600 adjusts the delay between the output timing of the video recording demand infrared rays and the audio recording infrared rays.
It would also be advantageous to allow operation of the video recording button 604 while the audio recording button 602 is simultaneously depressed or alternatively within a given period of time after depression of the audio recording button 602. This ensures a good match between the audio sound and image upon reproduction. On the other hand, although the audio recording button 602 in the preferred embodiment set out above is disabled in AUTO mode, it would be possible to disable the video recording button and enable the audio recording button.
It should also be appreciated that, although not shown in the accompanying drawings, the camera 10 may be provided with a finder, a focusing mechanism associated with the lens assembly and/or an exposure control associated with the shutter mechanism, which are all well known in the field of film-type cameras.
The operation of the aforementioned preferred embodiment of the still camera according to the present invention will be described in more detail with reference to FIGS. 3 to 5. It should be appreciated that FIGS. 3 to 5 show different timings of audio recording and video recording.
FIG. 3 shows audio recording and video recording in a case where the video recording control button is depressed after expiration of the audio recording period, which begins in response to depression of the audio recording control button 602. Specifically, at time t 1 , the audio recording button 602 is depressed until time t 2 , as shown in FIG. 3(A). Therefore, during the period between t 1 and t 2 , infrared light representing an audio recording demand is transmitted by the remote controller 600. This audio recording demand signal is received by the remote control sensor 502. The sensor output indicative of the audio recording demand is detected by the detector 506. The detector 506 then outputs the detector signal Sd a to the gate 512. The gate 512 responds to the trailing edge or alternatively, the leading edge of the detector signal Sd a by sending the write-enable signal Sc 5 to the memory 206. At the same time, the gate 512 starts measuring elapsed time by counting the clock pulses from the clock generator 514. At time t 3 at which the predetermined audio recording period, e.g. 10 sec., expires, the gate 512 terminates the write-enabling signal Sc 5 .
It should be appreciated that the write-enabling signal Sc 5 is sent to the memory in the form of clock pulse serving as a write clock pulse.
During the period t 2 to t 3 , the memory 206 allows storage of the audio data. The audio data is received by the microphone 202 as an analog audio signal S s . The audio signal S s is converted into PCM signals by the A/D converter 204 and input to the memory 206. Therefore, in the presence of the write-enabling signal Sc 5 in form of the write clock pulse, the PCM signals indicative of the audio data are stored in the memory 206 in a compressed time-base form.
It would be possible to provide a certain response delay of the gate 512 to the detector signal Sd a as shown by the broken line in FIG. 3(B). For this purpose, the gate 512 may be provided with a delay circuit responsive to each occurrence of the detector signal Sd a . It would be preferable to allow adjustment of this delay by providing a delay time adjuster associated with the gate 512.
After completing storage of the audio data, the video recording control button 604 is depressed at a time t 4 . The remote controller 600 transmits infrared rays representative of the video recording demand, as shown in FIG. 3(C). The detector 504 detects the video recording demands and outputs the detector signal Sd v . The detector signal Sd v is sent to the video-recording controller 510. The video-recording controller 510 is responsive to the trailing edge of the detector signal Sd v to output the disk drive control signal Sc 3 , at a time t 5 . Then, the disk drive motor 308, which comprises a spindle motor, starts turning. After a predetermined period long enough to allow the motor of the disk drive motor 308 to come up to speed, the shutter control signal Sc 1 is output to the shutter drive circuit 106, at a time t 6 . The shutter control signal Sc 1 remains HIGH for a period of time corresponding to the exposure duration of the shutter 104.
The exposure duration of the shutter may be derived manually or automatically according to the well known parameters. Therefore, the video-recording controller may derive the pulse width of the shutter control signal Sc 1 according to the optimum exposure period.
While the shutter control signal Sc 1 is HIGH, the shutter drive circuit 106 is active to hold the shutter 104 open and expose CCD to the image passing through the lens assembly 102. During this exposure period, CCD picks up one field or frame of image data. In response to the trailing edge of the shutter control signal Sc 1 , the video data read control signal Sc 2 is transmitted to CCD 108 from the video-recording controller 510, at a time t 7 . In response to the video data read control signal Sc 2 , the temporarily stored image data in CCD 108 is read out and sent to the video processor 402 via the amplifier 406.
At the same time, i.e, at the time t 7 , the audio data read control signal Sc 4 is output by the video-recording controller 510 to the gate 516. In response to the audio data control signal Sc 4 , the gate sends the read-enable signal Sc 6 in the form of a read pulse to the memory 206. Therefore, the compressed audio data in the memory is read out and transmitted to the audio recording circuit 404.
The video processor 402 performs FM modulation of the video data signal and then sends the result to the video head 304 through the recording amplifier 408. Likewise, the audio recording circuit 404 performs FM modulation of the audio data signal and then transmits it to the audio head 306. The video data and audio data are written onto the magnetic disk synchronously through the video head 304 and the audio head 306.
If desired, storage of audio and video data on the magnetic disk 302 may be non-synchronous, as shown by the broken line in FIG. 3(G). In this case, the gate 516 may delay transmission of the read-enable signal Sc 6 for a given delay time after receiving the audio data recording control signal Sc 4 . This non-synchronous method of recording on magnetic disk enables video recording and audio recording by a common magnetic head. In order to enable video recording and audio recording with a common head, it is preferable to allow a certain interval, e.g. 1/60 sec., between video recording and audio recording.
FIGS. 4(A) to 4(G) are similar to FIGS. 3(A) to 3(G). However, in this case, the audio recording button 602 is depressed at a time labelled t 10 and the video recording button 604 is depressed during the audio recording period, e.g. within 10 sec. of depression of the audio recording button.
In this case, the audio recording demand signal is produced at the time t 10 and terminates at a time t 11 . In response to the trailing edge of the detector signal Sd a from the detector 506, the write-enabling signal Sc 5 is transmitted from the gate 512 to the memory 206 to enable the latter to record the audio data received through the microphone 202 and converted into PCM signals by the A/D converter 204. After a while, the video recording demand signal is generated by the remote controller 600 in response to depression of the video recording button 604, at a time t 12 . In response to this, the detector signal Sd v is output from the detector 504. In response to the trailing edge of the detector signal Sd v , the disk drive control signal Sc 3 is sent at time t 13 to the disk drive spindle motor 308 to bring it up to speed. Once the disk drive is ready, i.e., at time t 14 , the shutter control signal Sc 1 is transmitted to the shutter drive circuit 106 to operate the shutter mechanism 104.
In the shown example, the timing of depression of the video recording button 604 is sufficiently early to complete exposure of the CCD 108 before expiration of the audio recording period. Therefore, at a time t 15 , i.e., at the end of the shutter control signal S 1 , the video data read control signal Sc 2 is transmitted to the CCD. At the same time, the audio data read control signal Sc 4 is transmitted from the video recording controller 510 to the gate 516. At the same time, the gate 512 is still outputting the write-enabling signal Sc 5 , and it also sends a disabling signal Sc 7 to the gate 516 (refer to FIG. 1). Therefore, despite the presence of the audio data read control signal, the audio data may not be read out of memory. At a time t 16 , the write-enabling signal Sc 5 , i.e., the audio recording period ends. At the same time, the disabling signal Sc 7 for the gate 516 ends. As a result, the gate 516 is free to transmit the read-enable signal Sc 6 to the memory 206. As a result, the audio data can be read from memory 206 after the time t 16 . Thus, the video data and audio data are written to the magnetic disk 302 at different times.
As mentioned above, the remote controller 600 in the preferred embodiment of the invention allows not only MANUAL mode operation but also AUTO mode operation. FIG. 5 shows an example of AUTO mode operation.
The mode selector switch 606 is shifted to the AUTO mode position to select AUTO mode. As a result, the audio recording button 602 is disabled. The remote controller 600 becomes active in response to depression of the video recording button 604 at a time t 21 . In this case, the remote controller 600 transmits the audio recording demand signal in response to depression of the video recording button. This initiates recording of audio data in memory 206 for the given period of time, e.g. 10 sec, starting at time t 22 .
After a predetermined delay which may be manually adjustable as set forth above, the remote controller 600 transmits the video recording demand signal at a time t 23 . In response to this, video data is picked up by CCD 108.
It should be appreciated that the predetermined delay time has to be longer than the time needed to bring the disk drive motor 308 up to speed. Therefore, the minimum delay time available to the manual adjusting means should be longer than the warm-up time of the disk drive motor.
The subsequent steps for transferring the audio and Video data to the magnetic disk 302 from the memory 206 and CCD 108 are essentially the same as disclosed with respect to FIG. 4.
As will be appreciated herefrom, the present invention fulfills all of the objects and advantages sought therefor.
It should be appreciated that, while the invention has been disclosed in terms of the specific embodiment, various embodiments and modifications to the shown embodiment would be possible without changing the significance of the invention.
For example, although the microphone is installed in the camera in the shown embodiment, it would be possible to use a wireless microphone installed in the remote controller or independent of the camera and the remote controller.
Therefore, the invention should be understood to include all possible embodiments and modifications to the shown embodiment which do not depart from the principle of the invention, which is set out in the appended claims. | An electronic still camera has a video recording feature and, in addition, an audio recording feature. The electronic still camera can control video recording timing and audio recording timing in accordance with the user's desires. The electronic still camera is also provided with a remote control system which can control video recording timing and audio recording timing in a mutually variable timing relationship. The electronic still camera has a video recording system and an audio recording system built into the camera, a data recording system including a recording medium for receiving video data from the video recording system and audio data from the audio recording system for recording and reproduction, and a remote control system associated with the video recording system and audio recording system for operating the video recording system and audio recording system. The remote control system can be used to adjust the video recording timing and audio recording timing relative to each other. Preferably, the remote control system includes manually operable device for operating the video recording system and the audio recording system at different timings. More preferably, the manually operable device has a remote controller which includes a independent video recording and audio recording switches. | 8 |
GENERAL DESCRIPTION
The present invention relates to a bicycle wheel with a plurality of spokes extending between a hub and a rim to which at least one disk cover is removably attached in order to provide the wheel with a lateral fairing.
All types of bicycles (touring, racing, mountain bikes, etc.) have in common that the energy produced by the rider is largely used to overcome the air resistance, the driver's frontal area making the biggest contribution to drag, followed by the wheels.
In order to reduce the effect of the wheels on air resistance, various embodiments of fully integrated disk wheels have been introduced. Fully integrated disk wheels are completely covered on both sides, the disk cover serving as a load carrying element for both tension loads and other kinds of loads during the ride.
Compared to spoked bicycle wheels, the disadvantage of the fully integrated disk wheels is their distinctly poor ability to absorb road shocks. In addition, their rolling performance is noticeably rougher than that of spoked wheels. Furthermore, due to the disk's stiffness, fully integrated disk wheels produce considerably more noise during the ride.
In order to transfer the aerodynamic advantages of a fully integrated disk wheel to a conventional spoked wheel, the U.S. Pat. No. 4,712,838 for instance recommends to provide the spokes adjacent to the rim with a number of clips by which a disk cover is held in place serving as a lateral fairing of the bicycle wheel.
Another method already in use employs a plastic film which is supported at the hub, stretched and glued at the outer edge to the rim of the wheel, in particular to the rim side walls.
Both the clip disk cover as well as the adhesively joined plastic film are usually fitted to both sides of the wheel, the spokes remaining inside the fairing.
The disk cover as disclosed in the U.S. Pat. No. 4,712,838 has the drawback of an air gap formed between the disk edge and the rim, thereby increasing the air resistance over that of the fully integrated disk wheel. In addition, changing of the disk cover requires undoing numerous fastening elements. Since these are simply clipped to the spokes, they can get lost. In this case, the disk cover is no longer uniformly supported along its circumference by the wheel.
Regarding the adhesively joined plastic film cover, damage of the plastic film requires its removal costing time and money. To inflate the tire, access to the valve is rather difficult in both cases.
Therefore, it is the intent of the present invention to improve the removable fastening of the lateral wheel cover by simultaneously providing the cover with a snug fit on all rim shapes omitting edges, bolts, air gaps or the like.
For a bicycle of the kind disclosed in claim 1 of the U.S. Pat. No. 4,712,838, the present invention offers a satisfactory answer to the above intent by providing the rim laterally with at least one circumferential catch groove into which the disk cover is engaged.
On the rim the catch groove is formed between the spoke hole side and the side wall of the rim. A catch groove of this kind can be formed on all types of rims, as for instance aluminum rims, stainless steel rims, hollow cross-section rims or concave flange rims. Catch groove fitted rims can therefore be used with both wire reinforced tires and folding tires. The disk cover disclosed by the present invention is simply clipped to the hub and then inserted in the catch groove along its outer edge. Since the catch groove is formed as an integral part of the rim, no additional fastening elements are needed. Neither air gaps nor edges are produced between the disk cover and the rim and/or rim side wall. The disclosure by the present invention offers a complete lateral wheel cover of optimum aerodynamic design as is usually provided only by the fully integrated disk wheel. At the same time, the bicycle wheel disclosed by this invention offers all advantages of the spoked wheel. All hub and spoke types in use for bicycles are suitable. Instead of conventional wire spokes, tensioned high-strength fibers, made of Kevlar, for instance, can be used to connect the hub and the rim.
By completely covering the bicycle wheel, an enclosed interior is obtained which is most favorably protected against humidity, dirt and wear from entering road debris or the like.
At the same time, the rim side walls can be fully used as braking surfaces in contrast to the plastic film cover which is glued to the rim side walls. In addition, ease of maintenance and access to the valve of the spoked wheel is maintained in contrast to the fully integrated disk wheel and/or the adhesively joined plastic film cover.
A favorable embodiment of the present invention consists of an essentially circular hoop and a cover which is stretched over and retained by the hoop. The diameter of the hoop is of a size which permits the disk cover to be engaged easily in the catch groove and to be held firmly therein during the ride. The so formed wheel covers are easy to handle and assembled. The center opening of the cover is provided with a clip ring by means of which the disk cover is installed on the hub. The clip ring fits on the hub flange into which the spokes are inserted.
A preferred embodiment of the present invention consists of a recessed catch groove located in the section between the spoke hole wall and the side wall of the rim in which the disk cover having an edge reinforcement is engaged and held. This extremely easy method of installation provides a sealed joint between the disk cover edge and the rim, keeping the outside surfaces of the rim smooth.
By using an elastic edge reinforcement in the edge of the cover, preferably of circular or tubular cross section, a particularly simple and elastic joint between the rim and disk cover is obtained enabling quick installation and removal of the disk cover.
On the inside, the outer edge of the disk cover can be provided with a ring-shaped web by means of which it is engaged in a respective groove of the rim.
A simple embodiment of the present invention consists of a catch groove having a semicircular shape enabling the disk cover to be securely held in place and to be easily removed.
Bicycle rear wheels are offset at the hub in order to allow for the accommodation of multi-speed gear clusters on one side of the wheel. For rims of offset wheels it is of advantage to have the rim side wall on the gear cluster side generally parallel to the wheel centerline, while in the direction of the hub the rim side wall on the opposite side of the wheel is outwardly inclined at an acute angle with the centerline. This configuration enables the disk cover to be installed generally vertically on the sprocket side without interfering with the gear clusters. Whereas on the opposite side of the wheel, the disk cover is installed at an inclined angle.
In this context, it is of advantage to have the inclination of the rim side walls parallel with the inclination of the cone-shaped configuration of the spokes.
Furthermore, it is advantageous for the installation of the disk cover to have the opening of the catch groove in the straight rim side wall face downward toward the hub, while the opening of the catch groove in the inclined rim side wall is swiveled or inclined outward.
It is of further advantage when the inclined angle of the catch groove and the angle of inclination of the rim are essentially identical. In this case, extending from the inclined rim side wall at the side wall's angle of inclination, the disk cover will cover the wheel down to the hub in such a way that there will be neither edges nor irregularities in the section between rim and disk cover.
In order to enable the spokes to be inserted in the spoke holes between the catch grooves with ease and at a certain angle of inclination, it is of advantage to have the spoke holes in the rim, especially those belonging to the spokes of the gear cluster side, offset from the centerline toward the .inclined rim side wall. In this manner, the spokes can be arranged at a reduced angle of inclination.
A preferred embodiment of the present invention provides for the spoke holes to be arranged offset from the rim centerline on the side of the inclined rim side wall. In addition, it is of advantage to have the spoke inserted in the hole closer to the inclined rim side wall at a greater angle with the spoke hole centerline than the spoke inserted in the hole closer to the rim centerline. The spoke hole centerline is essentially parallel to the rim centerline and offset toward the inclined rim side wall.
In order to improve the stiffness of a hollow cross-section rim, especially with an asymmetric configuration, it is of advantage to provide the hollow section with an essentially vertical reinforcing rib.
In addition it is advantageous to have the cover stretched over the hoop provided with a hollow casing on its inside into which a cord is incorporated for tightening the cover. By means of the tightening cord the cover can be easily installed on and removed from the hoop. It is easy to change the cover material, the color of the cover or the cover for cleaning.
Depending on the cover material used, the tightening cord can be omitted. A thermal treatment can be applied to fasten the cover by shrinking it on.
Another embodiment of the present invention consists of a cover which is glued to the hoop. In this case, the hoop is a flattened ring, one flat side being used to fasten the cover by adhesive bonding.
For the cover material a fabric, a film, a fabric-backed fabric, a coated fabric or the like can be used. The choice of the material depends on the conditions of the intended use, i.e., weather, wear or the like. The hoop is preferably made of a metallic or composite material. Due to its elasticity and low weight, titanium is a good choice for the hoop. In addition to a flexible material, a composite material can be used for the disk cover. In this case, the disk's outer edge is provided with the hoop profile making cover and hoop an integral part.
Another embodiment of the present invention consists of a profiled disk located on the inside of the wheel cover concentric with the hub of the wheel. The disk serves for contouring the wheel cover, thereby keeping the spokes from pushing through the wheel cover.
For easy access to the valve in the rim, it is of advantage to provide the wheel cover with an opening in the valve area through which the tire pump can be inserted.
In addition, it is of advantage to provide a device at least for expanding the hoop inside the access opening. There is a gap on the hoop and the expanding device is movably mounted to the free ends of the hoop which confine the gap. By moving the expanding device the diameter of the hoop is adjusted.
For installation, the wheel cover is simply inserted into the respective catch groove and fixed in position by expanding the hoop. For removal of the wheel cover, the order is reversed. Being actuated, the expanding device pushes the free ends of the hoop apart in the direction of the circumference. For removal of the wheel cover, the expanding device is simply released so that, due to the hoop's elasticity, the free ends of the hoop meet.
An interesting embodiment of the expanding device consists of a spring element acting in the direction of the hoop's circumference. For installation of the wheel cover, the spring element is compressed by hand. As soon as the hoop has engaged the catch groove, the spring element is released, thereby expanding and fixing the hoop in position.
Another embodiment of the expanding device consists of a rotating eccentric disc acting on the free ends of the hoop which are bent inward in a generally radial direction. By simply turning the eccentric disk, the free ends adjoining the disk are expanded, whereby the hoop is fixed in position in the catch groove.
A still further favorable embodiment of the present invention comprises the free ends of the hoop which are bent inward in a generally radial direction and away from each other as well as an expanding device which consists of a wedge designed to slide along the free ends of the hoop. The free ends are increasingly spaced apart in the direction of the center of the disk cover so that they are pushed apart when the wedge is moved toward the rim. By moving the expanding wedge along the free ends of the hoop, the disk cover can be fixed in position and/or removed in an easy manner.
In order to form a simple valve access opening and to hold and secure the free end of the loop in an easy manner, it is of advantage to provide an essentially U-shaped elastic frame to confine the access opening in the disk cover and to insert the free ends of the hoop in the U-legs of the frame, while the expanding wedge is slidingly arranged between the U-legs. With the help of the frame, the disk cover is favorably protected against damage or tearing at the access opening. By securing the free ends inside the U-legs, they are not in direct contact with the cover, thereby being prevented from damaging the cover. Moreover, damage to the free ends of the hoop is thereby avoided. The expanding wedge being arranged between the U-legs, the hoop can be easily adjusted by sliding the wedge toward the rim.
In this context, it is of particular advantage to have the expanding wedge and the U-legs provided with a tongued and grooved joint. For example, the expanding wedge can be fitted with two lateral grooves into which are engaged the respective tongues on the inside of the U-legs. In this manner, the expanding wedge is securely held in place, especially in its fully expanded position when it is tangent to the rim. Having been released from its position, the expanding wedge can be removed from the frame depending on the depth of the engagement.
In order to easily secure the expanding wedge in its expanded position, it is of advantage to provide the U-legs with a lug. Provided with corresponding projections, the expanding wedge engages this lug. It is safely secured due to the elasticity of the frame.
In order to easily seal the access opening, it is of advantage if a lid is pivotably fastened to the end of the expanding wedge opposite the rim. In its fully extended position, the expanding wedge and the lid will seal the access opening completely.
Furthermore, it is of advantage to arrange the lid and the expanding wedge flush with the wheel cover, thereby avoiding edges which increase drag.
An easy way to fasten the lid is to fit it with a snap nose which engages the web of the U-frame by gripping around it, thereby holding the lid in position.
For easy handling of the lid, it is of advantage to provide it with a fingerhole. By inserting a finger, for example, the lid is pivoted outward, thereby also allowing the removal of the expanding wedge from its expanded position.
The rim is jointed to a circular hoop with a closely fitting plug inserted at the joint. The thereby increased mass at this point of the rim causes a certain imbalance. In order to restore wheel balance to a certain extent, it is advantageous to locate the valve access opening diametrically opposed to the rim joint.
Furthermore, it is favorable, if the U-shaped frame, the expanding wedge, and the lid supply essentially the weight necessary to balance the wheel which is unbalanced by the rim joint. By doing so, there is no need for additional balancing of the wheel.
For easy removal of the completely closed hoop from the catch groove, a preferred embodiment of the hoop is provided with at least one indentation oriented away from the catch groove, which helps to remove the hoop as if with a lever.
In order to facilitate levering the hoop, it is of further advantage to place elastic supporting pieces at intervals between the catch groove and the hoop. In this way, the hoop will react to a radially applied lever by moving outward in radial direction, thereby facilitating its removal.
For spring-actuated closing of the lid, it is of advantage to provide a spring element between the lid and the expanding wedge. The lid is closed through the force of this spring element and stays closed when a ride is started. In this way, starting a ride with an open lid is prevented and safety is increased.
In order to improve load transfer and to reduce peak loads, a preferred embodiment of the present invention consists of beveling the rim joint faces. The application of a beveled rim joint is not confined to the rim shapes depicted herein. Beveling of rim joints can be used on any type of rim, such as aluminum rims, stainless steel rims, hollow cross-section rims, concave flange rims or the like.
In order to affect neither the radial stiffness of the bicycle wheel nor the performance of the brakes, it is also of advantage, if the beveled face plane of the joint runs across the rim section between the rim side walls, the plane's normal meeting the circumferential line at an acute angle. The joint face is essentially perpendicular to the upper or lower side of the rim.
In order to further improve stability, it is of advantage to incorporate at least one socket inside the hollow section of the rim, extending at equal length to either side of the rim joint in the direction of the circumference.
Another advantage is to place the socket face parallel with the rim joint plane. By doing so, peak loads in the joint area are uniformly distributed between the joint and the socket.
It is of great advantage, if the hollow section of a rim which has been partitioned by a reinforcing rib is fitted with one socket each for each subsection.
In order to improve the braking performance of the rim, the wet rim in particular, it is of advantage to coat the rim side walls with a fine-grain ceramic coating. A ceramic coating of this kind can be applied to any known bicycle wheel. Plasma spraying is one of the methods used.
Due to the different elastic behavior of the ceramic coating and the rim, the ceramic coating can chip. To prevent chipping as far as possible, it is of advantage to provide the ceramic coating with a stress-relieving gap concentric with the hub. In general, the stress-relieving gap is located midway on the rim side wall, its thickness ranging from 0.3 to 0.8 mm.
The disclosures and preferred embodiments of the present invention are further described and depicted by the following figures.
BRIEF DESCRIPTION OF DRAWING
FIG. 1 discloses a side view of a rear bicycle wheel;
FIG. 2 discloses line II--II of FIG. 1 in cross-section;
FIG. 3 discloses an enlarged view of detail III of FIG. 2;
FIG. 4 discloses a side view of another embodiment of the present invention with an access opening in the wheel cover;
FIG. 5 discloses line V--V of FIG. 4 in cross-section;
FIG. 6 discloses line VI--VI of FIG. 4 in cross-section;
FIG. 7 discloses another embodiment of the expanding device of the present invention;
FIG. 8 discloses a side view of another embodiment of the present invention;
FIG. 9 discloses line IX--IX of FIG. 8 in cross-section;
FIG. 10 discloses another embodiment of the present invention relating to FIG. 3; and
FIG. 11 discloses a simplified drawing of a rim as seen from above.
DETAILED DESCRIPTION
FIG. 1 shows a partial side view of a bicycle 2. A rear wheel 1 is rotatingly mounted to the seat stay 8 and the chain stay by means of a hub 5. Not shown are the saddle to which the seat stay 8 extends and the crank axle to which the chain stay 9 extends.
A great number of spokes 3 are arranged between the hub 5 and the circular rim 4. For convenience, only a few spokes are shown in FIG. 1. The hub 5 is located in the center of the circular rim 4. On its circumference, the rim 4 is fitted with the tire 17.
Concentric with the hub 5, a multi-speed gear cluster is provided. Between the hub 5 and the rim 4, a disk cover 6 having a cover 12 is provided in order to cover the side of the wheel.
FIG. 2 shows a cross-section of the bicycle wheel 1 along line II--II of FIG. 1. For convenience, the tire 17 mounted on the rim 4 of FIG. 1 has been omitted in FIG. 2.
Both sides of the bicycle wheel are fitted with the disk covers 6 between the hub 5 and the rim 4. The disk covers are mounted to the wheel by inserting their outer edge by means of the hoop 11 into the catch groove 7 of the rim 4. The catch grooves 7 are located on the spoke hole side 22 directly adjacent to the rim side wall 20. The disk cover is provided with a cover 12.
The cover 12 extends from the hub ring 54 holding the disk cover at the hub 5 to the hoop 11. It is stretched around the hoop 11 inserted in the catch groove 7 and is finished off with a peripheral casing 13 which contains the tightening cord 14. On the inside 15 of the disk cover 6, profiled disks 23 are arranged concentric with the hub ring 54. The diameter of these disks is greater than that of the hub ring 54. The disks 23 serve to keep the cover 12 at a distance from the spokes.
The spokes 3 extend between the hub flange 21 and the spoke holes 18 located on the centerline of the rim 4. The method used to insert the spokes 3 in the hub flange 21 and to tighten them in the rim spoke holes 18 by means of nipples is well known to those skilled in the art. Extending from the hub flange 5, the spokes are more strongly inclined toward the vertical 55 than is the cover 12 of the wheel disk 6. Thereby all the spokes 3 stay inside the two lateral disk covers 6.
The tire is mounted on the bed 19 of the rim 4 opposite the spoke hole side 19 and separated from it by the hollow cross section 16. The rim bed 19 and the spoke hole side 22 are interconnected by an aperture which enables the spokes 3 to be fastened in the spoke holes 18. On one side of the bicycle wheel 1, the hub 5 which projects beyond the disk cover 6 is fitted with a gear cluster 10. On this gear cluster side of the wheel, both the spokes 3 and the cover 6 are less inclined toward the vertical 55 than those on the opposite side of the wheel 1.
FIG. 3 shows an enlarged view of detail III of FIG. 2. For convenience, both the spokes 3 and the disk covers 6 of FIG. 2 are omitted.
The rim 4 comprises two fairly straight rim side walls 20 spaced apart. In the section between the spoke hole side 22 and the rim side wall 20, the essentially semicircular catch groove 7 is located. In this section, the rim side walls are extended into a lip 48 which confines the catch groove 7. The spoke hole 18 is located on the centerline between the catch grooves 7 and between the rim side walls 20. It is connected to the rim bed 19. The hollow section 16 extends between the rim bed 19 and the spoke hole side 22. The rim bed 19 is laterally confined by the rim side walls 20 which, fitted with hooked edges, serve as mounting supports 49 for tires, wire-reinforced tires for instance.
FIG. 4 depicts the bicycle wheel 1 with the rim 4 and the disk cover 6. Located in the rim bed 19 is the valve 25. It projects from the spoke hole side of the rim 4 and is accessible through the opening 24.
The hoop 11 is inserted in the peripheral catch groove 7, partially disappearing therein. In the vicinity of the valve, there is a gap in the hoop 11 so that the catch groove is visible. The free ends 28 and 29 of the hoop 11 are bent toward the center of the wheel and are more or less parallel to each other.
In order to confine the valve access opening 24 and the free ends 28 and 29, an essentially U-shaped frame 35 is provided within the cover 12 of the disk cover 6. Its U-legs 36 point toward the rim 4, the U-web 37 being arranged at a right angle to the free ends 28 and 29. The U-legs 36 and the free ends 28 and 29 are of essentially the same length, the free ends being inserted into the opening of the U-legs 36.
The U-legs 36 increase in thickness toward the rim 4, the legs being essentially straight on the outside, but sloped on the inside approaching each other toward the rim 4.
On the inside of the opposing U-legs 36, a wedge-like expanding device is slidably arranged, its width decreasing in the direction of the rim 4. By sliding the wedge 34 radially toward the circumference of the wheel 1, the U-legs 36 including the free ends 28 and 29 of the hoop 11 are expanded in the direction of the circumference 31. When the end 30 of the wedge comes into a close fit with the catch groove 7, it assumes its fully expanded position. In order to secure this position, the inside of the U-legs 36 are fitted with lugs 39 which interlock with the respective projections of the wedge 34.
A lid 40 is provide between the expanding wedge 34 and the web 37 of the U-shaped frame. It seals the valve access opening 24 in conjunction with the expanding wedge 34.
The lid 40 is fastened to the wedge 34 by means of a pin 41 enabling the lid 40 to pivot. The spring element 44 is arranged coaxially with the pin. It actuates the lid 40 to close in the direction of the web 37 of the U-shaped frame.
For handling, the lid 40 has a fingerhole located approximately in the center thereof. The lid 40 is provided with a small tab 51 shaped to fit the U-web 37.
FIG. 5 shows a cross section along line V--V of FIG. 4. The valve 25 is located in the valve stem hole 50 of the rim 4. Similar to the spoke holes in FIG. 3, the valve stem hole 50 is positioned on the centerline of the rim 4.
The outer surfaces of the expanding wedge 34 and the lid 40 are shaped to be flush with the rim side walls 20. The end 30 of the expanding edge 34 is engaged in the catch groove 7. The pin 41 is situated between the lid 40 and the expanding wedge 34.
The position of the expanding wedge 34 shown in FIG. 5 depicts the lid 40 in its fully closed position. The small tab 51 fits the web 37 of the U-shaped frame 37 on one side, while the snap nose 42 projecting from the lid 40 engages the web 37 on the opposite side. By means of the spring element 44 shown in FIG. 4, the lid 40 is forced to close in the direction 47.
The fingerhole 43 is positioned on the outside of the lid 40 approximately midway between the small tab 51 and the pin 41. It gives access to a finger rest 56 inside the lid 40 which is oriented toward the web 37 of the U-shaped frame.
FIG. 6 shows a cross section along line VI--VI of FIG. 4. The expanding wedge 34 has a flat oval shape and the width 52. The sides are provided with grooves in order to engage the U-legs 36. The free hoop ends 28 and 29 are fed into the U-legs 36. They have a flat oval cross-section in order to be prevented from twisting inside the U-legs 36.
The width 52 of the expanding wedge 34 is less than that of the valve access hole 24 at the level of the fingerhole 43 as shown in FIG. 4. Therefore, the expanding wedge 34 together with the lid 40 is removable from the valve access hole 24, if pushed far enough toward the web 37 of the U-shaped frame.
FIG. 7 depicts another embodiment of an expanding device. The free hoop ends 28 and 29 confine a gap of the width 53 and are facing each other. A spring element 32 is located between the free ends by means of a sleeve 33. The free ends 28 and 29 are partially fed into the sleeve 33 and can be adjusted in relation to it.
FIG. 8 depicts another embodiment of the bicycle wheel 1 as disclosed by the present invention. The hoop 11 retaining the cover 12 is inserted in the catch groove of rim 4, thereby covering the bicycle 1 laterally with the disk cover 6. At one point of its circumference, the hoop 11 is provided with a dent 45 for handling. It is formed by bending a segment of the curved hoop 11 to the inside of the hoop.
A further embodiment of the present invention permits to place a number of elastic supporting elements 46 at intervals around the catch groove.
FIG. 9 shows a cross section along line IX--IX of FIG. 8 to illustrate the supporting elements. A supporting element 46 is located in the catch groove 7 of the rim 4, thereby providing a resilient support for the hoop 11.
FIG. 10 shows another embodiment of the rims disclosed by the present invention and the description of FIG. 3. The rim 4 is provided with the rim bed 19 serving as a mount for a tire which is not shown. According to the description of FIG. 3, the tire is mounted between the hooked edges of the rim walls 20 and 20' and held in place by the tire mounts 49.
The vertical centerline 55 is shown to extend between the upper part of the rim side walls or tire mounts 49 respectively.
The rim side wall as shown on the right side of FIG. 10 lies essentially parallel to the centerline 55, whereas the inclined rim side wall 10', upon extension of its line of inclination, makes an acute angle 63 with the centerline 55. In the direction of the hub as shown in FIG. 2, the rim side wall 20' is inclined outward. On the side of the essentially parallel rim wall 20, the multi-speed gear wheels 10 are mounted on the hub 5 as shown in FIG. 2.
As a whole, the rim 4 is asymmetric in relation to the vertical centerline 5. The catch groove 7 to the right side of the centerline 55 has an essentially semicircular cross section. The pertaining center and diameter of the semicircle are located on the horizontal 65. The catch groove 7' to the left side of the centerline 55 has also as essentially semicircular cross section. The pertaining center and diameter of the semicircle are located on a line which is inclined upward relative to the horizontal 65 at the angle 63. The center of the catch groove circle is located at the intersection between the horizontal 65 and the line inclined at the angle 62. Both catch grooves 7 and 7' are extended beyond the horizontal line 65. The extensions are essentially tangent to the circle line of the catch groove and are given a curving for integration with the spoke hole side 22 nd the rim side walls 20 and 20'.
The hollow cross section 16 is located between the catch grooves 8 and 7' the spoke hole side 22 and the rim bed 19. On the side of the catch groove 7, to the right of the center line 55, the hollow section is reinforced with an essentially vertical rib 57.
The reinforcing rib 57 divides the hollow section into two parts. The resulting smaller hollow section is located above the catch groove 7, the larger hollow section above the catch groove 7', both extending across the spoke hole side 22 of the rim. The wall thickness of the spoke hole side below the larger hollow section is greater than that below the smaller hollow section. There is a transitional zone under the reinforcing rib 57. On the spoke hole side 22 adjacent to the catch groove 7, a recess is provided in order to save material.
The spoke holes 18 and 18' are offset from the vertical centerline 55 towards the catch groove 7'. They are successively arranged in the rim according to common practice. The spoke 3 enters the spoke hole 18 at the acute angle 61 with the spoke hole centerline 58 being given an outward inclination on its way toward the hub. The spoke 3' enters the spoke hole 18' at the acute angle 60 with the spoke hole centerline 58 being given an outward inclination on its way to the hub. The spokes 3 and 3' diverge in the direction of the hub 5 shown in FIG. 2. They are hooked in the hub flange 21 according to common practice.
The spoke hole centerline 58 lies parallel to the vertical centerline 55 from which it is offset at a distance 59 toward the inclined rim side wall 20'. The acute angle 60 enclosed between the spoke 3' and the spoke hole centerline 58 is slightly bigger than are the acute angles 62 and 63 which are equal. The size of the angles depend among other things on the wheel diameter and the offset 59 between the spoke hole centerline 58 and the offset 59 between the spoke hole centerline 58 and the vertical rim centerline 55. For the embodiment of the present invention disclosed in FIG. 10, the angle 60 is essentially twice as big as the angle 61.
The ceramic coating 66 and 67 is shown to cover the surface of the rim side wall 20. It is divided into two equal sections which are spaced apart by the stress-relieving gap 68 by 0.3 to 0.8 mm. The circumferential gap 68 is located midway on the rim side wall 20, the coating sections extending equally far to either side of the gap in the direction of the vertical centerline 55.
For convenience, the corresponding ceramic coating on the opposite rim side wall 20' is omitted in the figure.
FIG. 11 shows a simplified view of the rim 4 depicted in FIG. 10 as seen from above in the direction of the rim bed 19. It illustrates the joint 76 of the rim 4. The joint is defined by the face plane 76 which extends across the rim 4 between the two rim side walls 20 and 20' the plane's normal 77 meeting the circumference 31 at an acute angle. The rim joint plane is essentially vertical between the rim bed 19 and the spoke hole side 22 shown in FIG. 2.
The sockets 70 and 71 are inserted into the hollow section 16 shown in FIG. 10 and/or are inserted into the hollow sections partitioned by the reinforcing rib. They can be made to match the shape of the partitioned hollow sections enabling their installation by a pressed fit. The faces 72 and 73 and/or 74 and 75 of the sockets 70 or 71 are parallel with the plane of the rim joint 69. The rim joint 69 is shown to not be transverse with the sides of the rim, i.e. it is beveled. As a result, the cross section of the sockets 70 and 71 is shaped like a parallelogram, the longer sides being parallel to the rim side wall 20 or 20' and the reinforcing rib 57. The shorter sides, i.e., the faces, being located at an approximately equal distance from the rim joint plane 69.
For a hollow cross section rim 4 without reinforcing rib 57, i.e., the hollow section being a single unit, the socket is a one-piece element, as a rule. | A bicycle wheel has a plurality of spokes arranged between a continuous profiled rim and a hub (5). At least one covering disk (6) is releasably secured to the wheel in order to provide it with a lateral cover. In order to obtain an easy to release and aerodynamically optimum cover, at least one continuous snapped groove (7) into which the covering disk can snap-in is shaped in the side of the rim profile. | 1 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] The present application claims the benefit of U.S. Provisional Application No. 61/286,125 filed Dec. 14, 2010, which is incorporated herein by reference in its entirety.
FIELD OF THE INVENTION
[0002] The present inventive subject matter relates generally to the art of woven fabric material and/or labels made therefrom. Particular relevance is found in connection with brand identification such as may be used with garment and/or apparel labels and/or other consumer products, and accordingly the present specification makes specific reference thereto. However, it is to be appreciated that aspects of the present inventive subject matter are also equally amenable to other like applications.
BACKGROUND OF THE INVENTION
[0003] Most garments or apparel items contain at least one brand identifier, product data or other information. The brand identifier may be printed, imaged or fully woven fabric, to create a brand identification label or tag. For example, these labels may contain any one or more of the following pieces of information: brand name, logo, fiber content, country of origin, care instructions, manufacturer codes, production lot, etc. The majority of these fabric labels are made of 100% polyester yarn. Other materials might include nylon, TYVEK®, cotton, etc. Polyester is used often due its desirable properties, e.g., such as low cost, high tear resistance and fabric hand or feel.
[0004] One common polyester fabric material used for labels is known generally as woven edge tape (WET). This material is typically woven in narrow ribbons whose width conforms to the final width the individual label. For example, if the finished label size is 60 mm in length and 33 mm wide, then that base material would typically be woven on a loom which weaves several 33 mm wide ribbons at one time. A conventional WET loom (referred to as a six space loom) may weave as many as 6 separate ribbons at a time.
[0005] WET has grown in popularity in part as a result of consumer preference for a softer label edge created by the weaving process combined with advances in rotary letterpress printing technology. The prior alternative method of creating polyester ribbon material was to weave polyester fabric in large widths (e.g., 50″-60″) and then hot slit it into individual ribbons. However, this created a label with an objectionably scratchy edge as the fused edge of the polyester material developed a crust. The advances in printing technology included the ability to print both the front and back side of the label and at the same time to be able to print up to six colors. Prior to this advancement commercial fabric label printing was limited to printing only 3 colors on one side of the label using screen printing.
[0006] With regard to label production, there is increasing interest in sustainability and/or environmentally friendly practices. For example, there is generally interest in adopting practices which reduce energy consumption, eliminate the use of carcinogenic and/or hazardous materials, employ more renewable or recycled source material, etc. In addition, there is a desire to increase the level of personalization and brand identity labeling.
[0007] There is a current desire that is being driven by a new level of consciousness related to preserving resources and the environment. Retailers and retail brand owners in an effort to satisfy the demands of consumers have begun seeking new ways to respond to consumer requests as well as delivering an impactful way of maintaining the brand integrity.
[0008] Accordingly, a new and/or improved fabric label and/or method for producing the same is disclosed which addresses the above-referenced problem(s) and/or others.
BRIEF SUMMARY OF THE INVENTION
[0009] The embodiments of the present invention described below are not intended to be exhaustive or to limit the invention to the precise forms disclosed in the following detailed description. Rather, the embodiments are chosen and described so that others skilled in the art may appreciate and understand the principles and practices of the present invention.
[0010] In accordance with one embodiment, a woven edge tape and/or label made therefrom as essentially described herein is provided.
[0011] In accordance with another embodiment, a method as essentially described herein is provided for making a woven edge tape and/or label therefrom.
[0012] In a further exemplary embodiment, a woven label material is provided having a pair of woven edges that run parallel to a machine direction, the woven label material is constructed from 100% post consumer waste material and is provided with indicia that may be printed by at least one of thermal transfer, direct thermal, wet ink or hot stamping. The woven edges extend both above and below a plane created by the woven material.
[0013] In a still further exemplary embodiment of the presently described invention, a method of making a woven edge label is described and includes the steps of initially providing a continuous web of material composed of approximately 100% post consumer waste. Then, separating the web into individual widths of material, each width corresponding to a width of a brand identification label. Next, first and second edges are created on each of the individual widths of material and each of the individual widths of material are printed with indicia. Finally, each of the individual widths of material are cut into separate brand identification labels.
[0014] In a still further exemplary embodiment of the presently described invention includes an apparel item to which a woven label constructed of approximately 100% post consumer waste is attached. The woven label including at least one of brand identification and care instructions and a security feature selected from at least one of EAS or RFID.
[0015] Other features and advantages of the present invention will become apparent to those skilled in the art from the following detailed description. It is to be understood, however, that the detailed description of the various embodiments and specific examples, while indicating preferred and other embodiments of the present invention, are given by way of illustration and not limitation. Many changes and modifications within the scope of the present invention may be made without departing from the spirit thereof, and the invention includes all such modifications.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The inventive subject matter disclosed herein may take form in various components and arrangements of components, and in various steps and arrangements of steps. The drawings are only for purposes of illustrating preferred embodiments and are not to be construed as limiting. Further, it is to be appreciated that the drawings may not be to scale.
[0017] FIG. 1 is photograph showing a slitter having distinct fusing and cutting operations used to convert a broad woven fabric into a plurality of ribbons in accordance with aspects of the present inventive subject matter;
[0018] FIG. 2 shows micrographs of different ribbon edges for comparison, one produced in accordance with aspects of the present inventive subject matter, the other produced conventionally;
[0019] FIG. 3 provides the woven material being cut into individual label lengths;
[0020] FIG. 4 shows a side elevation of an individual brand identification label;
[0021] FIG. 5 depicts a front few of an individual brand identification label; and
[0022] FIG. 6 illustrates a brand identification label produced in accordance with the present invention attached to an apparel item.
DETAILED DESCRIPTION OF THE INVENTION
[0023] The apparatuses and methods disclosed in this document are described in detail by way of examples and with reference to the figures. Unless otherwise specified, like numbers in the figures indicate references to the same, similar, or corresponding elements throughout the figures. It will be appreciated that modifications to disclosed and described examples, arrangements, configurations, components, elements, apparatuses, methods, materials, etc. can be made and may be desired for a specific application. In this disclosure, any identification of specific shapes, materials, techniques, arrangements, etc. are either related to a specific example presented or are merely a general description of such a shape, material, technique, arrangement, etc. Identifications of specific details or examples are not intended to be, and should not be, construed as mandatory or limiting unless specifically designated as such. Selected examples of apparatuses and methods are hereinafter disclosed and described in detail with reference made to FIGURES.
[0024] The present specification describes a woven fabric material and/or label along with a method for producing the same, wherein the material or label retains all or many of the performance characteristics of a conventional WET while being made largely from recycled material, e.g., 100% or nearly 100% post-consumer recycled material. In particular, the present specification describes a broad woven fabric which is cut to emulate a WET and is made from 100% or nearly 100% post-consumer recycled, polyester, PET (polyethylene terephthalate) and/or a method for producing the same. Suitably, the recycled polyester, PET is obtained from recycled plastics, such as soda bottles, consumer packaging or other similar beverage bottles or the like.
[0025] Suitably, the material and/or label proposed herein has a hand or feel (e.g., softness, etc.) which is as good or better than conventional WET, and the cost of material is equal to or less than conventional WET products. In exemplary embodiments, a ribbon cut from the broad woven fabric has an edge with the following qualities:
[0026] a. durability, i.e., an edge that does not unravel during laundering, e.g., as evidenced by it suitably standing up to an industry standard AATCC (American Association of Textile Chemists and Colorists) method 61-option 3A test;
[0027] b. softness, i.e., the edge is as smooth or smoother than the edge of conventional WET material; and,
[0028] c. visual appearance, i.e., the edge looks somewhat like a conventional woven edge, e.g., with a selvedge of approximately 0.7 to 0.8 mm wide.
[0029] In one exemplary embodiment, the ribbon conversion process is able to convert broad woven fabric (e.g., 60″-70″ wide) at very high speeds (e.g., 90-180 feet/min) in order to meet large demands. In contrast, traditional hot knife slitting of polyester not only yields an inferior rough edge but is also very slow, e.g., as slow as 10-20 ft/min, making it an impractical process for meeting the demands for very large volumes of converted ribbons.
[0030] Suitably, the fabric proposed herein contains or has certain properties (e.g., discoverable via forensic testing or otherwise) so that it can be distinguished from its virgin polyester counterparts. This is desirable since customers may from time to time want to validate that the fabric used for the labels is truly made of recycled material. For example, there has been developed a means to distinguish the new labels or material disclosed herein from conventional virgin polyester WET. In particular, the method employs XRF (X-ray fluorescence) analysis which is a spectroscopic method that is commonly used to identify materials or components thereof in which secondary X-ray emission is generated by excitation of a sample with X-rays and can show the existence of certain chemicals which are not found in virgin polyester but are a component of recycled material. Another method known as DSC (Differential Scanning Calorimetry) may also be used. In particular, the melting point of virgin polyester is different from that of recycled PET and DSC analysis determines if the fabric is made of virgin polyester or recycled material or some blend thereof based upon this difference.
[0031] Optionally, the fabric is also able to be visibly authenticated. For example, a particular logo or trademark or other identifier (e.g., in the form of a watermark or the like) is applied to a fabric surface. Suitably, the identifier meets the following criteria: a) it is visible but does not adversely affect the legibility or washability of other printed text or the like appearing on the finished label; and b) it is legible or otherwise visible to the human eye and of a size where at least one complete logo or image appears on any label that is of a minimum area, i.e., equal to the minimum size of a label cut therefrom, e.g., a 18 mm by 30 mm label.
[0032] The fabric or material may also contain indicia which can be produced in a number of ways such as by direct thermal printing, thermal transfer printing, flexographic, gravure, wet ink, hot stamping, non-impact printing or by any other suitable means.
[0033] The fabric or material web may also be provided with security devices, such as an EAS device or an RFID device, which can be provided at regularly spaced intervals that correspond to the individual length of a fabric label.
[0034] In order to achieve a very soft hand, a light weight weave construction is employed using a fine denier yarn. Suitably, the weave construction of the fabric includes a 75 denier yarn in the fill direction and a 150 denier yarn in the warp direction. In one exemplary embodiment, a 75 denier yarns is used in both the warp and fill to give even a softer feel.
[0035] Suitably, the yarn used is made from recycled PET (RPET) that is extruded into filaments or strands. In one suitable embodiment, each 75 denier yarn is actually comprised of 36 individual strands or filaments which are twisted in line to make the one yarn. The finer the denier yarn the more difficult it is for a yarn extruder to make using RPET due to the fact that the RPET often has minute impurities therein. For example, these impurities originate from recycled bottles and can be comprised of paper, polyethylene from the bottle cap, glass, etc. Making this fine denier of a yarn using RPET is difficult, e.g., since the impurities tend to block up the filter portion of the extrusion unit. Notably, due to the fact that the individual strands are so fine in 75 denier yarn, any impurities making there way into the yarn can result in a web break on the extruder or adversely impact the tensile strength of the completed yarn which then might create a yarn break on the weaving machines in subsequent production of the fabric itself. Accordingly, it is important to strike an optimal balance between the two opposing factors of the yarn: lower denier for softness and higher denier for strength.
[0036] Hand is generally a function of the overall weight of the fabric. A traditional fabric weight for WET labels is around 125-130 gms/m 2 . However, RPET yarn is generally more costly then traditional polyester yarn. Accordingly, in order to achieve good hand and also to achieve lower costs, a fabric construction made from RPET yarn as proposed herein has a weight of approximately 110-115 gms/m 2 , thereby reducing the amount of yarn employed and in turn reducing the cost of production. Additionally, reduced weaving costs are realized by weaving in large widths, e.g., about 60″-70″, and slitting at higher speeds, rather than weaving individual ribbons which is much slower.
[0037] In general, it is desirable for a label to have a durable edge, but it is also desirable to produce the ribbons at relatively high speeds. With conventional slitters, a relatively wide fabric web is cut into ribbons or otherwise divided with one or more heated slitting knives. To get a sufficiently durable edge, a conventional slitter typically runs at a speed of about 10-15 fpm (feet per minute). The relatively slow speed allows a sufficient dwell time of the knife next to or proximate the created edge of the ribbon in order for the heat from the knife to properly melt and fuse the polyester, thereby creating the desired durable edge. If a conventional slitter is run faster, there is commonly insufficient time for the heat from the knife to suitably fuse the edge and impart the desired durability. Of course, it is to be understood that the amount of heat transferred from the knife in a given time (e.g., via conduction) to sufficiently melt and/or fuse the edge of the ribbon is limited in part by the relatively thin or narrow edge of the knife making contact with the fabric. According to Fourier's Law, when two solid bodies come into contact with one another (e.g., the heated knife and the fabric web), heat flows from the hotter body to the colder body and the heat flow is directly related to the contact area between the bodies. Therefore, when the contact area is relatively small (e.g., as is the case when the edge of the heated knife contacts the fabric), then the heat flow from the knife to the fabric is also relatively small. Accordingly, a longer dwell time and/or slower run speed is demanded in order to permit a sufficient amount of heat to be transferred so that the edge of the ribbon is suitably melted and/or fused to the degree appropriate for achieving the desired durability.
[0038] With reference now to FIG. 1 , there is shown an exemplary slitter 10 usable in accordance with aspects of the present inventive subject matter. Generally, the present slitter divides, (i) the fusing function and (ii) the cutting or slitting function, into two distinct operations.
[0039] First, the web under goes fusing where the edge of each ribbon is to be ultimately formed. As illustrated in FIG. 1 , one or more heated fusing elements or rollers 20 conduct the fusing. Suitably, a plurality of heated fusing elements or rollers 20 are spaced out along the width of the web at the desired slitting locations or widths. More specifically, at and/or near the region where the heated fusing elements contact the web, the fabric or fibers thereof are melted and/or fused together. Accordingly, as the web moves past each of the heated fusing elements 20 , this forms a track wherein the fabric or fibers of the web are fused together.
[0040] Second, the web is run past one or more slitting knifes or cutting wheels 30 . For example, as shown in the illustrated embodiment, there is one knife or cutting wheel that corresponds to each heated fusing element/roller 20 . More specifically, each slitting knife or cutting wheel is likewise space out along the width of the web at the desired slitting locations or widths. Suitably, each knife or cutting wheel cuts or otherwise separates the web at or near the middle of the fused track formed by the corresponding heated fusing element/roller. Suitably, the width of the track is controlled by the width of the heated fusing element/roller. For example, in one suitable embodiment, the heated fusing element/roller has a size and/or width that is chosen so that when the track is slit or otherwise divided in half it yields a fused edge with a width of approximately 0.7 mm to approximately 0.8 mm, which gives the slit fabric the appearance of a traditional WET which has a woven selvedge of about 0.6 mm.
[0041] Notably, without an appreciable loss of desirable edge quality, the run speed of the slitter illustrated in FIG. 1 is significantly improved over traditional slitters employing heated knifes to perform both the fusing and cutting functions. In part, this is because the fusing is performed by a separate element or roller which in turn improves the heat transfer to the web due the larger contact area therewith as compared to the contact area achieved with a conventional heated knife. That is to say, insomuch as the contact area is enlarged to allow better heat transfer to the web, the run speed of the web can be increased while still permitting a sufficient amount of heat to be transferred to the web so as to obtain a suitable degree of melting and/or fusing of the web fibers that in turn results in the quality edge desired.
[0042] For example, FIG. 2 shows micrographs of the edges of two different ribbons for comparison. Notably, the edge 50 produced by the present method (as shown in the image on the left) as compared to the conventional process 40 (as shown in the image on the right) is smoother and hence has a softer feel. Again, suitably, the ribbon conversion process is able to convert broad fabric woven (e.g., from about 60″ to about 70″ wide) at very high speeds (e.g., from about 90 to about 180 feet/min) in order to meet large demand. Traditional hot knife slitting of polyester not only yields an inferior rough edge but is also very slow (e.g., from about 10 to about 20 ft/min) making it an impractical process for meeting very large volumes of converted ribbons.
[0043] Optionally, to provide visual identification of the label as being made from recycled material, a logo or other image or some form of indicia or identifier is printed on the fabric surface that will provide visual confirmation that the fabric is in fact made of recycled material, e.g., 100% or nearly 100% recycled PET. In order to achieve this, a suitable pattern is print in a very faint watermark across the web of the fabric, e.g., just after weaving it. Suitably, the printing is done while the fabric is in wide form (e.g., 60″-70″) in order to make it economical. For example, the printing technology can be either be ink jet or rotary screen if printed in wide form. Optionally, the fabric can be printed using a dry toner digital press.
[0044] Reference is now directed to FIG. 3 which provides a schematic of a process for producing brand identification labels of the presently describe invention. The material is provided in a continuous format 60 having a plurality of segments 62 , 64 defining individual label lengths. The continuous web is fed to a cutting device 66 which separates the web 60 into individual brand identification labels 68 , 70 . A web 72 providing security devices 74 , 76 are unwound and attached to each of the brand identification labels as they advance beyond a particular position. The security devices may be provided as “inlay” such as are available from Avery Dennison RFID Company of Clinton, S.C. The inlays may be attached via adhesive or may be included as in a pocket formed in the web of material. The separated brand labels 68 , 70 are then collected 78 for later use.
[0045] FIG. 4 provides a cross section of a brand identification label 80 produced in accordance with the present invention. The label 80 has a planar surface 82 which makes up at least 90% of the surface area of the label and preferably more than about 95%. The label 80 has first and second edges 84 and 86 which are produced in a machine direction. As can be seen from the drawing, the first and second edges extend above and below the planar surface and are generally perpendicular to the planar surface.
[0046] Turning now to FIG. 5 , a complete brand identification label 90 , having first and second edges 92 , 94 running substantially longitudinally to the planar surface 96 . The planar surface 96 is provided with indicia 97 , 98 which may identify the brand and provide care instructions. In addition, the label 90 is shown with a security device 100 .
[0047] Reference is directed to FIG. 6 , which shows an apparel item 200 having an opening 210 to which a first brand identification label is attached 220 in the opening and a second label 230 is attached at a different location.
[0048] In any event, it is to be appreciated that in connection with the particular exemplary embodiment(s) presented herein certain structural and/or function features are described as being incorporated in defined elements and/or components. However, it is contemplated that these features may, to the same or similar benefit, also likewise be incorporated in other elements and/or components where appropriate. It is also to be appreciated that different aspects of the exemplary embodiments may be selectively employed as appropriate to achieve other alternate embodiments suited for desired applications, the other alternate embodiments thereby realizing the respective advantages of the aspects incorporated therein.
[0049] It is also to be appreciated that particular elements or components described herein may have their functionality suitably implemented via hardware, software, firmware or a combination thereof. Additionally, it is to be appreciated that certain elements described herein as incorporated together may under suitable circumstances be stand-alone elements or otherwise divided. Similarly, a plurality of particular functions described as being carried out by one particular element may be carried out by a plurality of distinct elements acting independently to carry out individual functions, or certain individual functions may be split-up and carried out by a plurality of distinct elements acting in concert. Alternately, some elements or components otherwise described and/or shown herein as distinct from one another may be physically or functionally combined where appropriate.
[0050] It will thus be seen according to the present invention a highly advantageous fabric label constructed from recycled material has been provided. While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it will be apparent to those of ordinary skill in the art that the invention is not to be limited to the disclosed embodiment, and that many modifications and equivalent arrangements may be made thereof within the scope of the invention, which scope is to be accorded the broadest interpretation of the appended claims so as to encompass all equivalent structures and products. | The present invention relates to brand identifiers, more particularly to woven labels used to mark, advertise or otherwise brand apparel and other consumer articles to identify the source of the particular goods. The woven labels of the present invention are preferably composed of post consumer waste or recycled materials, such as polyethylene, PET, polyester, cellulosic and other readily available materials that may be converted for the purpose of the present invention. | 3 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The invention relates to a connecting device for fluid conduits.
[0003] 2. Prior Art
[0004] Generically, the connecting device for fluid conduits is designed with at least one connecting element that is suitable for tightly connecting two lines to one another.
[0005] A tight connection is understood to mean a pressure-tight connection which in particular prevents the discharge of liquid under pressure.
[0006] The connecting device for fluid conduits is provided in particular in coffee and espresso machines.
[0007] According to the prior art, hose and tube connections are produced by adhesive bonding, for example. However, such connections involve connection procedures that require precise timing, in particular for the curing of an adhesive. The finished connections are not easily detachable.
[0008] Other, detachable connections are achieved, for example, using coupling nuts and cooperating threaded connecting parts. These connection arrangements require parts that are expensive to manufacture, in addition to time-intensive installation procedures.
[0009] The prior art also includes a tube connection having a clamping sleeve comprising two sleeve half-shells which screw into one another and whose flange-like projections are tightened together by screws (DE-A-198 37 803). The clamping sleeve overlaps two tube ends, a first tube end having an annular bulge and a second profiled tube end having a section of larger diameter. In addition, due to the screwing and tightening the clamping sleeve is cumbersome to install, and is not very well suited for connecting two hose ends.
[0010] Other tube connectors of the prior art are used only for connecting a specialized tube end to at least one annularly expanded wall (DE 41 42 640, U.S. Pat. No. 6,086,118).
[0011] In one known connecting device for fluid conduits of the aforementioned generic type to which a hose end can be connected, a metal ring is used as a coupling sleeve, from which internal hook-shaped projections are formed which externally engage with the hose end as a first line (U.S. Pat. No. 3,637,240). In particular by eddy-current induction in, and accompanying heating of, the metal ring, the hook-shaped projections are anchored in the plastic line thus softened. However, nicks are created in the hose end, thus weakening it. On the other side, a connecting sleeve has an internal borehole in which the hose end can engage, in addition to an expanded internal borehole into which the metal ring on the end section of the first line fits. In a space in the connecting sleeve, between an annular shoulder formed between the internal borehole and the expanded internal borehole, and a front annular front face of the metal ring, a sealing O-ring made of rubber or an elastomer is inserted which contacts the front annular end face of the metal ring but which does not simultaneously contact the annular shoulder in the connecting sleeve. Thus, a seal can be produced on an internal peripheral side and on the external peripheral side of the metal ring only when the O-ring is tightly fitted to both the first line and the internal periphery of the connecting sleeve. For installation, an essentially U-shaped clamp is used which is inserted into lateral boreholes in the connecting sleeve, namely, behind the connecting sleeve that is inserted into the connecting sleeve together with the end section of the first line.
BRIEF SUMMARY OF THE INVENTION
[0012] The object of the present invention, therefore, is to provide a connecting device for fluid conduits that functions using connecting elements that are easily manufactured, with connection procedures that are quickly performed, while at the same time providing a good external seal for the lines connected to one another. The connecting device for fluid conduits is distinguished by versatile applications, and, if necessary, line connections made with same are detachable.
[0013] This object is achieved by a connecting device for fluid conduits having the features stated in the characterizing part of claim 1 .
[0014] The object is achieved by placing on an end section of a first line a coupling sleeve having an annular end face on the front side, i.e., external to the connection side, that has an annular shape next to a first line end, and having a rear, annular end face situated at a distance from the first line end, that makes positive friction fit contact. For this purpose, the inside of the coupling sleeve has a simple, continuous cylindrical peripheral wall that is placed, for example crimped, on a correspondingly continuous end section of the first line, which similarly has no bead-like expansion. In this respect, a line may be understood to be a flexible line or a hose, in particular made of plastic, or a rigid line or line section made of plastic, or a metal tube. A connecting sleeve that projects from one end of a second line to be connected to the first line is suitable for receiving the end section of the first line together with the coupling sleeve.
[0015] Inside the connecting sleeve, at the end of the second line or of the line section forming the second line, an annular shoulder is provided which together with the front annular end face of the coupling sleeve performs a sealing function. By detachably placing a locking element on the connecting sleeve, which locking element in the interlocked state of the coupling sleeve and the connecting sleeve contacts the rear end face of the coupling sleeve, in the inventive design of the fluid connection arrangement, in particular for the interior of the connecting sleeve and the length and position of the coupling sleeve on the end section of the first line, the front annular end face of the coupling sleeve directly or—via a sealing element, indirectly—comes to rest on the annular shoulder of the connecting sleeve. It is thus possible to achieve a fluid connection arrangement that provides a reliable seal, even at high internal pressures.
[0016] As a sealing element, in particular according to claim 2 , a simple O-ring may be used which is enclosed with a tight fit between the annular shoulder of the connecting sleeve and the front annular end face of the coupling sleeve. By pressing the O-ring between the annular shoulder of the connecting sleeve and the front annular end face of the coupling sleeve, the O-ring may also create a good seal on its outer periphery in the connecting sleeve and on its inner periphery on the end section of the first line.
[0017] In this manner, it is possible to achieve a tight fit of the coupling sleeve on the end section of the first line.
[0018] The mutually contacting walls of the coupling sleeve in addition to the connecting sleeve are essentially cylindrical according to claim 3 . These allow a reliable connection that is independent of the rotational position of the coupling sleeve and the connecting sleeve.
[0019] Further advantageous features of the connecting device for fluid conduits are stated in claims 4 through 16 .
[0020] According to claim 4 , the connecting sleeve is an injection-molded plastic part, which is favorable for manufacturing.
[0021] To further streamline manufacture, according to claim 5 , the connecting sleeve together with the end of the second line may be formed from plastic, it also being possible for the second line to be an outlet or inlet for another integral structural element. In this case, the second line is preferably a rigid plastic line.
[0022] However, according to claim 6 , it is also possible for the connecting sleeve to be made of metal, and to be soldered onto an end section of a metal tube as a second line.
[0023] The coupling sleeve which is mounted on the end section of the first line has a simple ring-shaped design, and is preferably made of metal. However, the ring may also be injection molded as a rigid plastic part.
[0024] An alternative embodiment of the connecting sleeve according to claim 8 has a first section that receives an end section of the first line in addition to a second section that is narrower than the first section and projects from one end of the first line. The front, annular end face is thus formed as a sealing surface by means of a shoulder between the first section and the second section. The inside diameter of the first section of the coupling sleeve corresponds to the outer diameter of the first line. The diameter of the second section is smaller than that of the first section. The second section projects beyond the end of the first line in the installed state, so that this end forms a guide for the coupling sleeve in the receiving connecting sleeve.
[0025] Furthermore, according to claim 9 , a support tube may be inserted into the end section of the first line which is able to support the end section when the coupling sleeve is pushed on.
[0026] By use of the form features of the aforementioned connecting device for fluid conduits, at least two connecting sleeves according to claim 10 may be formed in a common connecting part which comprises at least one line section connecting the connecting sleeves. In particular, the common connecting part may be designed with three connecting sleeves which are connected to one another in the connecting part via a branched line section. The latter connecting part may thus be referred to as a three-sided connecting part. As mentioned above, one of the connecting sleeves may also be an integral component of another structural element, such as a continuous flow heater, for ex ample.
[0027] Furthermore, two embodiments of the locking element have been developed which are used to hold the coupling sleeve in its desired position when inserted into the connecting sleeve:
[0028] In a first embodiment according to claim 12 , the locking element is designed as a spring clip that extends through an internally laterally open receiving slot in the connecting sleeve and comes to rest against the rear annular end face of the inserted coupling sleeve. If necessary, the spring clip may be removed from the receiving slot to detach the connection of the connecting sleeve to the coupling sleeve. Likewise, the spring clip is reusable.
[0029] In one variant, the receiving slot in the connecting sleeve is also laterally open to the outside. This allows for uncomplicated fabrication of the connecting sleeve and easier handling of the spring clip for locking or loosening the fluid line connection.
[0030] However, according to claim 14 , it is also possible for the connecting sleeve to be laterally closed to the outside, so that the spring clip essentially goes all the way into the receiving slot and is held therein, even when forces are exerted on the spring clip from internal pressure in the hoses, which in the worst-case scenario tend to laterally push the spring clip from the receiving slot.
[0031] Alternatively, the locking element according to claim 15 may be designed as connected half-shells that fold together. On their face ends the half-shells have ridges with recesses, so that the coupling sleeve and the connecting sleeve which receives the coupling sleeve are enclosed between the folded-together, interlocked half-shells and the ridges. By releasing the interlocking elements, the half-shells may once again be removed from the line ends with the connecting sleeve and the coupling sleeve to loosen the connection of the two line ends. Likewise, the half-shells are reusable.
[0032] According to claim 16 , both half-shells and the elements molded thereon are made of plastic.
[0033] It is particularly advantageous for the half-shells to be captively connected to one another as a single piece by means of a film hinge. This locking element may be economically manufactured and installed, since the relative position of the half-shells is fixed in place on the hinge side, and the half-shells need be connected only on the opposite side by interlocking elements in order to enclose the line ends.
[0034] All of the variants of the connecting device for fluid conduits according to the invention are suitable for quick assembly.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0035] FIG. 1 shows a first embodiment of the connecting device for fluid conduits as an exploded view;
[0036] FIG. 2 shows the connecting device for fluid conduits according to FIG. 1 , but completely assembled as a sectional drawing;
[0037] FIG. 3 shows a second embodiment of the connecting device for fluid conduits as a variant of the first embodiment, as an exploded view;
[0038] FIG. 4 shows a third embodiment of the connecting device for fluid conduits as an exploded view;
[0039] FIG. 5 shows the completely assembled connecting device for fluid conduits according to FIG. 4 , as a longitudinal section;
[0040] FIG. 6 shows a detail of the third embodiment, namely, a locking element having half-shells in the folded-up state in a front view; and
[0041] FIG. 7 shows a fourth embodiment of the connecting device for fluid conduits in the assembled state, in a sectional view.
[0042] Corresponding parts in the various embodiments are provided with the same reference numbers in all figures.
DETAILED DESCRIPTION OF THE INVENTION
[0043] Exemplary embodiments of the connecting device for fluid conduits according to the invention are described below, with reference to the drawings comprising seven figures, as follows:
[0044] FIG. 1 shows in detail a flexible plastic line as a first line 1 , together with a rigid plastic line as a second line 2 which is part of a structural element 3 , a continuous flow heater, for example (only partially shown), for connecting to a connecting device for fluid conduits.
[0045] For this purpose, a coupling sleeve 4 designed as a metal ring, which is used to fix the first line 1 in place in a connecting sleeve 5 , is crimped onto the flexible plastic line or first line 1 , just in front of its connection-side end. To prevent the flexible plastic line as first line 1 from being deformed by the crimping process and to ensure a secure seating of the coupling sleeve 2 , an inserted support tube 6 is located on the connection-side end of the flexible plastic line in the vicinity of the coupling sleeve 2 .
[0046] The connection of lines 1 and 2 is achieved by the connecting sleeve 5 , into which lines 1 , 2 are inserted. To create a seal, on the side of the connecting sleeve 5 an O-ring 7 is provided which contacts a connection-side end face of the coupling sleeve 4 (not designated by a reference number) and a shoulder (likewise not designated by a reference number) at which the second line 2 ends and the connecting sleeve merges into a section of larger inner diameter which receives the coupling sleeve 4 . The section of the first line 1 situated at the connection-side end of the coupling sleeve 4 is thereby pushed through the O-ring.
[0047] In the first embodiment according to FIGS. 1 and 2 and in the second embodiment according to FIG. 3 , the connection of the two lines 1 and 2 is locked by a spring clip 8 or 9 , respectively, which in each case is pushed through a pair of receiving slots oppositely situated in the connecting sleeve until the spring clip comes to rest against the end face of the coupling sleeve 4 facing away from the connection-side end. In the first embodiment according to FIGS. 1 and 2 , the receiving slots are laterally closed off in an expanded section of the connecting sleeve 5 ; an opening 10 only on the top side, visible in FIG. 1 , is located at right angles between the two actual receiving slots, not shown. On the other hand, in the embodiment according to FIG. 3 , the receiving slots 11 a and 11 b are laterally open to the outside, thereby simplifying the shaping of the coupling sleeve 12 . As a result, the spring clip 8 is situated inside the connecting sleeve 5 , and the spring clip 9 is situated partially outside the connecting sleeve 12 .
[0048] The third embodiment of the connecting device for fluid conduits according to FIGS. 4 and 5 is used to connect a first line 1 , which once again is a flexible plastic line, to a second line 13 , which in this instance is designed as a rigid metal line or tube. Accordingly, a coupling sleeve 4 and a support tube 6 are situated on an end section of the first line 1 in a manner similar to that described for FIGS. 1 and 2 . A connecting sleeve 14 in this instance is made of metal, and once again has a first section 15 of relatively large diameter which is suitable for receiving an end section of the first line 1 , in addition to a second section 16 of smaller diameter into which the second line 13 or tube is inserted in order to be soldered to the second section. As can be seen from FIG. 5 , between the first section and the second section a shoulder is formed on which the O-ring 7 comes to rest when the front section of the line 1 with the O-ring is pushed into the connecting sleeve until the O-ring 7 presses tightly against the front end face of the coupling sleeve 4 and the shoulder between sections 15 , 16 . The direction in which the first line 1 is pushed is indicated by an arrow 18 a in FIG. 4 , for example.
[0049] The pushed-together lines 1 and 13 can then be locked by clipping together two half-shells 18 , 19 , made of plastic, in the direction of arrows 18 b , 18 c to produce a closed, approximately cylindrical shape over the coupling sleeve 4 and connecting sleeve 14 . For this purpose, half-shell 18 has spring tabs 20 , 21 as interlocking elements which fit into slots 22 , 23 . Additional spring tabs, not shown in FIG. 4 , may be received by slots 24 , 25 . The slots thus have a locking function. As can be seen from FIG. 5 , when the half-shells 18 , 19 are in the clipped-on position their ridges 26 - 29 on the end-face side inwardly contact the rear, i.e., the side facing away from the connection site, end faces of the coupling sleeve 4 and connecting sleeve 14 .
[0050] It should be noted that the second line 13 once again may be a component of a structural element, not illustrated.
[0051] In FIG. 6 , half-shells 30 , 31 , shown from the front, are provided as injection-molded parts together with a film hinge 32 , and for mutual locking in the folded-down state (see arrow 18 d ) therefore have fewer spring tabs, e.g. 33 , and slots, e.g. 34 , which can engage with one another to securely enclose a connecting sleeve and a coupling sleeve.
[0052] One particularly interesting embodiment of the connecting device for fluid conduits is illustrated in FIG. 7 in which the connecting device for fluid conduits comprises a connecting part 35 from which three connecting sleeves 36 , 37 , 38 are formed. The common connecting part is thus suitable for receiving three lines which can communicate with one another in the essentially T-shaped connecting part. In a manner similar in principle, variants of the common connecting part can be provided for receiving only two lines, which can be connected to one another in elongated form or at right angles.
[0053] In the three-sided embodiment of the connecting part 35 , according to FIG. 7 two flexible lines 39 , 40 and a rigid line 41 are connected to one another. The rigid line may once again be a metal tube, a continuous flow heater, for example.
[0054] The rigid line is provided with a soldered-on coupling sleeve 42 at its connection point to the connecting part 35 , and comprises a first section 43 which receives an end section of the line 41 , and a second, end-side section 44 of smaller diameter which can be inserted into a central line section of the connecting part 35 . Between the first section 43 and the second section 44 of the coupling sleeve 42 a shoulder is formed which supports a sealing O-ring 45 . On its other side, the O-ring 45 rests on a shoulder of the connecting sleeve 36 or a connecting sleeve section of the connecting part 35 , at which point the connecting sleeve section merges into the line section 46 of the connecting part 35 , which has a smaller diameter than the outwardly oriented connecting sleeve section. For locking the rigid line 41 inserted into the connecting part 35 to the connecting part, and therefore also to the other lines opening into the connecting part, a spring clamp 47 is used which on one side rests in a receiving slot, not designated by a reference number, in the connecting sleeve 36 and on the other side pushes against a rear, in FIG. 7 an upper, end face of the coupling sleeve 42 .
[0055] The connecting sleeves 37 , 38 or connecting sleeve sections are shaped in the same way as the connecting sleeve 36 for the connecting part 35 , and are used for connecting the two flexible lines 39 , 40 to the connecting part 35 , for which purpose end sections of the lines 39 , 40 are provided with coupling sleeves and support tubes, not designated by reference numbers, as in the embodiments according to FIGS. 1 through 5 . Tightly fitting O-rings 48 , 49 are enclosed between the end-side, i.e., connection-side, end faces of the coupling sleeves and the shoulders of the connecting sleeves 37 , 38 . In this instance as well, the end sections of the lines 39 , 40 are held in their inserted position by spring clamps 50 , 51 .
[0056] The system of the connecting device for fluid conduits thus comprises only a few components, which may be combined with one another in numerous ways, namely: coupling sleeves, optionally with support tubes, connecting sleeves, or O-rings for sealing, and spring clamps or interlockable half-shells for locking the connection. | A connecting device for fluid conduits having at least one connecting element that is suitable for tightly connecting two line ends to one another, wherein a coupling sleeve ( 4 ) having a front annular end face and a rear annular end face makes positive friction fit contact with an end section of a first line ( 1 ). A connecting sleeve ( 5, 14 ) projects from one end of a second line ( 2, 13 ), and inside the connecting sleeve an annular shoulder is formed that is suitable for receiving the end section of the first line ( 1 ) together with the coupling sleeve ( 4 ). A locking element is detachably mounted on the connecting sleeve ( 5, 14 ) which contacts the rear end face of the coupling sleeve ( 4 ) inserted into the connecting sleeve. | 5 |
FIELD OF THE INVENTION
This invention relates generally to operations involving the handling and deployment of sand control screens used in down hole oil and gas well completion packing operations and more particularly to the apparatus used to make up and uncouple the various screen assemblies used in such operations.
GENERAL BACKGROUND
After the open hole in a well has been cleaned, what is known in the art as a gravel-packing screen and/or gravel-packing tool assemblies are run into the well bore. The tool assembly is usually run with one or more subsection screen sections extending from the toe of the well to the well casing with at least one joint located inside the well casing followed by several joints of blank tubing before being connected to a shear-out safety joint and the gravel pack tool itself. A wash pipe is usually run inside the screen for effective circulation of fluids.
The function of the gravel pack tool is to maintain hydrostatic pressure on the open-hole section of the well at all times to prevent bore hole collapse. Maintaining a hydrostatic over-balance throughout all operations and the use of proper fluid characteristics eliminates the need to run alternative flow path devices.
When running the gravel pack tool and the various screen assemblies in or out of the well bore, a screen table or support structure adaptively fixed to the rotary table located at the drill rig floor, is used to catch or capture the sand screen subsections of the tool assembly at each joint connection. The tubing string containing the screens is thus suspended within the well bore without damaging the screens or the gravel packer itself. The screen table is used to support the string in place of pipe slips because of the limited space at the joint between the screen subsections and to prevent damage to the screens. However, in some cases, slips are used in conjunction with the screen table to capture and suspend the wash pipe being inserted or withdrawn from within the screen string assembly.
Presently the screen and wash pipe connections are made up with conventional pipe wrenches or manual pipe tongs. However, recent requirements make it necessary to apply specified torques to these joints, thereby presenting a problem. Conventional power tongs having torque setting capability are simply too large due to space limitations and too expensive to downsize in most cases due to limited applications requirements.
Until recently hand tongs or pipe wrenches had no torque setting capability. Generally only the larger tongs and pipe spinner system have torque control and presetting capability. However, in some cases, torque indication systems have been employed whereby the tong or other such gripping tools are attached to a cable (cat line) that in turn is attached to a load cell. This arrangement requires significant time to set up and use and requires significantly more space than is generally available when working with sand screen replacement. Such systems are inherently inaccurate, dangerous, cumbersome, and lack efficiency.
A more unitized hand tong is available that utilizes a traditional torque setting handle integral with the tong as seen in U.S. Pat. No. 6,439,064. However, even this tool is too slow in some cases and requires a significant amount of labor, generally two men to manipulate the tong and a backup gripping tool in place and then apply the proper torque to each joint.
A more convenient and labor reducing assembly is obviously needed that allows for both a relatively small torque head and backup tong assembly. The tong assembly should remain in place adjacent the centerline of the well bore and be capable of swiftly coupling and uncoupling sand screens where space between the screen elements is minimal. It is equally important that the tong assembly be capable of coupling and uncoupling wash pipe being inserted within the sand screen string, also with preset torque capability. It would be advantageous for such an arrangement to utilize a manual tong assembly with shorter tong handles than are in current use and be confined to within the perimeter of the screen or rotary table and further reduce the manpower required to make up such connections. It is therefore an object of the following disclosure to provide such an apparatus.
SUMMARY OF THE INVENTION
A screen table and tong assembly whereby a sand screen table structure adaptable to a rotary table is used to capture and suspend sand screen subsections within the well bore is further adapted to include a pair of articulated opposing manual tong assemblies. The tong assemblies are pivotal and transversely positionable relative to the screen table. Provision is made for adapting a slip set in cooperation with said screen table and tong assembly for capturing and supporting wash pipe within the sand screen subsections. Additional adaptations include a custom spinner tong assembly for rotating the sand screen tubular subsections and wash pipe sections.
The tongs and their torque arm assemblies are interchangeable with a range of tong heads of different types and sizes including pipe wrenches, chain tongs, and strap wrenches and provide reversibility between left and right hand torque applications.
BRIEF DESCRIPTION OF THE DRAWINGS
For a further understanding of the nature and objects of the present invention, reference should be made to the following detailed description taken in conjunction with the accompanying drawings, in which, like parts are given like reference numerals, and wherein:
FIG. 1 is a frontal isometric view of the screen table and tong assembly;
FIG. 2 is a rear isometric view of the screen table and tong assembly;
FIG. 3 is a top view of the screen table and tong assembly with torque applicator extended;
FIG. 4 is a top view of the screen table and tong assembly with torque applicator retracted;
FIG. 5 is a partial elevation view of the screen table with tongs gripping the screen tool joints;
FIG. 6 is a partial isometric view of the torque and retaining tongs seen in FIG. 1;
FIG. 7 is an isometric exploded view of the tong and screen table assembly;
FIG. 8 is an isometric exploded view of the tong torque assembly;
FIG. 9 is an isometric exploded view of the retainer tong assembly;
FIG. 10 is an isometric view of the screen table assembly without tongs;
FIG. 11 is an isometric view of the screen table with retaining tong and screen coupling joint;
FIG. 12 is an isometric view of the screen table with both torque tong and retaining tong and screen coupling joint;
FIG. 13 is a partial isometric view of the screen table, retaining tong with spinner attachment; and
FIG. 14 is a side elevation view of the retaining tong with spinner attachment as shown in FIG. 13 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Looking first at FIG. 1 it can be seen that the screen table assembly 10 is composed of a screen table 12 attached to the rotary table 14 generally located on the floor 16 of an oil and gas well platform. Slips used for gripping and supporting the tubing string within the well bore when coupling and uncoupling the various sections of pipe, tubing or tool joints that make up the well's tubular string are not used when coupling and uncoupling sand screen subsections during packing operations. However, a set of slips 18 is required when inserting washout tubing 20 within the screen sections 22 being suspended within the well bore by the screen table 12 . The slip set 18 is supported by a slotted plate 24 , which is in turn supported by a slotted tubing collar 26 .
As seen in FIGS. 1 and 2, the screen table assembly 12 is fitted with a threaded vertical column 28 from which a pair of tong assemblies 30 , 32 is pivotally attached, one of the tong assemblies being a backup or retaining tong assembly 30 and the other being a hydraulic or gas actuated torque tong assembly 32 . Upon grippingly engaging the wash pipe 20 adjacent the pipe joint 33 , the torque tong assembly 32 is actuated, thus rotating the upper pipe and uncoupling the joint 34 as shown in FIG. 1 . Conversely, as seen in FIG. 2, retracting the torque arm assembly 32 tightens the joint 33 to a pre-set torque requirement.
Turning now to FIGS. 3 and 4 we see that the tong assemblies 30 , 32 work in close proximity to the screen table assembly 12 thus providing clear movement around the rotary table 14 and requiring no cables or long extension torque arms to be manipulated by rig personnel. Further, as seen In FIG. 3, the back up tong assembly 30 and the torque tong assembly 32 are positioned at 90 degrees to one another. When the torque tong assembly 32 is actuated and the pipe is rotated all pivotal motion is inboard as seen in FIG. 4, thereby reducing risk for personnel. It should also be noted that only one person may manipulate the arm easily.
Looking now at FIG. 5 we see that the tong assemblies 30 , 32 may also traverse the threaded vertical column 28 to a point slightly above the screen table assembly 12 . In FIG. 6 the tong assembly heads 34 and arms 36 may be replaced with larger ones, as seen in FIG. 5, to accommodate the sand screen collars by removing the pins 42 and the clips 76 in each of the tong assemblies as shown in FIG. 6 and better seen in FIG. 9 . The tong heads 34 may be any type of tubular griping apparatus including pipe wrenches, chain wrenches or strap wrenches as well as the tong heads shown.
As seen in FIG. 7, the tong assemblies 30 , 32 and their vertical, threaded, support column 28 may be easily removed from their support sockets 44 for transport. The vertical. threaded column 28 may be secured within the socket 44 at assembly or simply allowed to rotate therein. Rotating the vertical threaded column 28 while holding the tong assemblies 30 , 32 traverses the tong assemblies from a high to a lower position or vise-versa.
Looking now as FIG. 8 we see that the torque assembly 32 includes a mounting plate 50 attached perpendicularly to a threaded collar 52 and an actuator adaptor plate 54 mounted perpendicularly to the mounting plate 50 , and a pair of linear actuators 56 attached to the adaptor plate 54 in a manner whereby the rods 58 of the actuators are attached to a pivot head assembly 60 and are free to extend and retract the pivot head assembly 60 relative to the mounting plate 50 .
As seen in FIG. 9 the backup or retainer tong assembly 30 includes a pivot head assembly 60 attached to a box tube arm 62 , which is in turn attached to a threaded collar 64 . The pivot head 60 further includes a base clevis member 66 , a pivotal hub member 68 having a central pin bore 72 , and a perpendicular bore 74 is captured within the clevis member by removable flanges 70 attached externally to the base clevis member 66 . The tong head 34 and its arm 36 are rotatably connected to the pivotal hub member 68 by inserting the arm portion 36 through the perpendicular bore 74 and securing it with clip 76 . It should be noted that the tong head 34 may be reversed for opposite left or right hand rotation gripping by removing the pull pin 42 inserted in a perpendicular bore 78 located in the tong arm 36 . It should be noted that the tong arms 36 and heads 34 are interchangeable and easily exchanged by removing the pull pins 42 and the clips 76 .
Turning now to FIG. 10, we can see that down hole sand screens are connected as close as possible, leaving little or no room for gripping the tubular joint 80 without damaging the screens 21 , 22 . Therefore, as previously discussed, slip sets 18 are not applicable. Suspension of the screen string is therefore accomplished by utilizing what is known in the industry and previously referred to herein as a screen table assembly 12 , the table being placed directly over the well head and supported by the rotary table and rig floor partially encircles the tubular column extending into the well bore. When the screens 21 , 22 are being run in or out of the well bore, capture doors 82 as shown in FIG. 10 are positioned below the box end 85 of the tubular joint 80 . This allows the string to be held in suspension while the upper screen section 21 is added or removed from the lower screen section 22 . Simply sliding the doors 82 in or out within the channel 84 captures or releases the screen string.
Once the screen string has been captured by the screen table assembly 12 , as illustrated by FIG. 11, the backup or retaining tong assembly 30 is traversed into position along the threaded vertical column 28 to a position laterally adjacent the screen tubular joint 80 being captured and the tong head 34 is positioned around the joint to be coupled or uncoupled. Likewise, the torque arm tong assembly 32 is traversed into position along the vertical threaded column 28 , as seen in FIG. 12, to a point above the retainer tong assembly 30 and positioned for engagement with the screen section 21 , 22 to be coupled or uncoupled. The actuators 56 are then engaged, thus applying rotative torque to the joint.
In some cases it may be advantageous to spin the tubulars into place prior to applying the required torque. Therefore, a miniature spinner assembly with torque actuator 86 as shown in FIG. 13 may be provided in combination with the backup or retainer tong 30 . In this case the spinner assembly grips the upper tubing section of the joint 80 , as seen in FIG. 14, while the backup tong assembly 30 grips the lower tubular section. The spinner assembly 86 then rotates the upper section through several turns to engage or disengage the pipe threads comprising the joint 80 . When the spinner 86 has reached a predetermined torque, the linear actuator 89 provides the final predetermined torque to the joint 80 .
Because many varying and different embodiments may be made within the scope of the inventive concept herein taught, and because many modifications may be made in the embodiments herein detailed in accordance with the descriptive requirement of the law, it is to be understood that the details herein are to be interpreted as illustrative and not in any limiting sense. | A screen table and tong assembly whereby a sand screen table structure adaptable to a rotary table is used to capture and suspend sand screen subsections within the well bore is further adapted to include a pair of articulated opposing manual tong assemblies. The tong assemblies are pivotal and transversely positionable relative to the screen table. Provisions are made for adapting a slip set in cooperation with said screen table and tong assembly for capturing and supporting wash pipe within the sand screen subsections. Additional adaptations include a custom spinner tong assembly for rotating the sand screen tubular subsections and wash pipe sections. | 4 |
FIELD OF THE INVENTION
The invention relates to the field of aerial platform devices of the type used in construction and repair. In particular, the invention relates to a release assembly for pivotally releasing a worker's bucket on an aerial boom from an upright position to a dumping position.
BACKGROUND AND PRIOR ART
Aerial manlift devices commonly take the form of an interconnected series of one or more boom members supported on a vehicular platform. The boom members may be adjusted relative to one another, for example by a telescoping action, to various heights and angles relative to the vehicular platform to achieve access to a repair site. Alternatively, a single boom section may be raised or lowered to orient the outer end of the boom to the desired height and directional orientation.
A common attachment to an aerial manlift device is a walled platform comprising a worker's bucket which is affixed, for example by a support bracket, to the outermost end of the boom. An example of an arrangement wherein a worker's bucket is connected to the boom by a mounting bracket is shown in U.S. Pat. No. 3,295,633.
It is desirable in an aerial manlift arrangement including a worker's bucket to be able to pivotally release the worker's bucket to allow the bucket to fall from its upright position, under the influence of gravity, to a horizontal position without completely detaching the bucket from the mounting bracket structure. This feature is useful, for example, to empty water or debris which may have accumulated in the bucket, or more importantly, to assist in removing an injured worker in the event of an accident or an emergency. In prior art structures having a bucket release feature of this type, the structure utilizes a removable detent pin, whereby the bucket is held in upright position by the pin and is permitted to pivot to a horizontal orientation upon removal of the pin. An example of this type of bucket support arrangement is disclosed in U.S. Pat. No. 4,334,594. A significant drawback of a structure utilizing a removable detent pin is that any load or weight inside the worker's bucket tends to make the pin difficult to remove, and renders operation of the bucket release cumbersome when any substantial weight is present within the bucket.
SUMMARY OF THE INVENTION
It is an object of the invention to provide a novel bucket release assembly on an aerial manlift device which pivotally releases the worker's bucket from a vertical position to a horizontal position for emptying the contents therefrom.
It is a further object of the invention to provide a bucket release assembly on an aerial manlift device which is easily actuated even when the bucket contains a weight load.
The invention comprises a release assembly for pivotally releasing a worker's bucket affixed by a mounting bracket on an aerial boom from a vertical orientation to a horizontal orientation without detaching the bucket from the boom. The mounting bracket is pivotally attached to a retainer plate provided on the worker's bucket, and the pivotal connection allows the worker's bucket to move under the force of gravity from a vertical upright position to a horizontal dumping position. The bucket is maintained in its upright position by latch means comprising a rotatable plate provided inside the mounting bracket structure. The rotatable plate is provided with openings to engage protruding means, such as headed studs, provided on the bucket retainer plate. The rotatable plate includes lever means for rotating the plate between engaged and disengaged positions relative to the headed studs. In the disengaged position, the bucket is free to fall to its horizontal dumping orientation. The release assembly allows the bucket to be readily disengaged for pivotal movement without substantial hindrance by weight present inside the bucket.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a rear perspective view of a worker's bucket including a release assembly made in accordance with the invention, the worker's bucket being shown in its vertical orientation with the release assembly in its engaged position;
FIG. 2 is a fragmentary view of the worker's bucket of FIG. 1, the release assembly of the invention being shown in disengaged position, and the bucket shown moving towards a horizontal orientation;
FIG. 3 is a cut-away rear perspective view of the inner detail of the bucket release assembly of the invention;
FIG. 4 is a rear elevational view of the bucket release assembly of the invention;
FIG. 5 is a sectional view taken along line 5--5 of FIG. 4.
DETAILED DESCRIPTION OF THE INVENTION
In the preferred embodiment of the invention depicted in the drawings, wherein like reference numerals designate corresponding parts throughout the several views, a worker's bucket is designated generally at 10. The workers' bucket 10 is upwardly open to accommodate a worker, and is preferably formed of a dielectric material, for example reinforced plastic. On the rear side of the worker's bucket 10, an integral vertical channel 11 is formed by parallel wall protrusions 12. Secured rigidly inside the channel 11 is a retainer plate 13, which is secured in the channel 11 by bolts 14 extending through wall protrusions 12 into side flanges 13a provided on retainer plate 13.
Referring to FIGS. 1 and 2, a bucket-supporting mounting bracket 20 is mounted in a shaft 23 at the outer end of an aerial boom (not otherwise shown). The mounting bracket 20 generally comprises side plates 21, a rear wall 24 and lateral walls 22.
The mounting bracket 20 is mounted on the shaft 23 at the outer end of the aerial boom by a tubular weldment 25 held captive between lateral walls 22a and 22b. Weldment 25 is keyed to a piston rod (not shown) which extends from the cylinder 26 of a hydraulic rotation mechanism, up through the lower lateral wall 22a, through the tubular weldment 25, through the upper lateral wall 22b, and into a rotation control means 27. By activating the rotation control means 27, the worker's bucket may be rotated sideways under the power of the cylinder 26 relative to the shaft 23.
Mounting bracket 20 is pivotally connected to the retainer plate 13 by a pin 28 disposed on a horizontal pivotal axis, as shown in FIG. 3. As seen in FIGS. 1 and 2, the side plates 21 of the mounting bracket 20 taper downwardly to a point at their lower end. At the narrow portion 21a of side plates 21, holes are provided to receive pin 28. A tube 28a spans between the side plates 21 to provide a journal for the pin 28. Holes are also provided in side flanges 13a of the retainer plate 13 to accommodate pin 28. By this arrangement, the mounting bracket 20 is pivoted to the retainer plate 13 by the pin 28, and the bucket 10 is free to pivot under its own weight relative to the shaft 23.
In accordance with the invention, a novel quick-release assembly is provided to latch the retaining plate 13 in its upright position, as shown in FIGS. 1 and 3, and is quickly and easily operated to afford pivotal movement of the plate 13 to the dumping position shown in FIG. 2. Referring to FIG. 3, latch means in the form of a rotatable latch plate 30 is rotatably secured to the rear wall 24 of the mounting bracket 20 by a bolt 31. An operator in the form of a lever 32 is affixed to latch plate 30 for rotating it. The lever 32 includes an extension 32a defining a handle extending through and beyond the side plate 21 of mounting bracket 20 through a slot 21c. Accordingly, the lever 32 can be manipulated from a position outside the mounting bracket 20. Operating the lever 32 rotates the latch plate 30 on its mounting bolt 31 between clockwise and counterclockwise limit positions as determined by the extension 32a engaging the opposite ends of the slot 21c.
The latch plate 30 is provided with openings 33 therein. Openings 33 are key-hole shaped, each comprising a large round body portion 33a and a narrow tail portion 33b. As seen in FIG. 2, the retainer plate 13 on the worker's bucket is provided with protruding means in the form of headed studs 15 projecting therefrom. The heads of the studs 15 correspond in diameter to the body portions 33a of the openings 33 of the latch plate 30, and the shanks of the studs correspond in diameter to the width of the tail portions 33b. When the worker's bucket 10 is in upright position and the latch plate 30 is rotated to its counterclockwise limit position in which the body portions register with the studs, the headed studs are positioned in alignment with the body portions 33a of the openings 33 and retainer plate 13 is free to separate from mounting bracket 20. When the latch plate 30 is rotated to its clockwise limit position, the headed studs are engaged within tail portions 33b of openings 33 and movement of retainer plate 13 away from mounting bracket 20 is prevented. Tension spring 34 is attached between lever 32 and the inner face of mounting bracket side wall 21a, as shown in FIGS. 3 and 4, to bias the latch plate 30 toward the clockwise limit position.
In operation of the release assembly, the worker's bucket 10 is normally held in an engaged verticle orientation by retention of the headed studs 15 in the tail portions 33b of latch plate 30 (see FIGS. 3 and 4). By operating the lever 32 upwardly by the lifting extension 32a, the plate 30 is rotated counterclockwise until the headed studs 15 are aligned with body portions 33a of the holes. Upon such alignment, the bucket 10 is free to fall under the force of gravity away from the mounting bracket 20 about the pivot pin 28. To close the worker's bucket in its upright position, it is necessary only to lift the bucket into its vertical orientation, rotating the plate to its counterclockwise limit to register the body portion 33a with the studs, and allow plate 30 to return to its engaged position on the headed studs 15 by the spring force on lever extension 32a.
It will be apparent from the foregoing that release of the worker's bucket from its upright position in accordance with the invention is greatly facilitated over release using a pin arrangement. If the worker's bucket contains a heavy load, a pulling force on the operator lever is conveyed as rotational force to the rotatable latch plate. The user may exert considerable leverage using the operator lever in accordance with the invention. With such leverage exerted, it is a relatively simple to rotate the latch plate to disengage the worker's bucket. Such facilitated operation is desirable under normal working conditions and would be particularly useful in the event of an emergency.
In the preferred embodiment of the invention, certain additional features may be provided to enhance the operation of the release assembly. For example, a safety latch in the form of a detent pin 29 may be provided to penetrate openings 29a in side flange 13a and mounting bracket side plate 21, to prevent release of the bucket under the force of gravity when the release assembly is in its disengaged position. Preferably, the pin 29 is extended to engage in a housing 29b on the latch plate 30 to prevent inadvertent rotation of the latch plate. It is noted that the weight of the worker's bucket, when the release assembly is in the normal engaged position, is borne by the release assembly, and not by the detent pin 10. In this manner the detent pin 29 serves as a safety feature or backup system to prevent inadvertent rotation of the plate 30 to its counterclockwise limit position. Accordingly, any weight present in the bucket does not interfere with removing the detent pin when the plate is in its normal clockwise limit position.
In the preferred embodiment, a rub pad 40, which may be formed of plastic, hard rubber or a like material, is placed behind latch plate 30, to prevent excess wear thereof. The rub pad 40 is provided with openings (not shown) to allow passage of headed studs 15 therethrough. A stop chain 50 may be affixed between the mounting bracket 20 and the worker's bucket 10 to limit the fall of the worker's bucket 10 to a desired horizontal orientation.
While the invention has been described in terms of the preferred embodiment and best mode contemplated by the inventor, various modifications will be apparent to those skilled in the art, and the above description of the preferred embodiment is intended as illustration and not as limitation on the scope of the invention. | A release assembly for an aerial device for pivotally releasing a worker's bucket from an upright orientation to a horizontal orientation. The assembly consists of protrusions from the worker's bucket and a rotatable latch plate for selectively engaging and disengaging the protrusions. | 1 |
This is a division of application No. 123,316, filed Nov. 20, 1987, now U.S. Pat. No. 4,948,875.
FIELD OF THE INVENTION
The present invention relates to a novel polypeptide having an anti-tumor activity wherein the polypeptide is prepared by modifying the structure of a known anti-tumor polypeptide that causes serious adverse side effects by utilizing recombinant DNA technology to reduce the incidence of adverse effects, and a method of preparation of this novel anti-tumor polypeptide utilizing recombinant DNA technology. More particularly, the present invention relates to a derivative of human tumor necrosing factor [hereinafter abbreviated as h-TNF (N1)], wherein the 31st and 32nd arginine residues from the N-terminal of the amino acid sequence of h-TNF (N1) are replaced with asparagine residue (Asn) and threonine residue (Thr), respectively, [this novel derivative will be abbreviated as TNF (Asn) hereinafter]and a method of preparation of TNF (Asn), wherein a gene coding for TNF (Asn) is linked with a vector expressed in Escherichia coli, and by culturing the prokaryotic cells transformed by the vector, the TNF (Asn) is obtained
BACKGROUND OF THE INVENTION
Much has been expected from tumor necrosing factor (hereinafter abbreviated as TNF) since its discovery as an anti-tumor drug, because of its in vivo activity of causing hemorrhagic necrosis of various tumors without seriously affecting normal tissue cells, and also its in virgo activity of killing various tumor cells directly or inhibiting their growth. Pennica, et al [Nature 312, 724-728 (1984)] isolated cDNA of human TNF, determined the amino acid sequence of human TNF, and reported its expression in Escherichia coli [hereinafter, the polypeptide having an amino acid sequence of human TNF found by Pennica, et al. is abbreviated as h-TNF (N1)]. It is well known that similar reports were subsequently made by other groups. Now that it is possible to obtain a highly purified TNF standard substance by DNA recombinant technology, studies on the biological activities of TNF have been actively conducted. As a result, it has been revealed that TNF has, in addition to its known anti-tumor activity (tumoricidal activity and cytotoxic activity on hemangioendothelium), a wide variety of biological activities. Such biological activities include: 1) the activity of promoting growth of fibroblast cells; 2) the activation of leukocytes; 3) the activity of increasing the production of various cytokins (interleukin 1, interferon β 2 , colony-stimulating factor); 4) the activity of increasing the production of prostaglandin E 2 and collagenase; 5) the activity of increasing the production of various membrane proteins; 6) the activity of increasing the absorption of bone and cartilage; and 7) differentiation-inducing activity.
As described above, it has been revealed that TNF possesses a wide variety of biological activities. Recently, Cerami, et al. pointed out an important factor in the clinical application of TNF as an anti-tumor agent. That is, Cerami, et al. found that, in the process of studying cachectin which is a causative agent of cachectic effects observed in serious or chronic infections or in cancer patients, TNF and cachectin are in fact identical substances [Beutler, et al., Nature, 316, 552-554 (1985)]. This fact implies that if TNF per se is applied clinically as an anti-tumor agent, a serious adverse effect (cachectic effect) will accompany it. At present, therefore, the development of TNF derivatives which have reduced cachectic effect is highly desirable.
BRIEF EXPLANATION OF THE DRAWINGS
FIG. 1 shows the amino acid sequence of TNF (Asn) and a nucleotide sequence of DNA coding for it.
FIGS. 2-4 show the processes of various examples of plasmid preparation: FIG. 2 shows a method of preparation of M13mp19TNFRFDNA (RI/HindIII); FIG. 3 the same for M13mp19TNF (Asn) RF (RI/HindIII); and FIG. 4 the same for pIN5TNFST4 rop - (Asn) which expresses TNF (Asn).
FIG. 5 shows the lipoprotein lipase activity of h-TNF (N1) and TNF (Asn) (∘).
FIG. 6 shows the growth-inhibiting activity of h-TNF (N1) (A) and TNF (Asn) (B) on hemangioendothelial cells. In the figure, shows the growth pattern of hemangioendothelial cells in the absence of said TNF, ∘ and show the same in the presence of 1 ng/ml and 10 ng/ml of said TNF, respectively, and Δ shows the same in the presence of 5 μg/ml of monoclonal antibody (neutralizing antibody) against h-TNF (N1).
DETAILED DESCRIPTION OF THE INVENTION
The present inventors prepared various derivatives of h-TNF (N1) by means of recombinant DNA technology and concentrated therein efforts on finding a TNF derivative in which anti-tumor activity is retained while the cachectic effect is reduced. As a result, the present inventors have found a novel TNF derivative which has a lower cachectic effect while retaining a similar level of anti-tumor activity in comparison with h-TNF (N1), and thus completed the invention. In other words, the present inventors have found that a TNF derivative [hereinafter abbreviated as TNF (Asn)], in which the 31st and 32nd arginine residues (Arg) from the N-terminal of the amino acid sequence of h-TNF (N1) are replaced with asparagine residue (Asn) and threonine residue (Thr), respectively, has remarkably lower lipoprotein lipase inhibiting activity, which is a measure of the cachectic activity of TNF, than that of h-TNF (N1), while a level of cytotoxic activity on hemangioendothelium, which is supposed to be strongly related to anti-tumor activity, which is similar to that of h-TNF (N1) is retained, and thus completed the invention.
In the following, the present invention is illustrated further by examples and referential examples.
EXAMPLES
1. Preparation of a plasmid [pIN5TNFST4 rop - (Asn)] for production of TNF (Asn)
A plasmid for production of TNF (Asn) was prepared from the plasmid pBR322-PL-T4-hTNF expressing h-TNF (N1) (the Escherichia coli strain C600 in which said plasmid is introduced has been entrusted to The Culture Collection of Deutsch Sammlung von Mikroorganismen with the Accession No. DSM 3175) by the following method:
(A) Preparation of M13mp19TNFRF (RI/HindIII) (see FIG. 2)
3 μg of the plasmid pBR322-PL-T4-hTNF was digested completely with 10 Units (hereinafter abbreviated as U) of Aval and 10 U of HindIII, and DNA fragments containing most of the TNF gene were isolated. On the other hand, 3 μg of the plasmid pIN5T4 (the method for preparation of this plasmid is disclosed in detail in European Patent Application, disclosed on Mar. 20, 1985, with Disclosure No. 0134673A1) was partially digested with 10 U of EcoRI and 10 U of HindIII and DNA fragments of 3.8 kb were isolated. DNA fragments obtained by these two processes and 1 μg of chemically synthesized DNA linker, ##STR1## (Supplied from Applied Biosystem, 380A DNA synthesizer was used), which has ends cohesive to EcoRI and AvaI, respectively, were mixed and linked using 2 U of T4DNA ligase. Using the thus obtained reaction solution, the Escherichia coli strain W31l0 was transformed and the desired plasmid pIN5T4TNF was obtained. Next, after complete digestion of 3 μg of the plasmid pIN5T4TNF using 10 U of EcoRI and 10 U of HindIII, DNA fragments containing TNF gene were isolated. On the other hand, 3 μg of M13mp19RF was digested completely using 10 U of EcoRI and 10 U of HindIII, and DNA fragments of 7.2 kb were isolated. DNA fragments obtained by these two processes were mixed and ligated using T4DNA ligase, and by transfecting the ligated product into the Escherichia coli strain JM103, the desired M13mp19TNFRF (RI/HindIII) was obtained.
(B) Preparation of M13mp19TNF (Asn) RF (see FIG. 3)
One pmole of single stranded DNA of M13mp19TNFRF (RI/HindIII) and 10 pmole of chemically synthesized DNA ( 5' CTCCAGTGGCTGAACAACACGGCCAATGCCCTCC 3' ), whose 5' end was phosphorylated, were mixed and heated at 100° C. for 3 minutes, and then cooled down to room temperature over 2 hours for annealing. To this reaction solution, dNTP, DNA polymerase, ATP and T4DNA ligase were added and allowed to react, to make complete double-stranded cyclic DNA. The reaction solution thus obtained was used to transfect the DNA into the Escherichia coli strain JM103. Next, the desired clone was isolated and identified by plaque-hybridization according to the method of Benton, W. D. and Davis, R. W. [Science, 196, 180 (1977)]. Finally, DNA was isolated from the desired plaque and its nuclectide sequence was determined; thus M13mp19TNF (Asn) RF was obtained.
(C) Preparation of pIN5TNFST4 rop - (Asn) (see FIG. 4)
In order to prepare the plasmid pIN5TNFST4 rop - (Asn) expressing TNF (Asn), pIN5TNFST4 (Asn) plasmid was first prepared by combining the following four DNA fragments:
DNA fragment, 1: 3 μg of M13mp19TNF (Asn) RF was digested with 10 U of EcoRI and 10 U of BstEII and DNA fragments containing structural gene of TNF (Asn) of 400 bp long were isolated.
DNA fragment, 2: 5 μg of pT4TNFST8 rop - (the method for preparation of this plasmid is disclosed in Japanese Patent Application No. 217740/1985) was digested completely using 10 U of BstEII and 10 U of SalI, and DNA fragments of 90 bp long were isolated.
DNA fragment, 3: 3 μg of pBR322 was cleaved with 5 U of EcoRI, and linear DNA fragments were collected. Using T4DNA polymerase and dNTP, the EcoRI-cohesive end of the DNA fragments was turned into a non-cohesive end and the DNA fragments were collected by ethanol precipitation. To this DNA, 1 μg of SalI linker ##STR2## was added, and by using 1 U of T4DNA ligase, the reaction gave pBR322-SalI plasmid. Next, 3 μg of pBR322-SalI was digested completely with 10 U of SalI, and DNA fragments of 650 bp long were isolated.
DNA fragment, 4: pIN5T4 (described above) was digested with 10 U of EcoRI and 10 U of SalI, and DNA fragments of 2.1 kbp long containing 1 pp of promotor region were isolated. Four types of DNA fragments obtained above were linked together using T4DNA ligase, to give pIN5TNFST4 (Asn).
Next, a plasmid expressing TNF (Asn) very effectively, pIN5TNFST4 rop - (Asn), in which the rop (repressor of primer) region, deriving from pBR322 and controlling replication of pIN5TNFST4 (Asn) plasmid, was removed so that the number of plasmid copies could be increased, was prepared in the following way: 3μg pIN5TNFST4 (Asn) was cleaved with 10 U of Ball and 10 U of PvuII, and DNA fragments of 3.2 kbp long were isolated. After that, they were allowed to be cyclized. Using this reaction solution, the Escherichia coli strain W3110 was transformed, and DNAs were isolated from the clone which showed tetracycline resistance. Using a routine method, this DNA was analysed and the desired plasmid, in which BalI-PvuII DNA fragment of 600 bp long was removed from pIN5TNFST4 (Asn), pIN5TNFST4 rop - (Asn) was obtained.
2. Preparation of recombinant Escherichia coli strain
W3110/pIN5TNFST4 rop - (Asn) expressing TNF (Asn)
The desired recombinant Escherichia coli strain W3110/pIN5TNFST4 rop - (Asn), expressing TNF (Asn), was obtained by collecting tetracycline resistant clone after transforming the Escherichia coli strain W3110 by introduction of said pIN5TNFST4 rop - (Asn) plasmid.
The transformed Escherichia coli strain was named SBM287, and was deposited on Dec. 1, 1986 under the Budapest Treaty at the Fermentation Research Institute (one of the International Depositary Authorities) 1-3, Higashi-1chome yatabe-machitsukuba-gun Ibarabka-ken; with Accession No. FERM BP-1544.
3. Purification of TNF (Asn)
TNF (Asn) producing recombinant Escherichia coli [W3110/pIN5TNFST4 rop - (Asn)]was cultured in 800 ml of GC culture medium (2% glycerine, 3% casamino acid, 0.5% sodium dihydric phosphage, 0.2% yeast extract, 0.15 M sodium hydroxide, 0.1% MgSO 4 .7H 2 O, pH 6.5) in the presence of tetracycline (10 μg/ml) at 37° C. for 17 hours. Next, bacterial cells were collected by centrifugation and suspended in 10 mM Tris-HC buffer solution (pH 8.0). After that, the cells were disrupted with a French press under cooling, and the suspension was centrifuged at 8000 rpm for 20 minutes, 150 ml of supernatant being obtained. Using this crude extract solution, TNF (Asn) was purified in the following way: First, said crude extract solution was passed through DEAE Sephallose FF (Pharmacia, φ2.5×18 cm), a support for anion exchange chromatography equilibrated with 20 mM Tris-HCl buffer solution (pH 7.4), and after washing well with the same buffer solution, a solution containing a linear gradient of sodium chloride concentration from 0 M to 0.5 M was passed, and fractions eluted at around 0.15 M were collected; thus, the desired fractions containing TNF (Asn) were obtained. Next, ammonium sulfate was added to these fractions to give a solution 30% saturated with ammonium sulfate, and the solution was passed through Phenylsephallose 4B (Pharmacia, φ1.0×15 cm), a hydrophobic support for chromatography, equilibrated well with 20 mM Tris-HCI buffer solution (pH 7.4) containing 30%-saturated ammonium sulfate. After washing well with the same buffer solution, a solution containing a linear gradient of ammonium sulfate concentration (from 30% saturation to 0%) and ethylene glycol (from 0% to 50%) and the desired substance was eluted around 20%-saturated ammonium sulfate solution. After the obtained fractions were dialyzed well with 20 mM Tris-HCl buffer solution (pH 7.4), they were passed through S Sephallose FF (Pharmacia, φ1.0×15 cm), a support for cation exchange chromatography was equilibrated with the same solution, and after being washed well with the same solution, a solution containing a linear gradient of sodium chloride concentration from 0 M to 0.5 M was allowed to pass to have the desired substance [TNF (Asn)] eluted around 0.2 M sodium chloride. The TNF (Asn) standard substance obtained in this way shows a single band on SDS-PAGE, and the results of amino acid analysis were satisfactorily consistent with the theoretical values.
4. Biological activity of TNF (Asn)
The biological characteristics (lipoprotein lipase inhibiting activity and cytotoxic activity on hemangioendothelium) of TNF (Asn) obtained in Example 3 were compared with those of h-TNF (N1) as in the following: [h-TNF (N1) used here is TNF obtained from the transformed Escherichia coli strain W31l0/pT4TNFST8 rop - disclosed in Japanese Patent Application No. 295140/1985, by a method similar to the one described in Example 3].
(A) Lipoprotein lipase inhibiting activity
Lipoprotein lipase inhibiting activity which is an in vitro measure of cachectin effect was determined by the method described by Kawakami, et al. (Kawakami, et al., Proc. Nat. Acad. Sci. USA, 79, 912-916, 1982).
In other words, 3T3-L1 lipocyte precursor cells were cultured in a modified Dalbecco's Eagle (DME) medium containing 10% fetal bovine serum (FBS) until the cells were in a confluent state. The cells were cultured for another two days, and then further cultured in the DME medium containing 10% FBS, 10 μg/ml of bovine insulin, 0.5 mM of methylisobuthylxanthine and 1.0 μM of dexamethasone for 48 hours. After that, the cells were cultured in DME medium containing 50 ng/ml of bovine insulin for 4 days. After these cells were cultured in DME medium containing 10% FBS for 20 hours in the presence of h-TNF (N1) or TNF (Asn), the culture solution was discarded and 10 U/ml of heparin-containing DME medium was added. The cells were then cultured for 1 hour. In this way, lipoprotein lipase bound to the membrane was released in the culture supernatant. To 75 μl of this supernatant, 25 μl of 200 mM Tris-HCI buffer solution (pH 8.1) containing 22.6 mM of tritium-labelled triolein, 2.5 mg/ml of lecithin, 40 mg/ml of bovine serum albumine, 33% (v/v) of rat normal serum and 33% (v/v) of glycerol was added and the mixture was allowed to react at 37° C. for 30 minutes. The amount of fatty acid released was then determined. The results showed that, as shown in FIG. 5, TNF (Asn) has a clearly lower lipoprotein lipase inhibiting activity than that of h-TNF (N1). [When comparison is made with the IC 75 , the lipoprotein lipase inhibiting activity of TNF (Asn) is not more than 1/100 ff the same of h-TNF (N1).] "IC" is an abbreviation of Inhibition Concentration, and IC 75 denotes the concentration at which 75% of the growth is inhibited.
(B) Cytotoxic activity on hemangioendothelium
The cytotoxic activity on hemangioendothelium was determined by the activity of inhibiting the growth of bovine hemangioendothelial cells [prepared by the method of Sato, et al., Journal of National Cancer Institute (JNCI), 76, 1113-1121 (1986)].
Specifically, these endothelial cells were placed in a 96-well microplate so that each well contained 8,000 cells, and cultured in Eagle MEM medium containing 10% fetal bovine serum in the presence of h-TNF (N1) and TNF (Asn). Next, each cell was fixed in 10% formaline for 15 minutes, and dyed with 0.05% naphthol blue black for 30 minutes. After washing the plate well with water and drying it, the dye was extracted with 50 mM of sodium hydroxide, and absorbance at 630 nm was determined. The results showed that, as shown in FIG. 6, the cytotoxicity of TNF (Asn) on hemangioendothelium is equivalent to that of h-TNF (N1).
The results of studies on biological activities showed that the polypeptide of the present invention, TNF (Asn), is a TNF derivative very useful as a drug, which has a potent anti-tumor activity without being accompanying by any serious adverse effects (cachectic effects). | Disclosed is a human TNF derivative with a reduced tendency to cause adverse side effects that is obtained by replacing the 31st and 32nd arginine residues from the N-terminal of the amino acid sequence of human TNF, which has a potential for causing serious adverse effects, with asparagine residue and threoine residue, respectively, as well as a method of preparing the same utilizing recombinant DNA technology. | 2 |
BACKGROUND
[0001] 1. Field of the Invention
[0002] The present invention generally relates to data evaluation systems and methods. More particularly, the invention relates to financial systems and methods that use an encapsulated engine to perform evaluation and calculation of data sets.
[0003] 2. Background Information
[0004] Financial environments have become increasingly complex. Developers of computer systems and programs for these environments need to take into consideration an array of different factors and issues. As a result, any newly developed system or program, that aims at effectively dealing with the challenges of the financial sector, is typically developed on a case-by-case basis, and is limited to the specific application for which it was developed.
[0005] In recent years, programmers have devoted considerable effort to developing programs that are somewhat adaptable to different situations, so as to reduce the need to create and reprogram source code. Accordingly, such engines, although perhaps providing significant adaptability, are still application-specific engines and would require substantial code revision to be re-used in other applications.
[0006] The specific business environments for which the financial programs are developed are as varied as the companies and industries in which they exist. The differences include, for example, country-related factors and industry-related factors.
[0007] The country-related factors include various legal environments, for example, different tax laws; or different accounting methods, for example, the “declining balance method” used in Japan and Korea or the depreciation on the group asset level used in the USA.
[0008] Industry-related factors relate to the way assets are accounted for in different industries and the available business records. Often, the usage of accounting information may be provided in an industry standard or proprietary format. Accordingly, accounting, as well as, financial programs are generally designed on a case-by-case basis to handle particular types of data and specific data structures.
[0009] In order to deal with multiple factors, ready-made financial programs are usually inadequate and companies decide to custom-design programs for particular applications so as to support, for example, externally-defined data according to client-defined rules. However, the process of developing custom code on a per application basis is expensive, disruptive to the company's business, and unreliable. Significant company resources are often devoted to educating the developers, providing test data, analysing the test results and troubleshooting the program. In addition, due to the complexity of developing custom code from basic principles, the resulting programs are prone to errors or inadequate performance and may take significant time to develop into satisfactory products.
SUMMARY OF THE INVENTION
[0010] Embodiments consistent with the present invention may address one or more of the above-noted problems. For example, systems and methods consistent with the invention may address the need for flexible and reliable financial calculation/evaluation systems. Such systems and methods may support, among other things, externally defined data structures of various business environments and data handling according to client-defined rules. Moreover, systems and methods consistent with the invention may utilize an encapsulated calculation/evaluation engine that works independently of application-specific data structures. Thus, development time frames may be substantially reduced with corresponding cost savings. Further, system reliability may be enhanced, due to the ability to reuse the generalized platform.
[0011] According to one embodiment, a system and method are provided for processing data sets. The data sets may comprise financial data, and each data set may include at least a posting date and be indicative of a financial evaluation rule. As disclosed herein, the data sets may be received from an external application database. Further, the data sets may be sorted by posting date to provide an ordered sequence of data sets.
[0012] In the exemplary system and method, an initial segment covering a time span from the posting date of the initial data set of the sequence to the end date may be created. Thereafter, an ordered sequence of data sets may be processed by the engine, adding a consecutive data set of the sequence to the initial segment if the consecutive data set has the same posting date and financial evaluation rule as the first data set or, otherwise, splitting the initial segment into first and second segments. Loop processing of further consecutive data sets of the ordered sequence may follow, wherein adding occurs when a consecutive data set matches an initial data set.
[0013] In case the posting date of the consecutive data set is not the same as the first data set, splitting of the initial segment into first and second segments may occur. The first segment may cover a time span between an initial posting and a consecutive posting date, and the second segment may cover a time span between the consecutive posting date and an end date. Additionally, or alternatively, splitting may occur in case the posting date of the consecutive data set is the same, but the consecutive data set comprises different a financial evaluation rule.
[0014] It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only, and should not be considered restrictive of the scope of the invention, as described and claimed. Further, features and/or variations may be provided in addition to those set forth herein. For example, embodiments of the invention may be directed to various combinations and sub-combinations of the features described in the detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] The accompanying drawings, which are incorporated in and constitute a part of this disclosure, illustrate various embodiments and aspects consistent with the present invention. In the drawings:
[0016] FIG. 1 is a block diagram illustrating an exemplary data evaluation system for processing data sets with financial data, consistent with an embodiment of the present invention;
[0017] FIG. 2 is a flowchart of an exemplary process for performing financial data evaluation, consistent with an embodiment of the present invention;
[0018] FIG. 3 is a flowchart of another exemplary process for performing financial data evaluation; and
[0019] FIG. 4 is a block diagram of another exemplary data evaluation system for processing of data sets with financial data, consistent with an embodiment of the present invention.
DETAILED DESCRIPTION
[0020] The following detailed description of embodiments of the present invention refers to the accompanying drawings. Where appropriate, the same reference numbers in different drawings refer to the same or similar elements.
[0021] Embodiments consistent with the present invention are applicable to many different industries. Further, from this disclosure, one skilled in the art will appreciate that the various embodiments and concepts of the invention are applicable to plurality of industries without straying from the spirit and scope of the invention.
[0022] FIG. 1 illustrates an exemplary data calculation/evaluation system 100 for processing of data sets 116 comprising financial data, consistent with an embodiment of the present invention. Each data set may include a posting date and be indicative of a financial evaluation rule. The data sets may be transferred to data calculation/evaluation system 100 for processing via an interface 110 from an external application database 114 of a data source 112 .
[0023] According to one embodiment of the invention, data sets comprising financial data can originate from an investment database 118 , if future investments need to be evaluated and planned, and/or the data sets may come from an asset accounting module 120 , if the initial request includes calculation of such values as, for example, depreciation, interest or revaluation. When providing the data sets, a user may specify an evaluation period by entering an end date.
[0024] An externally-defined data structure of the data set may be mapped onto the internal data structure and the transformation of application-specific data structure into the flat, generic data structure may take place. Subsequently, evaluation system 100 may determine the start and the end period as requested by the user and accordingly an initial segment covering a time span from the posting date of the initial data set of the sequence to the end date is created.
[0025] Next, data sets 104 may be sorted by posting date to provide an ordered sequence of data sets that is then processed by evaluation engine 108 . At this point, a consecutive data set of the sequence may be added to the initial segment if the consecutive data set has the same posting date and financial evaluation rule as the first data set. Otherwise, the initial segment may be split into first and second segments. Creation of segments, determination of appropriate segment(s), and splitting or updating of segments may take place in segmentation module 106 . Further, calculation of the requested amounts with the use of the implemented algorithm may be performed by calculation module 102 .
[0026] FIG. 2 illustrates a flow chart of an exemplary process for performing financial data evaluation, consistent with an embodiment of the invention. The exemplary method of FIG. 2 may be implemented using, for example, the system of FIG. 1 .
[0027] In step 200 , data sets comprising financial data, each data set having at least a posting date and each data set being indicative of a financial evaluation rule, are received from an external application database. In step 202 , the user enters an end date to set the evaluation period. Next, in step 204 , an external application-specific data structure of the data set is mapped onto the internal structure and the structure is transformed.
[0028] Subsequently, as shown in FIG. 2 , the creation and determination of segments follows. Specifically, in step 206 , the posting dates representative of changes are identified and the evaluation engine determines how those changes relate to the initial segment. In step 208 , calculations according to financial evaluation rules are performed. Then, the structure of the data sets is transformed back into the original, application-specific structure (step 210 ) and, finally, the data sets are send back to the application (step 212 ).
[0029] FIG. 3 illustrates a more detailed flowchart of another exemplary process for evaluating financial data, consistent with an embodiment of the present invention. Step 300 permits flexible determining of evaluation period by entering of an end date by the user. In step 302 , data sets are ordered by the posting date into the ordered sequence D 1 , D 2 , . . . Di, where i is initially set to one (step 304 ). In step 306 , initialisation takes place. This may include creating an initial segment covering time span from the posting date (D 1 ) to end date with the assigned evaluation rule. In the following step (step 308 ), incrementing or loop processing of the data sets may be performed.
[0030] Each time the evaluation is performed and the decision is made (step 310 ), if data set Di matches an existing segments, then the consecutive data set is added to the existing segment (step 312 ). However, in case the consecutive data set does not match an existing segment, then the existing segments covering the posting date Di are determined (step 314 ) from the perspective of posting date representing the change and from the perspective of matching financial evaluation rules. If the data set Di does not fit the previous segment, then it may be split into the two consecutive segments (step 316 ). Also, if the posting date representing the change does fit the initial segment and the financial evaluation rules are different, then the previous segment may be split into the two new segments as well (step 316 ). Finally, if the change fits the initial segment, the data set is added to newly created segment (step 318 ).
[0031] FIG. 4 illustrates another exemplary data evaluation system, consistent with an embodiment of the invention. In FIG. 4 , data sets 416 are received from an external application database 414 of a data source 412 . The data sets may be received from an investment database 418 , if future investments need to be evaluated and planned, and/or from an asset accounting database 420 , if the initial request includes calculation of such values as, for example, depreciation, interest or revaluation (inflation). As shown in FIG. 4 , the data sets may be received via an application interface 426 .
[0032] The received data sets may comprise financial data, and each data set may include at least a posting date and be indicative of a financial evaluation rule. Further, the data sets coming from external applications may have an application-specific data structure, since calculation/evaluation system 400 of the shown embodiment works with a generic, flat data structure. The externally-defined data structure of the data set may be mapped onto the internal data structure of a data set 404 and data set 416 may be transformed using an internal interface 410 . In one embodiment, the transformation takes place in the main memory 413 . Further, the data set 404 may have an application-independent data structure, and also have at least a posting date and be indicative of a financial evaluation rule.
[0033] The set of financial rules used by the calculation/evaluation system may comprise validation rules 409 , 432 , calculation rules 407 , 430 and/or definitions of periods 411 , 434 . The set of rules used in the present invention may be partially client-defined, such as external validation rules 432 , calculation rules 430 , and/or specific periods 434 . Also, the set of rules may comprise internal rules, such as validation rules 409 , calculation rules 407 and/or period definitions 411 .
[0034] Validation rules 409 allow for the validating of data against master files or tables. For example, it may first be determined whether the received value(s) should be checked. Then, the received data may be checked using Boolean logic. Examples include: specification of the maximum possible depreciation; use of constrains including the use of the negative values, etc.
[0035] By way of example, calculation rules 407 may include a determination of the base value for the considered period where it is specified if the calculation has to be of the type arithmetic, geometric or similar, as well as a calculation factor where the type of the calculation method is taken into consideration, including for example: linear, stated percentage, declining, country specific, customer specific or other.
[0036] Period determination through the use of the period factor may also be performed by the evaluation engine 408 . It needs to be determined in this case if the user needs the calculation to be done on the basis of days, weeks or months, or if some other standard needs to be used, for example 13 periods for a fiscal year. Also, period weighting can be used, where for example, an additional weight can be added if the multiple-shifts were used in a specific period.
[0037] Subsequently, evaluation system 400 may determine the start and the end period as requested by the user and, accordingly, create an initial segment covering a time span from the posting date of the initial data set of the sequence to the end date. Next, data sets 404 may be sorted by posting date to provide an ordered sequence of data sets. An ordered sequence of data sets may then be processed by the evaluation engine 408 , adding a consecutive data set of the sequence to the initial segment if the consecutive data set has the same posting date and financial evaluation rule as the first data set. Otherwise, a splitting of the initial segment into first and second segments may be performed. The creating of segments, determining of the appropriate segment, and the splitting or updating of segments may take place in segmentation module 406 .
[0038] Before a calculation can be performed, it needs to be determined which master data 422 and which configuration data 428 is required for the calculation. When the evaluation engine has the necessary data and the financial rules, calculation module 402 may perform a computation using the following formula: amount=period factor*base value*calculation factor. The process of computing continues until the ordered sequence is not empty by looping at the determined periods. The results of the calculations are stored in memory 413 as data 415 or in the form of tables 417 . Then, they are returned to the application after transforming back the generic data structure of the data sets back into the application-specific data structure. The results are stored in application memory 424 unless the user specifies that the results should be stored permanently.
[0039] To provide a further understanding of the scope of the invention, the following example is provided for asset accounting:
[0040] According to an implemented algorithm of the calculation/evaluation program, the required amount is not calculated for each change separately. Instead, the amount is calculated by taking into account all changes, which are relevant for the considered time period.
[0041] There may be two changes on a fixed asset: an acquisition of 100,000 on the 1.01.2003, and a transfer of 20,000 on the 01.07.2003. The depreciation amount is calculated as, for example, 10% of the acquisition and production costs per year. Also assume that one period is equal to one calendar month.
[0042] In the first step, the depreciation amount is calculated for the first six months, taking into account the acquisition in the period one (1):
[0000] 100,000*10%*6/12=−5,000
[0043] In the next step, the amount will be calculated for the last six months, taking into account both the acquisition and the transfer:
[0000] (100,000+20,000)*10%*6/12=−6,000
[0044] The total depreciation amount is then computed as the sum:
[0000] −5,000+−6,000=−11,000
[0045] In the current program, the depreciation amount on the first acquisition is calculated for the 12 months:
[0000] 100,000*10%*12/12=−10,000
[0046] Depreciation amount on the transfer is calculated for the last 6 months:
[0000] 20,000*10%*6/12=−1,000
[0047] The total depreciation amount is the sum:
[0000] −10,000+−1,000=−11,000
[0048] Further, the application-independent data structure may be flat to allow the calculations to be performed quickly and very precisely, for example:
[0000]
Dura-
Depre-
No.
Start
Value
tion
Percentage
End
ciation
1
01.01.2003
100,000
10
10%
30.06.2003
−5,000
2
01.07.2003
20,000
10
10%
31.12.2003
−6,000
[0049] After the calculations are performed, the structure of the data sets is transformed back into the original, application-specific structure and the results are not stored in the database but they are sent back to the application as an accumulated result.
[0050] The foregoing description has been presented for purposes of illustration. It is not exhaustive and does not limit the invention to the precise forms or embodiments disclosed. Modifications and adaptations of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the disclosed embodiments of the invention. For example, the described implementations include software, but systems and methods consistent with the present invention may be implemented as a combination of hardware and software or in hardware alone. Additionally, although aspects of the invention are described for being stored in memory, one skilled in the art will appreciate that these aspects can also be stored on other types of computer-readable media, such as secondary storage devices, for example, hard disks, floppy disks, or CD-ROM, the Internet or other propagation medium, or other forms of RAM or ROM.
[0051] Computer programs based on the written description and flow charts of this invention are within the skill of an experienced developer. The various programs or program modules can be created using any of the techniques known to one skilled in the art or can be designed in connection with existing software. For example, programs or program modules can be designed in or by means of Java, C++, HTML, XML, or HTML with included Java applets or in SAP R/3 or ABAP. One or more of such modules can be integrated in existing e-mail or browser software.
[0052] Moreover, while illustrative embodiments of the invention have been described herein, the scope of the invention includes any and all embodiments having equivalent elements, modifications, omissions, combinations (e.g., of aspects across various embodiments), adaptations and/or alterations as would be appreciated by those in the art based on the present disclosure. The limitations in the claims are to be interpreted broadly based on the language employed in the claims and not limited to examples described in the present specification or during the prosecution of the application, which examples are to be construed as non-exclusive.
[0053] Accordingly, other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. It is therefore intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims. | Systems and methods are provided for evaluating financial information, including systems and methods with computational/evaluation capability to process data sets comprising financial data. In one of the implementations, the systems and methods may be utilized for asset accounting. A calculation module may be provided that includes an evaluation engine that operates internally on a flat, generic data structure that is independent of the particular application. The externally-defined data structure of the data set may be mapped onto the internal data structure. Further, rules-based modules may provide information related to the client-defined rules. A user interface may enable a user to receive back the evaluated financial information, for a specified time period, the financial information being responsive to an original user request entered via the user interface. As a result, the evaluation engine can be used for a variety of different applications. | 6 |
BACKGROUND OF THE INVENTION
[0001] U.S. Pat. Nos. 6,082,944 and 6,015,062, assigned to the assignee of this application, disclose closure constructions for reclosable containers (e.g a can body) wherein a domed container end with a neck portion having a pour opening is provided with a reclosable lugged type of cap. That invention provides a unique and versatile container for fluids, particularly for beverages, wherein various standard can bodies are provided with a two part end including a neck with a pour opening, a lug formation on the neck below the pour opening, a reclosable cap having a lug formation which can interlock with the lug formation on the neck and including a seal surrounding the pour opening, and thus capable of maintaining product under pressure. The two part end is affixed to a can body by conventional double rolled seam attachment between the bottom of the neck and the rim of the can body. However, it is possible to affix the domed end to a can body without a cap, fill the can though the pour opening, and then apply the cap.
[0002] With the possibility of expanded markets for these lugged caps, which are also useful on various jars and bottles, there is a need for a system (method and tooling) for producing lugged cap members in a single machine, e.g. a reciprocating press fitted with appropriate tooling, which is capable of precise high speed (e.g. in the range of 135 to 150 strokes/minute) to achieve acceptable commercial production of the cap.
[0003] To develop such production speeds it is desirable to divide the progressive tooling operations into more than one step, and this in turn requires a rapid and precise transfer system to move the partially completed caps from a first station to a second station, and precisely register the caps in the second station. Prior art transfer systems are known for moving and registering can end shells, such as in U.S. Pat. Nos. 4,770,022 and 4,895,012, however, the end shells are relatively flat disc-like objects with a quite small height to diameter ratio, whereas the caps made by the present invention have a substantially greater height with respect to their diameter.
[0004] Thus, the physical dimensions of the caps involved in this invention are quite different from can shells or easy self-opening can ends. This in turn introduces needs not required or anticipated in shell transfer systems, for example with regard to tipping of the caps during high speed transfer operations. Also, because of the relatively high press cycling, and need for precision in cap positioning and deceleration immediately after each transfer to another press station, there is a requirement for precise transfer of each cap from a first press station through high acceleration, very rapid transfer to the next press station, and high deceleration to a precisely defined stationary location at that next station.
SUMMARY OF THE INVENTION
[0005] The present invention provides a transfer apparatus and method for a first to a second station of progressive tooling in a cap making press. The caps are of a type having substantial height with respect to their diameter. Thus a first station punch and die form a cap of generally inverted cup shape, with an outward curled rim, and a second station punch and die form lugs into that rim, requiring just two strokes of the press to sever a disc from a supply sheet, form it, and discharge a completed cap.
[0006] Thus, in the first station, a cap is formed except for lugs which are added to the cap in the second station. The formed cap in the first station, which is in the nature of an inverted cup, has an outward curl formed on its lower edge during the initial up stoke of the press. This cup is then biased against the upper forming punch, by a first airstream introduced into the cavity within the underside of the cap, and moves upward in contact with the first station punch. As the punch approaches its top dead center location (tooling fully open), a second airstream begins, before the first station punch is fully raised and while the first airstream is still on. This second airstream moves the cap off the raised first station punch, and into and through a transfer chute directed toward the second station.
[0007] At the second station, the cap departs the chute and passes detents on a pair of closed retention fingers which, with the tooling open, define an extension of the transfer path from the chute into the open second station tools. As the second station tools begin to close and the partially finished cap is located, the fingers are opened and the tooling operates to form lugs into the cap rim.
[0008] As the second station tooling opens, a vacuum applied to a port in the second station punch begins to hold the finished cup against that punch tool, and when that punch clears the closing fingers and approaches its top dead center location, an ejection airstream commences to propel the finished cup from the tooling via a discharge chute.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is a bottom view of a container cap as provided by the invention.
[0010] FIG. 2 is a transverse cross-sectional view of a typical completed cap, as shown in FIG. 1 .
[0011] FIG. 3 is an over all perspective view of the tooling for a four-out cap making system.
[0012] FIG. 4 is an enlarged perspective view, with the die shoe removed, showing details of the tooling, including four first station tools in the center and four related second station tools outwardly in opposite directions of the first stations.
[0013] FIG. 5 is a further enlarged perspective view showing details of one pair of first and second stations of the tooling.
[0014] FIG. 6 is a cross-section view of a first station punch or upper tool.
[0015] FIG. 7 is a cross-section view of a first station die or lower tool.
[0016] FIG. 8 is a cross-section view illustrating the first station punch and die in closed position, and showing a cap formed except for an outward curl at the lower rim of the cap.
[0017] FIG. 9 is a cross-section view showing first station and corresponding second station tools, a transfer chute between them, the fingers which provide an extension of the chute into the second stage tool, and cams which control movement of the fingers.
[0018] FIGS. 10 and 11 are detail views of the top of the second station die, showing the open and closed positions of the fingers.
[0019] FIG. 12 is an enlarged cross-section view of the second station tools, and FIG. 12A is a further enlargement of the circled area in the center of FIG. 12 .
[0020] FIGS. 13 A and 13 B 1 & 13 B 2 (three sheets) together are a schematic diagram of the pneumatic supply & control system of the press and tooling.
[0021] FIG. 14 is a flow diagram of the electronic control system for the tooling package.
DESCRIPTION OF PREFERRED EMBODIMENT
[0022] The present invention provides a transfer apparatus and method for two station progressive tooling in a cap making press and system. The caps are of a type having substantial height with respect to their diameter. A typical such cap is shown in FIGS. 1 and 2 , which is also shown in FIGS. 2, 4A and 4B of U.S. Pat. No. 6,015,062. The preferably integral cap 11 , in the general form of an inverted cup, includes a top panel 12 , a peripheral sidewall 13 , and a curled rim 14 .
[0023] In the present drawings, FIGS. 3-12A depict multi-lane progressive tooling comprising four lanes for simultaneously forming four caps 11 , each lane comprising pairs of first and second tooling stations 15 A, 15 B, 16 A, 16 B, 17 A, 17 B, and 18 A, 18 B, with the first stations 15 A- 18 A arranged centrally of the tooling ( FIGS. 3, 4 & 5 ) and corresponding second stations 16 A- 16 B arranged outward of the first stations toward opposite sides of the upper and lower die plates 20 A, 20 B which support the upper (punch) and lower (die) tooling, and mount between the bed and slide of a reciprocating press (not shown).
[0024] Except for their orientation in the overall tooling package, the respective first station and second station tools are alike, and the following detailed description applies to all. Taking stations 15 A and 15 B as examples, each pair of corresponding first and second stations has an associated transfer chute 19 ( FIGS. 4, 5 & 9 ) between them, and each second station has a discharge chute 19 A, the four of which are directed out opposite sides of the tooling ( FIGS. 3 & 4 ).
[0025] Sheets of metal, with an appropriate pattern of lithographed materials for each cap, are fed centrally into the first stations by sheet feeding mechanism of known construction (not shown) which moves the sheets one at a time in step wise fashion, synchronized to the press strokes, along the feed path indicated by arrow IN in FIGS. 3 & 4 .
[0000] First Station
[0026] The first station tools comprise an upper or blank punch tool 45 and a compound lower die. During the initial operation of the first station tools, with the lithographed patterns aligned with respect to the first station tools, a blank is cut from the material (typically aluminum or thin cold rolled steel) on the down stroke of the press by blank punch 45 . On the continuation of the down stroke, the blank punch and lower die tool cooperate such that the blank is drawn into a cup shaped cap part 11 P ( FIG. 8 ). At the bottom of the stroke the panel shape 12 is formed into the top of cap part lip by the punch 45 and cooperating die 46 ( FIGS. 6, 7 & 8 ).
[0027] On the up stroke, the lower curl ring 48 , which is under spring pressure, raises with the blank punch. The bottom edge of the cap part 11 P is curled outward into the cavity 49 formed by curl ring 48 and blank punch 45 , completing a formed cap 11 with an outward curled rim 15 .
[0028] The formed cap in the first station, which is in the nature of an inverted cup, is biased against the upper forming die by a first airstream introduced through passage 50 (see FIGS. 8 & 9 ) into the cap as the first station tooling opens, and causes the cap to follow upward against the bottom of the punch 45 . During the upward travel of the cap, a second airstream is initiated through a nozzle 52 directed across the upper fist station tooling toward chute 18 , and is at its full power when punch 45 (with a cap 11 held thereto by the upward directed first airstream) traverses the space between nozzle 52 and the entry 18 E to chute 18 (see FIG. 9 ). By the time the first station tooling reaches full open at the top-dead-center of a press stroke, the cap has actually been transferred into the second station 15 B; see the Press Rotation timing chart below (page 8).
[0029] Thus, the first and second airstreams, appropriately switched on and off, together with the associated chute, constitute a first part of an essentially passive press transfer system.
[0000] Second Station
[0030] At the second station, a separated pair of fingers 60 reach around the sides of the second station tooling ( FIGS. 9, 10 & 11 ), defining partial sides of a receiving space 62 when the second station tooling is open, and an extension of the transfer chute when closed. The fingers are supported by pivots 63 inward of their rear ends 61 , and are biased into their closed position ( FIG. 10 , forward ends parallel) by spring mechanism 64 . Each finger has a narrow ledge-like track 65 extending part way along its forward upper edge ( FIGS. 10-12 ), facing each other and ending in a curved section 66 . Extending horizontally inward over tracks 65 are spring-loaded ball detents 67 which, together with the curved track sections 66 , define the termination of the transfer path for the incoming caps.
[0031] A cap propelled from the first station traverses the adjacent transfer chute 19 and enters receiving space 62 , passing across ball detents 67 and resting against the curved track sections 66 (see FIG. 11 ). The fingers and their operating mechanism form the remainder of the unique transfer system.
[0032] As the tooling proceeds to close during the beginning of a next stroke, fingers 60 are swung outward by descending cams 48 pressing against followers 49 on the rear ends 61 of the fingers to move the followers 49 inward and the forward section of the fingers outward ( FIGS. 10 & 12 ) before the second station tools close. The elongated cams 48 are mounted on the upper (die) tooling base ( FIG. 12 ), and this action centers a cap ( FIG. 11 ) and then opens the fingers associated with the second station tooling, before that tooling closes to form lugs on rim 15 of a cap 11 . This closing action of fingers 60 is momentary, and they are then opened substantially before the second station tooling closes; see Press Rotation timing chart below.
[0033] In the second station 15 B in the press, the tooling includes an upper punch 70 and a lower die 72 . The punch tool 70 includes an annular knock out ring 71 with an inner shape conforming to a cap exterior, and a headed knock out pin 73 which is spring loaded toward a position flush with the lower edge of ring 71 ( FIGS. 12 & 12A ) when the tooling is opened. In the lower die 72 there is a vertically extending tapered cam 74 mounted onto a base plate 75 and surrounded by a plurality of die pins 76 also mounted onto plate 75 . The cam 74 and pins 76 project through a vertically movable, upwardly biased ring 78 which contains a plurality of lug forming dies 80 , equal in number to pins 76 and movable laterally outward through forces from cam 74 as it is made to enter ring 78 . The top of ring 78 has an upper surface 82 contoured to fit within a cap 11 .
[0034] Thus, when the second station tooling closes a cap is positioned with the curled rim 15 between the upper ends of pins 76 and the radially outward moving forming dies 80 , to for the predetermined number of lugs in the rim ( FIG. 1 ). Then, the completed cap is held to the knockout pin by means of a vacuum created in passage 85 though the head of that pin 73 , such that the cap is carried upward past an air nozzle 87 directed across the path of the rising upper tool toward an associated discharge chute 19 A. The vacuum is created by air flow through a small venturi (not shown) so the vacuum is relieved immediately upon cessation of air flow through that venturi. A discharge air stream is started from nozzle 87 and moves the cap from the upper knock out ring and pin, into and through the associated discharge chute 19 .
[0000] Press Rotation Relation to Tooling Function
[0035] 1st Station
0° Top of the Stroke; Top Dead Center 140° Material is Blanked 180° Form & draw complete; Bottom Dead Center; Cap Overall Height ˜0.810 inch 190° Cap Curl complete; Overall Height is ˜0.625 inch 190° 1st Air turned on; Blows cap against punch tool 220° Blank punch exits Die tool, cap against its face 230° 2nd Transfer Air on; Blows cap into transfer chute 330° 1st Cap arrives into catch fingers at 2nd Station.
[0044] 2nd Station
0° Top of a stroke; Top Dead Center 60° Upper vacuum is turned on 136° Catch fingers start open, upper vacuum holds 1 st cap against upper knockout and tools close 180° Lugs formed in 1st cap; Bottom Dead Center 181° 1st cap (completed) and tools move up together 224° Catch fingers close completely after tooling passes 270° Upper vacuum to knockout turned off 280° Discharge air valve to nozzle is turned on 290° Knock out air to nozzle 87 is turned on 330° 2nd Cap arrives into catch fingers 336° 1st Cap actually moves to discharge position 335° Vacuum actually turns off on Cap #1 350° 1st Cap actually leaves press via chute 19
[0058] FIGS. 13A and 13B comprise a pneumatic diagram for the pneumatic portion of the press control. A “shop air” source of compressed air is supplied to the various electrically controlled valves (which are all labeled) to direct air under pressure to the above mentioned parts of the tooling, under management control of the electronics control ( FIG. 14 ) of the system. The details of such controls are apparent to persons skilled in this art from these diagrams
[0059] FIG. 14 is a block diagram of electrical/electronics controls for the system, which selectively turn on and off the compressed air to the nozzles providing lift or “blow up” air to hold the cap part against the rising upper tools in the first station, and providing a transfer air stream to quickly move a cap part into a transfer chute 19 . The third (upper) control provides timed discharge airstreams through nozzles 87 to move the finished caps into the discharge chutes 19 A. A pulse generator PG is driven by the press crankshaft (not shown) in typical fashion to generate a train of pulses related to the angular position of the crankshaft as it rotates, and these pulses are directed to the system PLC (Programmable Logic Controller). Since the diagram is divided into three functions which occur during a press cycle, the controller PLC is shown in each of the three diagram parts, but in fact one PLC is employed in the control system.
[0060] While the method herein described, and the form of apparatus for carrying this method into effect, constitute preferred embodiments of this invention, it is to be understood that the invention is not limited to this precise method and form of apparatus, and that changes may be made in either without departing from the scope of the invention, which is defined in the appended claims. | Transfer apparatus and method are provided from first ( 15 A, 16 A) to second ( 15 B, 16 B) stations of tooling in a cap ( 11 ) making press. This cap is biased against the first upper tools by a first airstream ( 50 ) introduced under the cap and moves upward with the first station punch ( 45 ). As the punch approaches its top location, a transfer airstream ( 52 ) begins while the first airstream is still on, and moves the cap out through a transfer chute ( 18 ) to the second station. The cap departs the chute and passes detents ( 67 ) on a pair of closed retention fingers ( 60 ) which define an extension of the transfer path from the chute into the open second station tools. A vacuum ( 85 ) applied to a port in the second station punch then holds the cup against the rising upper tools. When the punch clears the closing fingers and approaches its top location, an ejection airstream ( 87 ) commences to propel the finished cup via a discharge chute ( 19 ). | 1 |
BACKGROUND OF THE INVENTION
[0001] The leaching of lead into the environment has been a major concern of health officials and water supply professionals for many years. In addition to concern over direct leaching of lead into ground waters and surface waters, regulators and professionals have also been concerned with indirect leaching of lead from unlined landfills which generate acidic leaching conditions due to decay of organic matter and thus high levels of lead leaching potential. In response to the concern of lead leaching from both water and landfill leachate borne conditions, the USEPA under direction from Congress, prepared regulations for testing, managing, and disposing of lead bearing wastes. The regulations under the Resource Conservation and Recovery Act (RCRA) and Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA—a.k.a. Superfund) are extensive, complex, and have great impact on industry and practices involving heavy metals including lead. Under RCRA, lead bearing wastes may be considered hazardous if failing the Toxicity Characteristic Leaching Procedure (TCLP) at 5.0 ppm, and thus required to be disposed of at a hazardous waste landfill or treatment, storage and disposal facility (TSDF). These options are very expensive, normally $200.00 per waste ton. Under CERCLA, regulators can control or require treatment of lead wastes at almost any level as the states have flexibility in setting cleanup standards. Consequently, producing Pb bearing waste can be very expensive. Similar regulatory and remedial cost conditions exist in Japan, Switzerland, and other countries.
[0002] To date, shooting range soils contaminated by projectile lead have mostly been subject only to CERCLA action which requires stabilization and/or disposal of the Pb projectile contaminated soils at closed range sites. The Pb projectile bearing soil produced by the firing of lead bullets and shot over land or into stop berms commonly fails TCLP criteria of 5.0 ppm and is thus a characteristic hazardous waste when disposed or managed as a solid waste, and also subject to Pb soil cleanup standards by the USEPA and state regulators which can be more stringent than TCLP criteria. The current methods used to manage these lead projectile contaminated soils are reactive, i.e., they treat the lead after the soil becomes contaminated and, consequently, after the hazard of lead exposure to the environment and biological community exists. The chemicals currently used to treat lead bearing soils include mostly phosphates, silicates, cements, and sulfides. The methods are, however, reactive in design except for U.S. Pat. No. 5,722,928 issued to Forrester which provides a method for stabilizing leachable lead by adding phosphate and complexing agents such as iron, aluminum, and chlorides to the lead bearing material or waste prior to generating waste from industrial waste production operations such as automobile shredders. Existing stabilization technology for shooting ranges also utilize methods of stabilization regardless of the range usage and thus apply readily soluble chemicals in all areas subject to lead exposure and not discriminating amongst the dosage of lead projectiles applied to any given area.
[0003] Although seemingly illogical given the state of toxicological knowledge and regulation regarding lead exposure to the environment and potential receptors such as foul, shotgun and rifle/handgun shooting ranges still operate with little or no environmental protection devices in place other than indoor trap and outdoor mechanical bullet traps at few locations. The greatest exposure to the environment and biological receptors from any open range is the use of shotguns, where the practice of firing small yet numerous lead shot pellets into the air at airborne clay targets is practiced at over 3000 sites in the US alone. The resulting shower of lead pellets covers the range site at the soil surface where the greatest degree of exposure to wildlife, storm water, surface water and biological entry exists. The more severe exposure of lead projectiles to the environment is when shotgun users fire small birdshot with relatively high surface area per pellet into the woods and open environment at birds, showering the uncontrolled open environment, streams, ponds and marshes (where bird hunting is common) with these highly toxic elemental lead pellets. Thus there exists an immediate need to provide a proactive measure that protects the environment from the exposure to the lead shot and lead projectiles while allowing shooters continuance of the target practice as well as actual field foul firing.
SUMMARY OF THE INVENTION
[0004] The invention pertains to a method of reducing the solubility of lead on the surface of a lead projectile, comprising contacting lead projectile surface with at least one lead stabilizing agent in an amount effective in reducing the leaching of lead from lead projectile surface. In one embodiment, the lead leaching should be reduced to a level no more than 5.0 ppm lead as determined in an EPA TCLP test, performed on the projectile impact area lead contaminated soils or lead contaminated material receiving the projectile, as set forth in the Federal Register, vol. 55, no. 126, pp. 26985-26998 (Jun. 29, 1990). In another embodiment, an effective reduction in lead leaching (e.g., to about 50 ppb) can be measured using the Simulated Precipitant Leaching Procedure (SPLP) method 1310 or other water leach test.
[0005] In yet another embodiment of the invention, a phosphate (the lead stabilizing agent) and a lead mineral complexing agent are used in combination to reduce lead leaching and solubility under natural or induced lead leaching conditions. The lead mineral complexing agent can be calcium, silicates, sodium silicate, lime, magnesium oxides, calcium chloride, sodium chloride, potassium chloride, vanadium, boron, iron, aluminum, sulfates, ferric sulfate, or combinations thereof. In certain embodiments, the phosphate source may contain the lead mineral complexing agent, e.g., amber wet acid is produced in a manner such that it inherently contains the lead mineral complexing agent. Thus, the method is carried out in the presence of the lead mineral complexing agent since the phosphate source also provides the complexing agent as one product. Additional complexing agent beyond the amount provided by the phosphate source can be used.
[0006] The invention also pertains to a method of reducing bioavailability of lead by reducing Pb solubility from the surface at least one lead stabilizing agent in an amount effective in reducing the leaching of lead from lead projectile surface under natural or induced lead leaching conditions.
[0007] The invention also pertains to lead-containing projectiles having coated thereon at least one lead stabilizing agent in an amount effective in reducing the leaching of lead from lead projectile surface under natural or induced lead leaching conditions, whereby the lead and stabilizing agent form a mineral coating on the projectile in which the lead is in a form that is less soluble than its uncoated counterpart. The insoluble mineralized, coated projectiles can be produced by the method comprising coating lead-containing projectile with at least one lead stabilizing agent in an amount effective in reducing the leaching of lead from lead projectile surface under natural or induced lead leaching conditions, and allowing the coating to cure, wherein the lead and stabilizing agent form a mineral coating on the projectile in which the lead is in a form that is less soluble than its uncoated projectile counterpart.
[0008] This invention has the advantage of reducing the solubility of lead immediately upon first generation of the projectiles as a contaminant into the berm soil as well as into the environment. This method allows the soil berm and other lead projectile exposed soils/materials to remain below TCLP levels and thus exempt from RCRA hazardous waste regulation. This pre-firing stabilization method also assures control of Pb leaching and reduction of ecological and human exposure risks by creation of immediate upon contact water insoluble lead mineral coating(s). The desired mineral coatings produced would include Pb 5 (P0 4 ) 3 C1 (chloropyromorphite), calcium complexed phosphorus, Pb 3 (P0 4 ) 2 (lead phosphate), lead silicates, corkite, plumbogummite, and other relatively insoluble lead minerals which have significantly less mobility and toxicity than the projectile lead form as elemental or lead oxides. The invention provides a means to control Pb solubility both under TCLP testing for hazardous waste classification as well as Pb bioavailability in the open environment without significantly modifying the lead projectile weight and function and providing for such Pb surface mineralizing at an affordable price.
DETAILED DESCRIPTION OF THE INVENTION
[0009] A description of preferred embodiments of the invention follows.
[0010] This invention relates to the method of forming highly insoluble lead minerals on the surface of lead projectiles used in shotguns, handguns, rifles, and other ammunition, to reduce the leaching of lead therefrom when the projectiles are exposed to leaching conditions. The term “leaching or leachable conditions” used herein means any natural or induced condition that causes lead to solubilize and be removed from the lead-containing projectile with the mineral stabilizing agents. The insoluble lead mineral surface is formed prior to firing the projectile into the collection soils and/or open environment by contacting the projectile, prior to assembly with propellant shells or after bullet assembly. The lead-containing projectile is treated with a solution or slurry of phosphate or phosphate in combination with lead complexing agents including calcium chloride, calcium oxide, magnesium oxide, iron, aluminum, surfactants, mineral precipitant agents and combinations thereof. Formation of insoluble Pb minerals upon the surface of the lead-containing projectile will stabilize the Pb such that its leachability, under natural or induced leaching conditions, is reduced compared to its untreated form. A reduction in leaching can be assessed by any natural or induced leach test conditions such as, but not limited to TCLP (Method 1311), Simulated Precipitant Leaching Procedure (SPLP- Method 1310 which simulates rainwater leaching), Japan DI (uses acid adjusted DI water for 6 hours to simulate rainwater leaching), Swiss sequential DI (uses sequential DI water leaching to simulate rainwater), rainwater and other related leaching of lead from the surface of rifle, handgun and shotgun bullets.
[0011] The invention further pertains to lead projectiles treated according to the method. In one embodiment, the lead projectiles, in the form of pellets or shot, are coated with the stabilizing agent and optionally the lead mineral complexing agent, prior to placing the pellets or shot into the shell casing or housing. Dicalcium phosphate and/or tricalcium phosphate are the preferred phosphates as they impart a film upon the pellets or shot which functions as a proactive and reactive stabilizing seed. See Example 3. The plastic casing within the housing protects the phosphate coating on the shot until the shot is released upon firing. In another embodiment, projectiles in the form of bullets that come in contact with the gun barrel will preferably be coated with a phosphate other than dicalcium or tricalcium phosphate, preferably amber acid as the coating resulting therefrom is integral to the projectile and less prone to be removed between the breach and gun barrel exit by rifling edge contact with the projectile.
[0012] The invention further pertains to methods of reducing the bioavailablity of such projectiles upon exposure to the stomach acids of animals, humans or other biological exposures. The term “bioavailability” is intended to mean herein the form of Pb that is hazardous to humans, animals and plants, and can be assessed, for example in animals by studying metal uptake in kidneys and other organs. The method includes contacting the lead projectile surface with at least one lead stabilizing agent such that lead projectile surface has reduced Pb leaching potential prior to exposure to the environment, projectile collecting traps and/or biological community.
[0013] The term “stabilization” is herein defined as any reduction in the leachable levels of lead from the surface of projectiles used in rifle, handgun, shotgun, or other lead projectile ammunition, where the reduction is compared to an untreated projectile. The confirmation of Pb surface leaching reduction can be determined by performing a suitable leaching test on the projectile as well as physical evaluations of mineral formation under selective electron microscopy (SEM) and/or x-ray diffraction (XRD) techniques.
[0014] Projectile lead surfaces can be in elemental form and/or cationic form. The most common form of projectile lead is elemental in the form of projectile slugs or shot pellets. Soils and materials subjected to Pb projectile surface exposure can contain commonly as high as 100,000 ppm compositional lead and 1500 ppm TCLP leachable lead. Leachable lead in lead projectile exposed soils is commonly from 50 to 500 ppm TCLP, 200 ppm California Soluble Threshold Limit Concentration (STLC) and between 0.5 and 5.0 ppm total soluble and 1.0 micron suspended colloidal lead by water column and water extraction tests.
[0015] Leach test conditions, as defined herein, include the conditions to which a material or soil is subjected during dilute acetic acid leaching (TCLP), buffered citric acid leaching (STLC), distilled water, synthetic rainwater or carbonated water leaching (US SPLP, Japanese and Swiss and SW-924). Suitable acetic acid leach tests include the USEPA SW-846 Manual described Toxicity Characteristic Leaching Procedure (TCLP) and Extraction Procedure Toxicity Test (EP Tox) now used in Canada. Briefly, in a TCLP test, 100 grams of waste are tumbled with 2000 ml of dilute and buffered acetic acid for 18 hours. The extract TCLP (fluid number 1) solution is made up from 5.7 ml of glacial acetic acid and 64.3 ml of 1.0 normal sodium hydroxide up to 1000 ml dilution with reagent water. SPLC uses the ame tumbling as TCLP, but replaces acetic acid with simulated acid rain (e.g., a solution of carboxyl acid to pH 5.8 east of the Mississippi river and pH 5.9 west of the Mississippi river).
[0016] Suitable water leach tests include the Japanese leach test which tumbles 50 grams of composited soil sample in 500 ml of water for 6 hours held at pH 5.8 to 6.3, followed by centrifuge and 0.45 micron filtration prior to analyses. Another suitable distilled water CO 2 saturated method is the Swiss protocol using 100 grams of cemented waste at 1 cm 3 in two (2) sequential water baths of 2000 ml. The concentration of heavy metals and salts are measured for each bath and averaged together before comparison to the Swiss criteria.
[0017] Suitable citric acid leach tests include the California Waste Extraction Test (WET), which is described in Title 22, Section 66700, “Environmental Health” of the California Health & Safety Code. Briefly, in a WET test, 50 grams of waste are tumbled in a 1000 ml tumbler with 500 grams of sodium citrate solution for a period of 48 hours. Leachable lead, contained in the waste, then complexes with citrate anions to form lead citrate. The concentration of leached lead is then analyzed by Inductively-Coupled Plasma (ICP) after filtration of a 100 ml aliquot from the tumbler through a 0.45 micron glass bead filter. A WET result of ≧5 ppm lead will result in the range soil as hazardous in California.
[0018] According to the methods of the invention, leachable lead at the surface of a lead projectile can be stabilized by contacting at least one lead stabilizing agent with the projectile surface at sufficient dosage and duration to allow for substitution and precipitation of relatively soluble lead to relatively insoluble lead minerals. The amount of stabilizing agent incorporated within and/or upon the projectile surface will be that which is effective in reducing the leaching of lead from the projectile as needed, for example to a level no more than 5.0 ppm lead, as determined in an EPA TCLP test performed on the projectile or material receiving the projectile as set forth in the Federal Register, Vol. 55, No. 126; pp. 26985-26998 (Jun. 29, 1990), or other leaching test.
[0019] Examples of suitable lead stabilizing agents include, but are not limited to, phosphate fertilizers (e.g., MAP, DAP, SSP, TSP), phosphate rock, pulverized phosphate rock, calcium orthophosphates, monocalcium phosphate, dicalcium phosphate, tricalcium phosphate, trisodium phosphates, dolomitic limestone, hydrated limestone, calcium oxide (quicklime), calcium carbonates, magnesium oxides, silicates, sodium metasilicates, potassium silicates, natural phosphates and lead mineralizing agents and combinations of the above, phosphoric acids, green phosphoric acid, amber phosphoric acid, technical phosphoric acid, wet process produced phosphoric acids, phosphonates, Coproduct solution, hypophosphoric acid, metaphosphoric acid, hexametaphosphate, pyrophosphoric acid, polyphosphate, fishbone phosphate, animal bone phosphate, fishbone apatite, herring meal, bone meal, phosphorites, and combinations thereof. Salts of phosphoric acid can be used and are preferably alkali metal salts such as, but not limited to, trisodium phosphate, dicalcium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, tripotassium phosphate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate, trilithium phosphate, dilithium hydrogen phosphate, lithium dihydrogen phosphate or mixtures thereof.
[0020] The lead stabilizing agent can be incorporated or applied onto the projectile surface by bath contact, spray, or other surface application means. It also remains possible that the projectile Pb may be modified during formation of the lead by applying stabilizing agent(s) to the lead melting and projectile production process, although such a process appears at this time to be more burdensome and costly than a simpler post-projectile production formation of a stabilized lead surface. Given that the lead surface is the primary exposure area to the environment and that the mineral surface will likely reduce or significantly retard lead diffusion from the non-stabilized lead core, the stabilization of the surface alone is offered as the most cost effective control of lead contamination. The invention however comtemplates use of the method of the invention in the “field” by the end user. A composition comprising the lead stabilizing agent and optionally the lead mineral complexing agent can be conveniently packaged in the form of a spray or wipes for application to older lead projectiles not stabilized during projectile and shell production.
[0021] In one embodiment of the invention, the projectile surface is contacted with a wet stabilizing agent mixture of hexametaphosphate and 32% calcium chloride solution in a simple bath reactor for 24 hours and thereafter allowed to drip dry while amorphous crystals continue to form for an additional 48 hours prior to projectile rinsing and drying, preferably at ambient temperature. The option to utilize various stabilizing agents, bath durations and complexing agents provides the production engineer flexibility in stabilizing agent recipe selection, with a preferred choice responding to the site and use criteria such as TCLP, DI or other biological based toxicity criteria.
[0022] The use of engineered phosphates such as wet process amber phosphoric acid, green phosphoric acid, aluminum finishing Coproduct blends of phosphoric acid and sulfuric acid, technical grade phosphoric acid, trisodium phosphate, tetrapotassium polyphosphate, monocalcium phosphate, monoammonia phosphate (MAP), diammonium phosphate (DAP), single superphosphate (SSP), superphosphate, triple superphosphate (TSP), hexametaphosphate (HMP) and combinations thereof would, as an example, provide various amount of water soluble phosphate contact with projectiles surface. The term “wet process amber phosphoric acid” refers to phosphoric acid formed by acidolation of phosphate rock ore with sulfuric acid. The term “green phosphoric acid” refers to phosphoric acid formed by calcined ore acidolated with sulfuric acid. The term “coproduct and coproduct blends” refers to a by-product from the finishing of aluminum comprising phosphoric acid and sulfuric acid and optionally comprising aluminum and other metals (such as iron).
[0023] In certain cases such as use of amber and green acid, such acids comprise sulfuric acid, vanadium, iron, aluminum and other complexing agents which could provide for a single-step formation of complex minerals on the lead surface. The phosphoric acids, coproducts, HMP, MAP, DAP, SSP, trisodium phosphate, tetrapotassium polyphosphate, monocalcium phosphate and TSP size, dose rate, mineral formation contact duration, application, and phosphate stabilizer contact means, could be engineered for each type of projectile and contact method employed. When lead comes into contact with the stabilizing agent, low water soluble compound(s) begin to form, typically a mineral phosphate or precipitate formed through substitution or surface bonding, which is less soluble than the lead originally in the projectile. For example, the mineral apatite lead phosphate Ca 4 (Pb)(P0 4 ) 3 OH, lead phosphate Pb 3 (P0 4 ) 2 , lead silicate Pb 2 (Si0 3 ), lead sulfide PbS, chloropyromorphite Pb 5 (PO 4 )Cl, corkite and plumbogummite can be formed by adding respective precipitating agents with complexing agents to the projectile surface at standard temperature and pressure.
[0024] It also remains possible that modifications to reactor temperature and pressure (preferably under standard temperature and pressure conditions) may accelerate or assist formation of lead minerals, although such methods are not considered optimal for this application given the need to limit cost and provide for optional field based lead stabilizing operations that would be complicated by the need for pressure and temperature control devices and vessels.
[0025] In another method, the lead projectiles are contacted with at least one phosphate in the presence of a lead mineral complexing agent selected to generate specific mineral on the projectile surface. The lead mineral complexing agent can include iron, aluminum, calcium, chlorides (e.g., sodium chloride, potassium chloride, calcium chloride), silicates (e.g., sodium silicate), sulfates (e.g., ferric sulfate), vanadium, boron, lime, magnesium oxide, surfactants and various other agents which provide for or assist in formation of phosphate minerals such as chloropyromorphite and other lead minerals. Use of phosphates in the presence of complex agents for mineral formations of lead bearing wastes is taught by U.S. Pat. No. 5,722,928 issued to Forrester, the entire teachings are incorporated herein by reference.
[0026] The amounts of lead stabilizing agent used, according to the method of invention, depend on various factors including projectile character, desired lead solubility reduction potential, desired lead mineral toxicity, and desired lead mineral formation relating to toxicological and site environmental control objectives. It has been found that an amount of certain stabilizing agents such as amber wet process phosphoric acid and calcium chloride solution, equivalent to between about 0.1% and about 2.0% by weight of projectile pellet or slug is sufficient for initial TCLP stabilization. However, the foregoing is not intended to preclude yet higher or lower usage of stabilizing agent or combinations if needed since it has been demonstrated that amounts greater than 0.5% by weight also work, but are more costly. Given the relatively smooth and non-porous surface character of lead projectiles and the atomic density of elemental lead, it is unlikely that larger amounts of stabilizers would bond, combine, precipitate or otherwise attach to the surface of the lead projectile.
[0027] Using the methods of the invention, it was discovered that insoluble mineral formation can be enhanced by one or a combination of duration in the coating bath and/or curing. The purpose of curing the projectile or shells is to allow for mineral crystals to form; more crystal growth over time. The optimal minimal duration for the projectile to reside in the coating bath is approximately 24 hours but other coating times can be used. Once the projectile is coated, it may be desirable to let it cure prior to use. The optimal duration for curing is at least 48 hours but shorter or longer cure times are contemplated. It should be noted that no curing is required to provide lead control. In view of this finding, the invention further pertains to methods of producing a lead-containing projectile having a mineral coating thereon, comprising coating lead-containing projectile with at least one lead stabilizing agent in an amount effective in reducing the leaching of lead from lead projectile surface under natural or induced lead leaching conditions, allowing the coating to cure, wherein the lead and stabilizing agent form a mineral coating on the projectile in which the lead is in a form that is less soluble than an uncoated projectile. The curing can occur during ammunition shelf storage.
[0028] The examples below are merely illustrative of this invention and are not intended to limit the invention in any way.
EXAMPLE 1
[0029] In this example, shot projectiles were stabilized with varying amounts of stabilizing agents in aqueous solutions, including amber phosphoric acid (WAA), green acid (WAG), technical grade acid (WAT), coproduct solution (WCP), 33% hexametaphosphate solution (HMS), 32% calcium chloride solution (CCS), 50% surfactant solution (Dow TergitolTM) (SFS), 50% sodium silicate solution (NSS) and lime (CaO) pH adjusted (6.10) batch reactors under full contact wet bath exposure of projectiles to solutions with up to 24 hours and curing for 48 hours, under standard temperature and pressure. Both stabilized and un-stabilized projectiles were subsequently tested for TCLP and DI leachable Pb. Projectiles were extracted according to TCLP procedure set forth in Federal Register, Vol. 55, No. 126, pp. 26985-26998 (Jun. 29, 1990), which is hereby incorporated by reference and water extraction by substituting deionized water for the TCLP extraction fluid solution in the TCLP test. This test procedure is also referenced in 40 C.F.R. 260 (Appendix 2) and EPA SW 846, 3rd Edition. The retained leachate was digested prior to analysis by ICP. Stabilizing bath dosages were calculated by measuring projectile weight increase after final drying or each given bath recipe. It was found that projectiles had higher retention of certain bath recipes likely due to differences in surface adsorption ability and mineral formations.
TABLE 1 Duration Stabilizer Dose (%) Bath/Curing (hrs) TCLP/DI Pb (ppm) 0 0/0 154/12 0.12 WAA 1/48 24/ND 0.11 WAA 24/48 1.7/ND 0.09 WAG 24/48 3.2/ND 0.07 WAT 24/48 3.4/ND 0.10 HMS 24/48 4.4/ND 0.11 WAA/NSS 1/1 blend 24/48 0.3/ND 0.14 WAA/CCS 1/1 blend 24/48 ND/ND 0.05 WAA/SFS 1/1 blend 24/48 2.2/ND 0.11 WAG/CaO 1/1 blend 24/48 (pH 6.10) 0.40/ND 0.10 WCP 24/48 17/ND 0.50 FBA/1 H 2 O 24/48 ND/ND 0.50 TSP/1 H 2 O 24/48 0.1/ND 0.10 WAA 10 seconds/0 32/ND
[0030] The results in Table 1 readily established the operability of the present process to stabilize lead on the surface of lead projectiles thus reducing projectile leachability and bioavailability. Given the effectiveness of the phosphates and complexing agents in causing lead to stabilize as presented in the Table 1, it is believed that an amount of the stabilizing agents equivalent to less than 2% by weight of lead projectile should be effective to stabilize lead projectile surfaces. It is also apparent from the Table 1 results that certain stabilizing agents and complexing blends are more effective for lead surface stabilization. It also is apparent that pH increase to neutral range pH levels in the mineral bath can improve the formation of Pb minerals, as seen from standard pPb-pH diagrams on lead amphoteric and non-amphoteric solubilities.
EXAMPLE 2
[0031] Shot projectiles were treated according to the method of Example 1 but using the formulation set forth in Table 2. Two hundred grams treated shot were fired into 5 lbs loam and leachable Pb was measured.
TABLE 2 hot Fired Samples: 200 gms into 5 lbs. Loam Recipe TCLP SPLP Baseline Soil/Lead 190 0.7 0.12 WAA 17.1 ND 0.14 WAA/CCS 4.1 ND 2.0 WAA/1 CaCl 2 ND ND
EXAMPLE 3
[0032] In this example, shot projectiles were stabilized using the method of Example 1 but using the formulations set forth in Table 3. The duration in the bath was for 24 hours. The curing time for all formulations was 24 hours.
TABLE 3 Formulation SPLP Pb (ppm) 0.0% (Aged Lead Shot) 0.54 2.0% WAA Amber Acid + 1% CaCl 2 <0.01 2.0% DCP + 1% CaCl 2 0.01 2.0% TCP + 1% CaCl 2 0.01
[0033] SPLC was performed on the shot. The 2.0% DCP+1% CaCl 2 blend produced a chemical film on the shot. Shot having this coating was selected for testing in shooting range applications. The residual film will act as the proactive and reactive stabilizing seed. The shot will serve as the carrier for delivering the stabilizing agent to the range soil and surrounding environment.
[0034] While this invention has been particularly shown and described with references to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention encompassed by the appended claims. | The invention pertains to a method for reducing the leaching of lead from lead projectile surface. The method includes contacting the lead projectile surface with a lead stabilizing agent or a lead stabilizing agent in the presence of a lead mineral complexing agent. The lead stabilizing agents provides a means to stabilize lead on the bullet/shot surface and thus reduce lead leaching and contact to the environment. This method eliminates the need to remove or re-treat range soils and greatly reduces the environmental and health risks associated with the use of lead as projectiles in the open environment as well as at control trap ranges. | 0 |
BACKGROUND AND SUMMARY OF THE INVENTION
Pipe protectors are tubular rubber members that surround pipe used in downhole drilling operations. The rubber pipe protector serves as a bumper for the pipe which is generally introduced into metal casing in the well hole. The pipe protector should fit snugly around the outside diameter of the pipe. During the drilling operation the pipe is rotated rapidly. If the pipe protector is not secure, slippage can occur and the pipe protector will slide off of the desired location on the pipe.
Reliable pipe protectors are necessary during directional drilling operations during which process the well is drilled at an angle in a non-vertical direction. The pipe will contact the casing wall with metal to metal contact that causes wear on the pipe. By spacing pipe protectors along the pipe string, the rubber pipe protectors rather than the pipe contact the well casing.
A typical pipe protector well known to those in the art is a split type pipe protector. The tubular rubber member is typically about 4 to 12 inches in length and has an opening the length of the member that can be further opened to facilitate installation onto the pipe. After the pipe is enclosed and encircled by the pipe protector, the rubber tubular member is secured or fastened. Many split type pipe protectors have interlocking metal teeth covered by rubber and close with a key fastener inserted lengthwise through the teeth. The metal teeth are connected to a cylindrical metal insert inside the tubular rubber member. The metal insert may be smooth or corrugated metal.
The inner diameter of the pipe protector is sized to match the outer diameter of the drill pipe. The conventional pipe protectors are sensitive to the outer diameter dimension of the pipe on which they are installed. Changes in the outer diameter of the pipe of about (-)0.010 inch reduce the gripping forces of the pipe protector and allow the protector to slip or rotate on the pipe at relatively low side forces. Drill pipe commonly can vary in outer diameter by -0.05% depending on pipe size. Conventional pipe protectors slip on the undersized pipe and fail to provide the desired bumper effect and can be detrimental to the drilling operation. It is possible to lose the pipe protector downhole. The drilling operation must then be shut down to fish out the pipe protector. Slipping of undersized pipe protectors on drill pipe is a serious problem. Attempts to alleviate this problem have included wrapping strips of rubber around the pipe circumference before placing the pipe protector onto the pipe. Although this method was moderately successful in reducing slippage, it is tedious and impractical in field applications.
The present invention provides a variable diameter pipe protector that prevents slipping on undersized pipe, but can also be used on full sized pipe. A pipe protector capable of surrounding a full size outer diameter pipe is provided with at least one rubber flap attached to the inside surface. In one embodiment the rubber flap attached to the inside surface can be cut. The severed portion is removed leaving the remaining portion of the flap attached. The flap provides sufficient inner diameter thickness to compensate for the undersized pipe. The smaller the diameter of the pipe the more of the flap is left inside the pipe protector to serve as additional volume of rubber needed to give a tight grip on the pipe. In a preferred embodiment the flap extends substantially the length of the rubber tubular member. If the pipe is sized to the full diameter, the flap is completely detachable and can be removed. The pipe protector can be a split type design with an opening the length of the rubber tubular member. The opening the length of the tubular rubber member is capable of separation to facilitate the introduction of the pipe. A closing means is used to secure the pipe protector for installation after the flap material has been cut and detached. The cylindrical metal insert with interlocking metal teeth is typically included in this design.
In an alternative embodiment, multiple detachable rubber flaps are attached to the inside surface of the pipe protector. During installation of the pipe protector on the pipe, as many flaps as needed to provide a tight grip are left attached to the inside the pipe protector. The flap or flaps are preferably attached with an adhesive for relatively easy removal. The flaps are placed on the inside surface of the rubber tubular member so as not to overlap each other.
Conventional split type pipe protectors can be adapted with a detachable flap or flaps to accompany undersized pipe of various diameters.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a top view of one of the preferred embodiments of the variable bore pipe protector showing three detachable flaps.
FIG. 2 is a side view of the variable bore pipe protector installed onto a length of pipe.
FIG. 3 is a lengthwise section through the installed pipe protector and pipe.
FIG. 4 is a cross section taken at 4--4 on FIG. 3 of the pipe protector installed onto the pipe.
FIG. 5 is a top view of a preferred embodiment with one flap.
DETAILED DESCRIPTION OF THE INVENTION
The pipe protectors of this invention can be made from polymers generally used for downhole drilling, and known to those skilled in the art. A preferred rubber is high acrylonitrile butadiene copolymer also known as nitrile base polymer. The range of durometer hardness for the tubular member is from about 50 Shore A to about 80 Shore A. The preferred range is from about 65-70 Shore A durometer hardness. The rubber flaps are made within the same range of durometer hardness, but do not have to be the same durometer hardness as the tubular member. In a preferred embodiment rubber characterized by high coefficients of friction can be used.
The acrylonitrile copolymer rubber has oil and fuel resistance, high tensile and tear strength, abrasion and gas impermeability resistance and heat resistance. The acrylonitrile copolymer rubber can be compounded with other additives known to those skilled in the art to improve and enhance certain characteristics. In the preferred embodiment the flaps are made of rubber with similar chemical and physical characteristics and chemical resistance.
A preferred polymer formula for a colored noncarbon reinforced rubber is shown in Table 1 below.
TABLE 1______________________________________Colored Non Carbon Reinforced PolymerComponent Parts Per Hundred Polymer______________________________________NBR Polymer 100Zinc Oxide 4-9silica 25-60Stearic Acid 1.0-1.5Antioxidants and 3.5-10.0AntiozonantsProcessing Oils 25-50Reinforcing Resin and 5-15Resin CurativeIron Oxide Colorant 3-8Sulfenamide Curative 2-5.5Thiuram Curative 1.5-4.5______________________________________
A preferred polymer formula for a carbon black reinforced polymer stock is shown in Table 2 below.
TABLE 2______________________________________Black Carbon Reinforced PolymerComponent Parts Per Hundred Polymer______________________________________NBR Polymer 100Zinc Oxide 4-9Stearic Acid 1.0-1.5Carbon Black (N774) 30-70Antioxidant and 3.5-10.0AntiozonantsProcessing Oils 25-50Reinforcing Resin and 5-15Resin CurativeSulfenamide Curative 2-5.5Thiuram Curative 1.5-4.5______________________________________
A preferred embodiment of the variable bore pipe protector is illustrated in the figures accompanying the application. FIG. 1 is a top view of one of the preferred embodiments with multiple flaps. The pipe protector in FIG. 1 has three rubber flaps to accommodate a relatively wide range of outer pipe diameters. Specifically, pipe protector body 10 is a generally tubular rubber member. Flaps 12, 14, and 16 are attached to the inside surface of the tubular member 10. The points of attachment 18, 20 and 22 to hold the rubber flaps in place are provided preferably by an adhesive suitable for two rubber parts. Also shown in the top view is the opening 24 typical in a split type pipe protector that is capable of separation to facilitate the installation of the pipe. The top of the latch key 26 is also shown.
FIG. 2 is a side view of the split type pipe protector installed onto a pipe 28. The flaps 12, 14 and 16 are not visible in this view. The opening in the pipe protector consists of interlocking teeth formed by the cut of the opening 24. Key 26 is inserted through the teeth to close and secure the tubular member 10 around the pipe 28. The tubular member has installation holes 30 and 32 provided to facilitate closing the tubular member 10 around pipe 28.
FIG. 3 is a lengthwise section through a portion of pipe 28 with at least two flaps shown between the pipe 28 and tubular member 10. In FIG. 3 the flaps are designated as F 1 and F 2 for reference. FIG. 1 shows a multiple flap embodiment, and the flaps shown in the section in FIG. 3 are two of the three flaps shown in FIG. 1. The reference numerals for the parts other than the flaps correspond to those used in the other figures for ease of comparison. The lengthwise section shows the cylindrical metal member 29 which is an insert in the rubber tubular member 10.
FIG. 4 is a cross section of a three flap embodiment installed on a pipe which has the outer diameter to accommodate all three flaps to provide for a secure fit for the pipe protector. The cross section in FIG. 4 shows tubular member 10 installed around pipe 28 with opening 24 in the closed position secured by key 26. In the cross section metal member 29 is a corrugated insert. The metal member 29 has hollow interlocking teeth one of which is shown in the cross section at reference numeral 27. Key 26 goes through a series of metal teeth that are covered by rubber, thereby securing the closure of the pipe protector around the pipe. The rubber flaps 12, 14 and 16 are shown between the pipe 28 and tubular member 10 providing additional inner thickness for the pipe protector to compensate for the undersized pipe. In the preferred embodiment there is a space provided between the flaps on either side of the opening 24 and key 26 so the flaps will not interfere with the closure.
FIGS. 5 is a single flap embodiment illustrated by a top view to show the flap. The rubber tubular member 40 is the pipe protector body and in the preferred embodiment for this design is a split type protector as described herein. The opening 42 to facilitate the introduction of the pipe as well as the key 44 are the same as described above for other embodiments with multiple flaps. The embodiment shown in FIG. 5 has one flap 46 with a point of attachment 48. The flaps can be attached at more than one point as long as it is easily removed. With the single flap design, a portion of the flap is severed and removed, leaving sufficient flap material to compensate for the undersized pipe and provide a tight grip.
In a field installation the pipe protector of the present invention would be test fit on the pipe. If the pipe protector fits securely and comfortably around the outer diameter of the pipe with all flaps in place, no flaps are removed. If the flaps provide too much volume for a good fit, flaps may be removed as needed until the proper fit is obtained. The flaps are attached so that detachment can be done manually. In the preferred embodiment the flaps are attached by an adhesive such as rubber cement. In an alternative embodiment, a mechanical fastener such as a staple may be used. In the single flap embodiment, a portion of the flap is severed, detached and the pipe protector is refitted on the pipe. Additional flap material can be severed and detached until the proper fit is obtained.
The following Table 3 illustrates the benefits of the variable diameter pipe protector. Drill pipe with outer diameters ranging from 5.00 inches to 4.830 inches were tested to determine the side load force on the pipe that would cause the pipe protector to slip. Standard drill pipe for a 5 inch outer diameter is often undersized. The API minimum for 5 inch pipe is 4.830 inches. A three flap variable diameter pipe protector as described herein was used in the side load test. The testing machine allows the measurement of slippage between the casing and the rotating pipe protector. Drilling fluid also may be injected between the casing wall and the rotating pipe protector to simulate actual drilling conditions. The testing procedure was developed by Mauer Engineering Inc., 2916 West T. C. Jester, Houston, Tex. 77018. The procedure is published in a paper entitled "Laboratory Drill Pipe Protector Tests", Garkasi Ali; Hall, Russell W. Jr., and Deskins, W. Gregory; PD Vol. 56 Drilling Technology, Editor: John P. Vozniak, Book No. G00827, ASME (1994); presented at Energy Sources Technology Conference & Exhibition, New Orleans, La. Jan. 23-26, 1994. The standard pipe protector without flaps is designed to fit securely around a pipe with a 5 inch outer diameter.
TABLE 3______________________________________Variable Diameter Pipe Protector Test ResultsPipeOuter Slip Loads (lbs)Diameter Standard 1 Flap 2 Flap 3 Flap______________________________________5.00 9663 NT NT NT4.975 7920 11102 >12000 >120004.950 3870 7945 10644 >120004.900 706 4890 6990 >120004.830 <100 <100 5113 8072______________________________________ NT = Not Tested
As shown in Table 1 the standard pipe protector sized to fit a 5 inch pipe slips on a 5 inch pipe at 9663 lbs. side load. The test machine capacity was 12,000 lbs. As the pipe diameter decreased, the additional volume provided by the flaps compensated for the difference in diameter and prevented slippage. In most cases, variable size pipe protector prevented slippage on a pipe with undersized diameters at a side load exceeding the side load that caused slippage of the standard pipe protector on a 5 inch pipe.
The examples provided in this specification are not intended to limit the scope of the claimed invention. Those skilled in the art will appreciate additional embodiments and variations that can be practiced based in addition to those disclosed herein. | A pipe protector is disclosed comprising a tubular rubber member with an inner diameter sized to the approximate outer diameter of a pipe. The protector is a variable diameter pipe protector that prevents slipping on undersized pipes, but can also be used on full sized pipes. The pipe protector is capable of surrounding a full size outer diameter pipe and is provided with at least one rubber flap attached to the inside surface to compensate for undersize pipe diameters. | 4 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] The present application claims the benefit of U.S. provisional application No. 60/566,594 filed on Apr. 30, 2004, which is incorporated in its entirety herein by reference.
STATEMENT OF GOVERNMENT FUNDING
[0002] The United States Government has a paid-up license in this invention and the right in limited circumstances to require the patent owner to license others in reasonable terms as provided for by the terms of NIH Grant Nos. RO1GM51449 and RO1A105088.
FIELD OF THE INVENTION
[0003] The present invention is concerned with HSV-1 vectors in which gene expression is controlled using the tetracycline operator and repressor. Expression of sequences coding for the tetracycline repressor is under the control of HSV-1 immediate-early promoters. Because gene expression from HSV-1 immediate-early promoters is significantly enhanced by the HSV-1 virion-associated transactivator VP-16 upon the entry of virus into a host cell, a very high level of repressor expression occurs at the time of infection. As a result, gene expression from promoters under the control of tetracycline operator sequences is essentially completely suppressed. Upon exposure of cells to tetracycline, repressor is released from the operator sequence and gene expression proceeds. Using this system, very high levels of expression can be obtained in neurons in vivo and this expression can be closely regulated.
BACKGROUND OF THE INVENTION
[0004] Herpes simplex virus type 1 (HSV-1) is a linear double stranded DNA virus with genome size of about 152 kb. The genome of HSV-1 is encapsided by an icosadeltarhedral capsid surrounded by a viral envelope. HSV replicates in epithelial cells and establishes life-long latent infection in neuronal cell bodies within the sensory ganglia of infected individuals. The latent viral genome is maintained in an episomal state and does not ordinarily cause serious disease or interfere with normal cellular function (Rock, et al., J. Virol. 55:849-852 (1985)). These characteristics have made HSV of particular interest for use as a vehicle for gene therapy procedures designed to treat diseases of the CNS (Latchman, Curr. Gene Ther. 2:415-426 (2002); Glorioso, et al, J. Neurovirol. 9:165-172 (2003); Jacobs, et al., Neoplasia 1:402-416 (1999); Advani, et al., Clin. Microbiol. Infect. 8:551-563 (2002); Martuza, et al., Science 252:854-856 (1991)). One difficulty that has been associated with the development of such procedures has been in finding vectors that induce high expression levels of delivered genes and do so in a manner that can be tightly regulated.
[0005] During the past decade, significant progress has been made in developing genetic switches that can be used to control the expression of recombinantly delivered genes (Clackson, Gene Ther. 7:120-125 (2000); Gossen, et al., Proc. Nat'l Acad. Sci. USA 89:5547-5551 (1992); Gossen, et al., Science 268:1766-1769 (1995); No, Proc. Nat'l Acad. Sci USA 93:3346-3351 (1996); Wang, et al., Proc. Nat'l Acad. Sci. USA 91:8180-8184 (1994); Rivera, et al., Nat. Med. 2:1028-1032 (1996)). In the case of prokaryotic elements associated with the tetracycline (tet) operon, systems have been developed in which the tet repressor protein is fused with polypeptides known to modulate transcription in mammalian cells. The fusion protein has then been directed to specific sites by the positioning of the tet operator sequence. For example, the tet repressor has been fused to the activation domain of transactivator (VP-16) and targeted to tet operator sequences positioned upstream from the TATA element of promoter of a selected gene (Gossen, et al., Proc. Natl. Acad. Sci. USA 89:5547-5551 (1992); Kim, et al., J. Virol. 69:2565-2573 (1995); Hennighausen, et al., J. Cell. Biochem. 59:463-473 (1995)). The tet repressor portion of the fusion protein binds to the operator thereby transporting the VP-16 activator to the specific site where the induction of transcription is desired. An alternative approach has been to fuse the tet repressor to the KRAB repressor domain and target this protein to an operator placed several hundred base pairs upstream of a gene. Using this system, it has been found that the chimeric protein, but not the tet repressor alone, is capable of producing a 10 to 15-fold suppression of CMV regulated gene expression (Deuschele, et al., Mol. Cell Biol. 15:1907-1914 (1995)). One problem with these types of systems is that a portion of fusion proteins corresponding to the mammalian transactivator or repressor trends to interact with cellular transcription factors and cause pleiotropic effects.
[0006] Recently, a tetracycline-inducible transcription switch for use in mammalian cells was developed (U.S. Pat. No. 6,444,871; Yao, et al., Hum. Gene Ther. 9:1939-1950 (1998)). This system was highly successful at regulating gene expression and has been used in developing plasmid-based vectors that are now sold commercially (T-REx™, Invitrogen, CA).
SUMMARY OF THE INVENTION
[0007] The present invention is concerned with HSV-1 vectors that can be used for recombinantly expressing a structural sequence in vivo. HSV-1 vectors are recognized in the art as being made up of three components: a capsid, a viral envelope, and genomic DNA. The present invention is particularly concerned with the genomic DNA but it will be understood that the other components which make up the vectors, i.e., the HSV capsid and viral envelope are also present. The term “structural sequence” as used herein refers to a sequence of nucleotides encoding either a polypeptide or an RNA segment, particularly an antisense RNA segment, that is not translated into protein.
[0008] More specifically, the invention is directed to a recombinant HSV viral vector containing a genomic DNA construct that includes at least two (and preferably only two) nucleotide sequences coding for tetR, each of which is under the regulation of an VP-16 responsive HSV-1 immediate-early promoter. This promoter may be the HSV-1 ICP-0 or ICP-4 immediate early promoter or a hybrid formed by combining these promoters with the HSV-1 latency-associated promoter LAP2. To make a hybrid promoter between ICP0 and LAP2 (ICP0/LAP2) or between ICP4 and LAP2 (ICP4/LAP2), a DNA fragment containing the LAP2 promoter (Palmer et al., J Virol 74:5604-5618 (2000)) is inserted at about 250-500 bp upstream of (i.e., 5′ to) the TATA element of the ICP0 or ICP4 promoter.
[0009] The genomic DNA construct carried by the HSV-1 vector also includes an additional promoter that is characterized by the presence of a TATA element. A tetracycline operator sequence (tetO) is positioned so that the first nucleotide in tetO is between 6 and 24 nucleotides 3′ to the last nucleotide in the TATA element (i.e., counting the first nucleotide 3′ to the TATA element as “1,” the first nucleotide in the tetO sequence would be nucleotide “6”-“24.” Lying 3′ to the tetO sequence is the structural sequence and this is operably linked to the additional promoter, i.e., expression of the structural sequence is under the control of the additional promoter.
[0010] The tetO sequence occurs in different forms depending upon the presence or absence of two well recognized tetR binding sites designated as Op-1 and Op-2. The most preferred form of operator for use in the present invention has two Op-2 sites, each such site having the nucleotide sequence: CCCTATCAGTGATAGAG (SEQ ID NO:1). In a preferred embodiment, these two Op-2 sites are joined by a linker sequence 3-10 nucleotides in length, with a linker of four nucleotides being most preferred.
[0011] In other preferred embodiments, the additional promoter present in the DNA vector described above is the human cytomegalovirus (hCMV) immediate early promoter or the LAP2/hCMV immediate-early promoter. However, other strong promoters may also be used. In one embodiment, the structural gene whose expression is regulated by the second promoter is LacZ. This gene serves as a marker that can be used for identifying infected cells that are actively expressing genes recombinantly. Methods for producing such vectors and using them to study gene expression in vitro and in vivo are described in detail in the Examples section below.
[0012] The HSV-1 vectors described above should, most typically, be replication deficient. The term “replication deficient” as used herein means that the genomic DNA of the virus has been engineered so that it cannot replicate when injected into a subject. As described further in the Examples section, one way of producing a replication-deficient HSV-1 vector is to modify its genome so that it is no longer capable of expressing a functional UL-9 gene. Under these circumstances, vector will only replicate if the UL-9 gene product is provided, e.g., during in vitro culture.
[0013] The genomic DNA constructs can be made using standard methods for synthesizing and splicing DNA. Alternatively, viral DNA can be directly altered so that either an endogenous ICP-0 gene or an endogenous ICP-4 gene has been replaced with a sequence coding for the tetracycline repressor. The replacement must occur in such a fashion that tetR is operably linked to either the ICP-0 or ICP-4 promoter and the tetR protein is correctly produced. The virus must also contain at least one recombinant structural sequence located 3′ to a tetO sequence and which is operably linked to an additional promoter. The additional promoter must have a TATA element and the tetO segment must begin 6-24 nucleotides 3′ to the last nucleotide in the TATA element.
[0014] Finally, the invention includes methods for recombinantly expressing selected nucleotide sequences in host cells by infecting them with the HSV-1 vectors described above. The selected nucleotide sequence should be present in the virus as the “recombinant structural sequence.” The method is particularly well adapted for obtaining recombinant expression in neurons in vivo. This will provide a means for scientists to determine how on- and off or dose-dependent expression of a variety of recombinant genes affects neuronal growth and development. Infection may also be performed on host cells in vitro which may then be transplanted into an animal or studied directly.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 : Schematic diagram of genomes of HSV-1 recombinants KOR (A) and QR9TO-lacZ (B): UL and US represent the unique long and unique short regions of the HSV-1 genome, respectively, which are flanked by their corresponding inverted repeat regions (open boxes). Replacements of the ICP0 coding sequences in both repeats surrounding UL region with DNA elements encoding tetR (black box) and intron II of the rabbit β-globin gene (obliquely striped box) flanked by ICP0 sequences are shown above the diagram of the HSV-1 genome. An expanded map of the region of UL9 containing the UL9 open reading frame (black line box) and flanking sequences between restriction sites BsiW I and Not I is shown below the diagram. Relevant restriction sites within the UL9 open-reading frame used to construct QR9TO-lacZ are indicated. (B) QR9TO-lacZ was generated by replacing the Xcm I-Mlu I DNA fragment within the UL9-coding sequences of KOR with DNA sequences containing lacZ gene (gray box) under control of the tetO-bearing hCMV major immediate-early promoter (cross hatched box). The line box shows the polyadenylation signal sequence of bovine growth hormone gene.
DEFINITIONS
[0016] The description that follows uses a number of terms that refer to recombinant DNA technology. In order to provide a clear and consistent understanding of the invention, including the scope to be given to terms, the following definitions are provided:
[0017] DNA genomic construct: As used herein, the term “DNA genomic construct” refers to the DNA that is carried by recombinant HSV-1 and which contains a variety of elements that allow for the expression of a structural sequence after the DNA is introduced into a host cell. The expression of the structural sequence is under the control of (i.e., operably linked to) regulatory sequences such as promoters or enhancers. Unless otherwise indicated, promoters may be constitutive, inducible or repressible.
[0018] Vector: The term “vector” or “viral vector” is the system for expressing a recombinant DNA sequence in a host cell. As used herein, it refers to a DNA genomic construct-containing HSV viral recombinant which can introduced said genomic construct into a host cell.
[0019] Expression: Expression is the process by which a polypeptide is produced from DNA. The process involves the transcription of a gene into mRNA and the translation of this mRNA into a polypeptide. Depending on the context in which it is used, “expression” may refer not only to the expression of polypeptide, but also to the production of RNA, particularly antisense RNA.
[0020] Promoter: A promoter is a DNA sequence that initiates the transcription of a gene. Promoters are typically found 5′ to the gene and located proximal to the start codon. If a promoter is of the inducible type, then the rate of transcription increases in response to an inducing agent.
[0021] Host cell: A host cell is the recipient of a DNA vector. Host cells may exist either in vivo or in vitro.
[0022] Recombinant: As used herein, the term “recombinant” refers to nucleic acid that is formed by experimentally recombining nucleic acid sequences and sequence elements. A recombinant host cell would be a cell that has received recombinant nucleic acid.
[0023] Operably linked: The term “operably linked” refers to genetic elements that are joined in such a manner that enables them to carry out their normal functions. For example, a gene is operably linked to a promoter when its transcription is under the control of the promoter and such transcription produces the protein normally encoded by the gene.
[0024] Structural sequence: As used herein, the term “structural sequence” refers to a sequence of nucleotides that undergoes transcription. Structural sequences may either encode a polypeptide or an antisense RNA sequence.
DETAILED DESCRIPTION OF THE INVENTION
[0025] The present invention is directed to HSV-1 vectors that can be used to express recombinant sequences in neuronal cells, especially in vivo. Expression is regulated using the tetracycline operator and repressor protein (for sequences see Postle et al., Nucl. Acid Res. 12:4849-4863 (1984); Hillen et al., Ann. Rev. Microbiol. 48:345-369 (1994); Wissmann et al., J. Mol. Biol. 202:397-406 (1988)). General methods for making vectors containing these elements have been previously described (see U.S. Pat. No. 6,444,871) and plasmids which contain the tetracycline-inducible transcription switch are commercially available (T-REx™, Invitrogen, CA). The essential features are the presence of a structural sequence (e.g., a gene sequence that one wants to be expressed in a host cell) which is operably linked to a promoter that has a TATA element. A tet operator sequence is located between 6 and 24 nucleotides 3′ to the last nucleotide in the TATA element of the promoter and 5′ to the structural sequence. When DNA with these characteristics is present in a cell that also expresses the tetracycline repressor, transcription of the structural gene will be blocked by the repressor binding to the operator. If tetracycline is introduced however, it will bind to the repressor, cause it to dissociate from the operator, and transcription of the structural gene will proceed.
[0026] The HSV-1 vectors also include at least two sequences coding for the tetracycline repressor and expression of each of these sequences is under the control of either an ICP-0 or ICP-4 immediate early promoter of HSV-1. The sequences for the ICP-0 and ICP-4 promoters and for the genes whose regulation they endogenously control are well known in the art (Perry, et al., J. Gen. Virol. 67:2365-2380 (1986); McGeoch et al., J. Gen. Virol. 72:3057-3075 (1991); McGeoch et al., Nucl. Acid Res. 14:1727-1745 (1986)) and procedures for making vectors containing these elements are described in detail in the Examples section below. These promoters are not only very active in promoting gene expression, they are also specifically induced by VP 16 a transactivator that is released when HSV-1 infects a cell. Thus, transcription from ICP-0 or ICP-4 is particularly high when repressor is most needed to shut down transcription of the structural sequence.
[0027] Vectors having the characteristics described above can be produced using standard methods of molecular biology and DNA synthesis. However, it is also possible to produce an appropriate vector by modifying the wild type HSV-1 genome. Specifically, the ICP-0 or ICP-4 genes may be deleted from the viral genome and replaced with a structural sequence in a manner that puts it under the control of the ICP-0 or ICP-4 promoter. Since the HSV-1 genome contains more than one ICP-0 or ICP-4 gene, more than one repressor element will be included in a vector. In the most preferred embodiment, two sequences coding for tet repressor are present. This provides a greater concentration of repressor for binding to the tetracycline operator and shutting off transcription.
[0028] The strength with which the tet repressor binds to the operator sequence is, preferably, enhanced by using a form of operator which contains two Op-2 repressor binding sites linked by a sequence of approximately four nucleotides. When repressor is bound to this operator, essentially no transcription of the structural sequence will occur. Many different promoters may be used for controlling the expression of the structural sequence. Examples include the mouse metallothionein I promoter (Hamer, et al., J. Mol. Appl. Gen. 1:273-288 (1982)); herpes virus promoters (Yao et al., J. Virol. 69:6249-6258 (1995); McKnight, Cell 31:355-365 (1982)); the SV 40 early promoter (Benoist, et al., Nature 290:304-310 (1981)); and, especially, the human CMV immediate-early promoter (Boshart, et al. Cell 41; 521-530 (1985)) or LAP2/hCMV immediate-early promoter (Palmer et al., J Virol 74:5604-5618 (2000)).
[0029] Once appropriate genomic DNA constructs have been produced, they may be incorporated into HSV-1 viral recombinants using methods that are well known in the art. The most preferred procedure is described in the Examples section, but other methods are also compatible with the present invention. It is preferred that the virus be replication deficient, i.e., incapable of replicating once it is introduced in vivo. Any method for producing a replication deficient virus known in the art may be used. In the case of HSV-1 the most preferred procedure is to either delete or mutate the viral UL-9 gene so that it no longer makes functional protein (for UL-9 sequence, see McGeoch, et al., J. Gen. Virol. 69:1531-1574 (1988)). Again, procedures for carrying this out are described in the Examples section and in references provided herein.
[0030] The structural sequence in HSV vectors can encode any protein or RNA sequence that one wants to express in a host cell. For example, HSV vectors in which the structural sequence codes for a marker such as LacZ may be used to study the ability of HSV-1 or another virus to deliver genes to cells in vivo and the extent to which the structural sequence is expressed after delivery. This type of evaluation is very important in the development of methods that can be used in gene therapy. Other genes, e.g., genes coding for growth factors, antisense sequences, cytokines or therapeutic agents, may also be used as the structural sequence and delivered to cells. The ability to turn on and off expression after delivery by administering or withholding tetracycline provides scientists with a way to study the effect of the expressed sequence on cell biology. It also provides a way for evaluating the therapeutic potential of a vector. For example, by studying factors that contribute to neuronal growth and development, procedures may be developed that can be used to help promote nerve regeneration in patients where tissue has been destroyed due to stroke or traumatic injury. Similarly, neoplastically transformed neurons can be targeted with vectors producing agents such as interferons or other therapeutic agents to determine whether there is an effect on tumor growth or metastasis. In addition CNS diseases such as Alzheimer's disease, Parkinson's disease, ALS, multiple sclerosis and Huntington's disease may also be studied and potential therapies for these diseases tested.
EXAMPLES
[0031] In the present example, a tetracycline-inducible transcription switch is introduced into a novel replication-defective HSV-1 vector, QR9TO-lacZ. Infection of cells with QR9TO-lacZ can achieve a 1000-fold increase in regulated gene expression by tetracycline in mammalian cells. The demonstrated ability of QR9TO-lacZ to deliver very high levels of sensitively regulated gene expression significantly expands the utility of HSV-based vector systems for the study of protein function in the nervous system and their potential in human gene therapy applications.
[0032] A. Materials and Methods
[0033] Plasmids: pSH is an ICP0-expressing plasmid with flanking sequences 957 bp upstream of the ICP0 open-reading frame to 415 bp downstream of the ICP0 translation stop codon (Cai, et al., J. Virol. 63:4579-4589 (1989)). pSH-tetR is a tetracycline repressor-expressing plasmid in which expression of tetR is under the control of the HSV-1 ICP0 promoter. It was generated by replacing the Nco I-Sal I ICP0 coding sequence-containing fragment in plasmid pSH with the Kpn I-Sal I tetR-containing fragment of pGEM-tetR (Yao, et al., Hum. Gene Ther. 9:1939-1950 (1998)). Nco I linearized pSH was blunt-ended with mung bean nuclease to remove the initiation codon, ATG, of the ICP0 open-reading frame while the Kpn I-linearized pGEM-tetR was blunt-ended by T4 DNA polymerase treatment. The HSV-1 UL9-expressing plasmid, pcDNAUL9, was constructed by inserting the BsiW I-Not I UL9-containing fragment of pL9 (Baradaran, et al., J. Virol 68:4251-4261 (1994)) into pcDNA3 at the Nru I and Not I sites. pcDNAUL9 expresses UL9 from the HSV-1 UL9 promoter with the bovine growth hormone (BGH) polyadenylation signal sequence at its 3′ end. Plasmid p9DNATO-lacZ, which contains the lac Z gene under control of the tetO-bearing hCMV major immediate-early promoter with the BGH poly A signal at the 3′ end of the lac Z gene, was generated by replacing the Xcm I-Mlu I fragment containing UL9 amino acids 217 to 803 in plasmid pUL9-V, with DNA sequences consisting of the tetO-hCMV-lacZ-poly A transcription unit (see FIG. 1 ) pUL9-V is a derivative of pcDNAUL9 with a deletion of a 17-bp Not I-Xba I fragment present in pcDNA3.
[0034] Cells: African green monkey kidney (Vero) cells and osteosarcoma cells, U20S, were grown and maintained in Dulbecco's modified Eagle's medium (DMEM) supplemented with 10% fetal bovine serum (Yao, et al., J. Virol. 69:6249-6258 (1995)). U20S cells express a cellular activity that can substitute functionally for the HSV-1 immediate-early regulatory protein, ICP0 (Yao, et al., J. Virol. 69:6249-6258 (1995)). U2CEP4R11 cells, a tetR-expressing cell line derived from U20S cells, were grown and maintained in the above-mentioned growth medium in the presence of hygromycin-B at 50 μg/ml (Yao, et al., Hum. Gene Ther. 9:1939-1950 (1998)).
[0035] RUL9-8 is a double-stable cell line expressing both tetR and UL9, which was established by stable transfection of U2CEP4R11 cells with pcDNAUL9 using procedures described previously (Yao, et al., Hum. Gene Ther. 9:1939-1950 (1998)). These cells can support the growth of an HSV-1 UL9 insertion mutant hr94 efficiently.
[0036] Rat pheochromocytoma (PC12) cells were grown and maintained in DMEM supplemented with 10% heat-inactivated horse serum (Invitrogen) and 5% heat-inactivated fetal bovine serum. For differentiation of PC12 cells, cells were seeded in PC12 cell differentiation medium (DMEM supplemented with 2% heat-inactivated horse serum and 1% heat-inactivated fetal bovine serum containing 50 ng/ml of 2.5 S NGF (Upstate Biotechnologies)) at 2×10 5 cells per dish on 60-mm culture dishes coated with collagen I for one week followed by treatment with medium containing 20 μM fluorodeoxyuridine (Sigma) to remove undifferentiated PC12 cells (Su, et al., J. Virol. 73:4171-4180 (1999)). Cells were maintained in PC 12 cell-differentiation medium for an additional 2 days prior to infection.
[0037] Viruses: The ICP0 null mutant 7134, in which both copies of the ICP0 coding sequence have been replaced by the Lac Z gene of Escherichia coli (Cai, et al., J. Virol 63:4579-4589 (1989) was propagated and assayed in U20S cells (Yao, et al., J. Virol. 69: 6249-6258 (1995)). Infectious 7134 DNA was isolated from purified 7134 virions according to procedures previously described ((Yao, et al., J. Virol. 69:6249-6258 (1995)).
[0038] KOR is an HSV-1 recombinant in which the Lac Z genes of 7134 were replaced by homologous recombination with a DNA fragment containing tetR in pSH-tetR. In brief, U20S cells were co-transfected with the linearized pSH-tetR plasmid and infectious HSV-1 7134 DNA using lipofectin (Yao, et al., Hum. Gene Ther. 9:1939-1950 (1998)). Progeny of the transfection were screened by standard plaque assay in the presence of 5-bromo-4-chloro-3-indolyl-β-D-galactoside (X-Gal) at 96 h post-infection (Yao, et al., Hum. Gene Ther. 10:1811-1818 (1999)). White plaques contain virus in which both copies of the Lac Z gene are replaced by the tetR DNA. These were isolated following four rounds of plaque purification to yield KOR. The expression of tetR in KOR was verified by Western blot analysis of cell extracts prepared from mock-infected U20S cells and from U20S cells infected with either 7134 or KOR. The tetR-specific monoclonal antibody used was purchased from Clontech, Palo Alto, Calif.
[0039] Infection and β-galactosidase Assay: Vero and PC12 cells were seeded at 1×10 6 cells per 60-mm dish. At 48 h post-seeding, Vero cells were mock-infected or infected with either 3 PFU/cell or 10 PFU/cell of QR9TO-lacZ. For PC12 cells, infections were carried out at 120 h post-seeding with either 1 or 3 PFU/cell. Infections were performed in the absence or presence of tetracycline. Mock-infected and infected cell extracts were prepared for β-galactosidase assays according the protocol described by Invitrogen (Carlsbad, Calif.). Protein concentrations in cell extracts were determined by the Pierce BCA protein assay (Pierce Biotechnology, Rockford, Ill.). β-galactosidase activity was expressed as nmoles of ONPG hydrolyzed/min/mg protein (Invitrogen). For visible X-Gal staining, at various times post-infection, cells were washed with PBS, fixed with 0.05% glutaraldehyde, and stained with X-Gal at 500 μg/ml in PBS solution containing 5 mM potassium ferricyanide and 5 mM potassium ferrocyanide.
[0040] Mice: Female CD-1 mice six to eight weeks of age were purchased from Taconic Laboratory (Germantown, N.Y.). Mice were housed in metal cages at four mice per cage and maintained on a 12-h light/dark cycle. Mice were allowed to acclimatize for one week prior to experimentation. Mice were randomly assigned to several different groups and fed with either a normal diet or a diet containing tetracycline at 6 g/kg (Bio-Serv, Frenchtown, N.J.). After 7 days of feeding, mice were anesthetized with sodium pentobarbital and inoculated either intracerebrally with 20 μl of QR9TO-lacZ into the left frontal lobe of the brain at a depth of 2.5 mm or by subcutaneous inoculation into hindlimb footpads. Mice were fed ad libitum with either a normal diet or a tetracycline-containing diet. Control mice were inoculated with DMEM. Mouse brains or footpads were harvested on days 1, 2, or 3 post-inoculation. After tissues were fixed in 4% paraformaldehyde for 2 h, they were washed with PBS and stained with X-Gal for 3 h at 37° C.
[0041] B. Results
[0042] Construction of the T-REx™-Containing Single Replication-Defective HSV-1 Vector:
[0043] To generate a replication-defective HSV-1 recombinant encoding the newly developed tetR-mediated repression switch, we first constructed a tetR-expressing HSV-1 recombinant, KOR, by replacing both copies of the HSV-1 ICP0 open-reading frame with DNA sequences encoding tetR ( FIG. 1A ). Second, to replace the essential UL9 gene of HSV-1 in KOR ( FIG. 1A ) with the Lac Z gene under control of the tetO-bearing hCMV major immediate-early promoter, we transfected UL9-expressing RUL9-8 cells with linearized p9DNATO-LacZ DNA followed by KOR super-infection. Progeny virus was plaque assayed on RUL9-8 cell monolayers in the presence of tetracycline and X-Gal. Blue plaques, indicating that the UL9 gene had been replaced by the lacZ gene, were isolated and plaque purified four times. QR9TO-lacZ ( FIG. 1B ) is a viral recombinant that exhibits strong X-Gal staining in infected Vero or U20S cells in the presence of tetracycline but little or no staining in the absence of tetracycline, indicating that the expression of Lac Z gene can be effectively controlled by tetracycline in cells infected with QR9TO-lacZ.
[0044] The replication-defective nature of QR9TO-lacZ was confirmed by plaque assays on RUL9-8, U20S, and Vero cell monolayers. The plaque-forming efficiency of QR9TO-lacZ on ICP0-complementing U20S cell monolayers was reduced more than 5×10 6 -fold compared with that in RUL9-8 cells. When assayed on non-ICP0 complementing Vero cell monolayers, the plaque-forming ability of QR9TO-lacZ was reduced to less than 1.14×10 −8 PFU/ml. Given that the plaque-forming efficiency of an ICP0 null mutant on Vero cell monolayers is reduced by more than 100-fold relative to U20S cell monolayers, the titer of QR9TO-lacZ on Vero monolayers is less than 5×10 −8 PFU/ml.
[0045] Quantitative analysis of tetracycline-regulated β-gal expression in QR9TO-lacZ-infected cells: To assess the efficiency of QR9TO-lacZ in delivering tetracycline-regulatable gene expression in mammalian cells, we compared the levels of lacZ expression following QR9TO-lacZ infection in both the presence and absence of tetracycline by quantitative β-galactosidase (β-gal) analysis. Compared with cells infected in the absence of tetracycline, levels of Lac Z expression in QR9TO-lacZ-infected cells in the presence of tetracycline were increased by 1024-fold and 541-fold at MOIs of 3 and 10 PFU/cell respectively.
[0046] An examination of tetracycline-dose-dependent regulation of β-gal expression in QR9TO-lacZ infected Vero cells, showed that levels of β-gal expression in QR9TO-lacZ infected cells can be finely adjusted by varying the dose of tetracycline. Maximum β-gal expression was detected at a tetracycline concentration of 0.5 μg/ml, which was 966-fold higher than that detected in QR9TO-lacZ-infected Vero cells in the absence of tetracycline.
[0047] Taken together, these results demonstrate that QR9TO-lacZ, a T-REx™ encoding replication-defective HSV-1 viral recombinant, is capable of delivering robust and tightly regulated gene expression to mammalian cells.
[0048] Regulation of β-gal expression in QR9TO-lacZ-infected un-differentiated and NGF-differentiated PC12 cells: In an effort to evaluate its potential application as an efficient vector for delivering regulated gene expression to neural cells, we next infected both undifferentiated and 2.5 S NGF-differentiated PC12 cells with QR9TO-lacZ in the absence and presence of tetracycline. The X-Gal staining experiments showed that, whereas very few X-Gal positive staining cells were detected in undifferentiated and NGF-differentiated PC12 cells infected with QR9TO-lacZ in the absence of tetracycline, close to 50% of undifferentiated and differentiated PC12 cells infected with QR9TO-lacZ exhibited strong X-Gal staining in the presence of tetracycline. No blue cells were observed in mock-infected cells. In addition, on the basis of the similarity of both cell density and morphology between infected cells and mock-infected controls, the study indicated that QR9TO-lacZ exhibits little cytotoxicity in infected, undifferentiated and NGF-differentiated PC 12 cells.
[0049] A quantitative analysis of β-gal expression in undifferentiated and NGF-differentiated PC 12 cells was performed after infection with QR9TO-lacZ in the absence or presence of tetracycline. It was found that a 200-fold or greater increase in tetracycline dependent induction of β-gal expression was achieved under the experimental conditions described. Infection of PC12 cells with QR9TO-lacZ at an MOI of 3 PFU/cell yielded a 669-fold increase in β-gal expression by tetracycline. The specific-β-gal activity detected in tetracycline treated QR9TO-lacZ-infected differentiated PC 12 cells at an MOI of 10 PFU/cell was nearly 300-fold higher than that detected in the absence of tetracycline.
[0050] Tetracycline-regulated β-gal expression in vivo: CD-1 mice were fed standard food or tetracycline-containing food one week prior to inoculation of the left frontal lobe or the hindlimb footpads with QR9TO-lacZ. X-Gal staining was examined in the brains of mice on days 1, 2, and 3 after inoculation of the left lobe. Direct in vivo delivery of QR9TO-lacZ led to strong X-Gal staining of tissue along the needle tract in brains of mice fed tetracycline. No X-Gal specific staining was detected in brains of mice fed standard food.
[0051] X-Gal staining was also examined in footpad tissues (n=6) of mice 48 h post-infection. For each mouse footpad, sagittal or transverse sections were cut at a thickness of 8 μm per section and every sixth section was examined for the presence of X-Gal staining. Large numbers of X-Gal positive staining cells were detected in QR9TO-lacZ-infected footpad tissues of tetracycline-treated mice. We did, however, observe a few X-Gal positive cells in footpad tissues of mice that were not fed tetracycline. These cells exhibited a staining intensity much lower than that observed in footpad tissue prepared from tetracycline-fed mice. The average number of X-Gal-positive cells from a total of 23 sections per footpad was: 0 in the mock-infected group, 6.67±6.121 in the absence of tetracycline and 813.33±777.79 in the presence of tetracycline.
[0052] C. Discussion
[0053] The hCMV major immediate-early enhancer-promoter is one of the most potent and promiscuous cis-regulatory elements used for enhancing expression of transgenes in both in vitro and in vivo. By inserting the tetracycline operator such that the first nucleotide is positioned 10 bp downstream of the last nucleotide of the TATATAA element (TATA element) of the hCMV major immediate-early promoter, we have shown that the tetracycline repressor (tetR) can act as a potent repressor to down-regulate gene expression from the tet operator-bearing hCMV major immediate-early promoter. It was shown that gene expression from the tetracycline operator-bearing hCMV major immediate-early enhancer-promoter can be regulated by tetR over three orders of magnitude in response to tetracycline, whereas in the absence of tetR, the tetO-bearing hCMV major immediate-early enhancer-promoter exhibits the same promoter activity as the wild-type promoter.
[0054] In the present example, two specific strategies were used for introducing the tet-On gene switch into a replication-defective HSV-1 vector. First, based on the fact that the efficacy of T-REx™ in achieving regulation of gene expression is influenced by the levels of tetR within cells and that the HSV-1 immediate-early ICP0 promoter is one of the strongest HSV-1 immediate-early promoters whose activity is significantly enhanced by the virion-associated transactivator VP16, we constructed an HSV-1 recombinant, KOR, encoding two copies of the tetR gene by replacing the ICP0 gene with DNA encoding tetR under control of the ICP0 promoter. This design allows high level of expression of tetR upon virus entry into the cell. Second, given that a combination of the deletion of ICP0 gene with the blockage of HSV-1 viral DNA replication by the dominant-negative HSV-1 UL9 origin binding protein, UL9-C535C, significantly reduces the cytotoxicity of the resulting recombinant as compared with HSV-1 recombinants with a deletion in genes encoding ICP4 or ICP27, we replaced the essential UL9 gene in KOR with DNA encoding the Lac Z gene under control of the tetO-containing hCMV major immediate-early promoter, which renders the resulting recombinant, QR9TO-lacZ, replication-defective in non-UL9 complementing cells. Notably, since QR9TO-lacZ is propagated in non-ICP0-transformed ICP0-complementing UL9-expressing cells, there should be no concern about potential generation of a viral recombinant that contains the wild-type ICP0 gene, which plays a major role in enhancing reactivation of latent HSV.
[0055] Analysis of QR9TO-lacZ infection of Vero cells, PC12 cells, and NGF-differentiated PC12 cells revealed a 300- to 1000-fold enhancement in gene expression by tetracycline in these cells. We also showed that expression of the lac Z gene in QR9TO-lacZ-infected cells can be controlled by tetracycline in a dose-dependent manner. This highly efficient means of regulating gene expression can also be achieved in vivo following intracerebral and footpad inoculations in mice, demonstrating its potential utility for regulating gene expression in gene therapy applications and analysis of gene function in the nervous system.
[0056] Although available evidence indicates that long-term gene expression can be achieved with the hCMV major immediate-early promoter in replication-defective HSV-1 vectors following intra-articular delivery in rabbits and injection into inguinal adipose tissue in mice, gene expression from the hCMV-immediate-early promoter is generally suppressed in latently infected neurons following HSV vector-mediated gene transfer. This shortcoming can, however, be overcome with the use of the LAP2/hCMV immediate-early promoter, a hybrid promoter between the HSV-1 latency-associated promoter LAP2 and the hCMV major immediate-early promoter. It has been demonstrated that HSV-1 recombinants containing the LAP2/hCMV immediate-early promoter can yield efficient long-term transgene expression in latently infected neurons (Palmer, et al., J. Virol. 74:5604-5618 (2000)). Thus, for achieving potential long-term regulatable gene delivery to the CNS, a QR9TO-lacZ-like HSV vector could be constructed, in which the expression of a target gene is controlled by the tetO-bearing LAP2/hCMV immediate-early promoter, while the tetR gene is under control of the LAP2/hCMV immediate-early promoter, or a hybrid promoter between LAP2 and an HSV-1 immediate-early promoter.
[0057] All references cited herein are fully incorporated by reference. Having now fully described the invention, it will be understood by those of skill in the art that the invention may be practiced within a wide and equivalent range of conditions, parameters and the like, without affecting the spirit or scope of the invention or any embodiment thereof. | The present invention is directed to HSV-1 vectors which rely on the tetracycline repressor and operator as a means for regulating expression. The vectors utilize VP-16 responsive promoters of HSV to control expression of the tetracycline repressor. The vectors are of particular interest as vehicles for recombinantly expressing genes in vivo. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to process machinery, and more particularly to machinery for the continuous manufacture of a web of multilayer material, such as asbestos.
2. Prior Art
Asbestos sheet is an item necessary for the manufacture of gaskets, brake pads, scuff plates, insulation and the like, all necessary for the functioning of our modern society. This modern society however, has also dictated safety standards for the production of such goods containing asbestos, because of its possible toxicological properties. These properties include the presence of fines and fumes which may be harmful to the operators of the machines which are currently utilized to make asbestos sheet. One of the machines which presently manufacture sheets of asbestos is generally comprised of a large roll onto which the asbestos fiber is fed. After a suitable accretion and curing of the fibers, the machine operator makes an axially directed cut through the build-up of fibers on the roll of the machine. The roll is then turned, and a single sheet is pulled (and scraped) off the roll. This is a time consuming method and involves a potentially dangerous operation because it involves close operator attention and contact, and creates atmospheric fines when the sheet is cut on the roll. Other examples of the prior art manufacture of asbestos sheet or other web material are shown in U.S. Pat. Nos. 3,770,569; 2,055,412; 3,967,043; 3,861,971 and 3,197,529.
BRIEF SUMMARY OF THE INVENTION
The present invention comprises a machine capable of manufacturing a continuous multilayered webbed article, such as a continuous sheet of asbestos. The machine comprises an endless conveyor belt horizontally arranged about a pair of rolls, at least one of which is powered. A plurality of hoppers are sequentially arranged above the top side of the upper run of the conveyor belt. The hoppers are filled from their top portions and discharge the material out an opening in their bottom portion. Each hopper has a rotatable vaned spreader across the opening in its bottom portion. Immediately downstream of each hopper, there is disposed a pair of nip rollers. One roller being arranged beneath the upper run of the conveyor belt, and the other roller being adjustably arranged across the top of the upper run of the conveyor. The nip rollers provide the pressure to any material which is dispersed across the belt from the hoppers. The entire machine is enclosed and is provided with forced hot air within the enclosure at the downstream end of the conveyor belt. The hot air helps process the asbestos sheet during its manufacture. A suction fan is disposed at the upstream end of the conveyor belt, to trap toxic fumes and fines generated during the manufacturing of the asbestos sheet and to recycle those toxic materials within the closed manufacturing system. The webbed material is scraped off the top of the conveyor belt at its downstream end, is passed out a door in the enclosure, onto a line of conveyor rollers, thus providing a continuum of safely manufactured product, which in the preferred embodiment is a continuous sheet of asbestos.
BRIEF DESCRIPTION OF THE DRAWING
The objects and advantages of the present invention will become more apparent when viewed in conjunction with the following drawing in which:
FIG. 1 is a side view of a continuous sheeter machine with portions of its side wall removed for clarity.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to FIG. 1, there is shown a continuous sheeter machine 10, comprising an endless conveyor belt 12 disposed about a horizontally arranged rotatively disposed drum 14 on a frame portion 15 of the sheeter machine 10 at its upstream end. The conveyor belt 12 is also arranged about a horizontally disposed drum 16 rotatively disposed on the frame 15 at its downstream end of the sheeter machine 10. The conveyor belt 12 has an upper run 18 and a lower run 20, which define the build-up path for the product, and the return path for the unloaded conveyor belt 12, respectively. The upstream drum 14 is rotatively powered by a motor 22 connected therebetween by a drive chain 24. The downstream drum 16 is adjustably arranged on the machine frame 15 by interconnection with a pair of belt tensioning arms 26, only one being shown. Each arm 26 is supported at one end, at the frame 15, and at the other end, to a bearing 28 rotatively supporting a journal 30 on each side of the downstream drum 16. Each arm 26 is longitudinally adjustable to vary the tension in the conveyor belt 12.
A plurality of feed hoppers 32 are sequentially disposed above the upper run 18 of the conveyor belt 12 and in one utilization, may be filled with various toxic or otherwise hazardous feed mixes of asbestos and latex. The feed hoppers 32 each have a generally rectangular opening 34 at their lowermost portions. The openings 34 extend across the width of the conveyor belt 12. The feed hoppers 32 each have an upstream and a downstream wall 36 and 38, slanted so as to permit efficient flow of feed through the openings 34. A spreader 40 is rotatively arranged along the length of the opening 34. The spreader 40 has blades or vanes which aid in the proper mix and distribution rate of the feed material through the opening 34 and onto the conveyor belt 12.
An upper and a lower arrangement of nip rolls 42 and 44 are rotatively disposed immediately downstream of the downstream wall 38 of each feed hopper 32. The upper nip roll 42 is disposed across the top side of the upper run 18, and the lower nip roll 44 is juxtaposed with respect to the upper nip roll 42, across the bottom side of the upper run 18. The upper nip roll 42 may be cooled with a flow of chilled water, down to a temperature of about 45° F., the chilled water entering and leaving the roll 42 through rotary joints, on each end thereof, not shown, by means well known in the art. The lower nip roll 44 may be heated up to a temperature of about 250° F. by steam entering and leaving the roll 44 through a similar arrangement of rotary joints. The lower nip roll 44 may be rotatively connected with the spreader 40 by a chain 50, belt or the like. The connection between the lower nip roll 44 and the spreader 40 maintains the proper speed of rotation of the spreader 40 in relation to the speed of the belt 12 and the nip rolls, 42 and 44. The upper and lower nip rolls 42 and 44, are also rotated by means, not shown, such as by motors or by engagement means with the conveyor belt 12 to maintain their rotative speed to correspond or be compatible with the linear speed of the conveyor belt 12. Each of the upper nip rolls 42 may be adjustable in the heightwise direction by any suitable means such as a regulatable pressurizable cylinder arrangement 52 journalled at each end of the upper nip roll 42. The pressures in the cylinder arrangements 52 may be governed by connection with a proper regulatable pressure source, not shown. The heightwise adjustment of the upper rolls 42 by the pressurizable cylinder arrangements 52 permits variation in/or maintenance of constant accretion in thickness of the accumulating product as it travels downstream on the conveyor belt 12. The pressurizable cylinder arrangements 52 also permit adjustment of the nip pressure which is preferably about 800 lbs. per linear inch of roll length in the application shown but which may be varied to suit the materials being processed.
A forced hot air system 60 may be arranged roughly parallel to the upper run 18 of the conveyor belt 12. The hot air system 60 includes a blower 62 arranged to blow controlled temperature air (which may be heated to a temperature of about 300° F., depending on the material being processed), through a duct network 64, only partially shown, having a plurality of vents 66 that extend partway over the conveyor belt 12 and are adapted to jet the hot air onto the feed material on the conveyor belt 12, between successive arrangements of the nip rolls, 42 and 44. A suction fan 70 is disposed at the upstream end of the sheeter machine 10 to draw off toxic fines and fumes from the feed hoppers 32 and as they are produced from the curing of the feed material on the conveyor belt 12. The entire continuous sheeter machine 10 is disposed in an environmentally safe containment enclosure 76. The enclosure 76 has an exit orifice 78 to permit the suction fan 70 to fully withdraw the toxic vapors and later to filter them, scrub, and prepare them, by means not shown, for recycling which may be within the continuous sheeter machine. The top of the enclosure 76 has a plurality of door means 77 which permit the filling of the hoppers 32 with the necessary feed material. The doors are sealed when closed to prevent contamination of the outside atmosphere during machine operation. The downstream end of the enclosure 76 has a flap door 79 which permits egress of the finished product, asbestos sheet in this case, onto a roller belt, after it is scraped off of the downstream drum 16 by a scraper blade 80.
In operation of the continuous sheeter machine 10 for producing asbestos sheet, the feed hopper 32, as shown to the left on FIG. 1, (the most upstream hopper) is filled through the sealable door means 77 in the top of the enclosure 76, with almost pure latex or uncured rubber. Successive downstream hoppers may be filled through similarly arranged doors 77 with about 15% latex and about 85% asbestos fibers. The last most downstream hopper would be filled with almost pure latex. Materials such as ground ceramic particles, e.g. silica, calcium carbonate, or clays such as alumina, barium sulfate, may be mixed with or substituted for the asbestos fibers, and plastics such as PVC may be used in place of latex to manufacture other continuous sheets of gasket-like material on the present invention. This premix of fibers and rubber compounds, or their substitutes, are deposited and built-up on the conveyor belt 12, during machine operation, by about 0.003"-0.006" of material, from each successive hopper 32. The mix of material is heated by the jets of hot air coming from the duct network 64 arranged between successive arrangements of nip rolls, 40 and 42. The hot air keeps the asbestos mix hot and workable. The upper rollers 40 are cooled during the manufacturing operation to prevent the asbestos sheet from sticking to them.
The suction fan 70 draws off the vapor solvents from the operation, and carries those vapors such as naphtha, toluene and the like, to a filter bed, not shown, and to scrubbers, also not shown, where the vapors are condensed for reuse. The complete enclosure 76 confines these vapors and permits the manufacture of continuous sheets of asbestos or other material without substantially exposing operators to potentially hazardous conditions.
An alternative embodiment of the present invention includes a hugger belt 90 with an arrangement of rotatable support rollers 92 which support the hugger belt along the bottom side of the lower run 20 of the conveyor belt 12. The hugger belt 90 may be used to bring a length of asbestos sheet around the conveyor belt 12 additional times to incrementally build up its thickness as it passes beneath the hoppers 32 and receives their discharge before being scraped off by the scraper blade 80.
Though the invention has been described with a degree of particularity, it is intended that the appended claims be interpreted as exemplary only, and not in a limiting sense. | A machine for the continuous manufacture of a multilayer toxicogenic web material, such as asbestos. The machine includes a series of controlled feed units sequentially arranged above a continuous conveyor belt to serially deposit incremental layers of asbestos and oil products on the conveyor belt to form a thick, continuous sheet which is removed after proper curing, from the downstream end of the conveyor belt by a doctor blade. The machine is housed in an environmentally safe containment enclosure to prevent escape of potentially harmful material therefrom. | 3 |
This non-provisional application is a continuation and claims the benefit of U.S. application Ser. No. 09/795,629, filed Feb. 28, 2001, now U.S. Pat. No. 6,832,050 which claims the benefit of Provisional Appl. Ser. No. 60/219,355, filed Jul. 19, 2000 and Provisional Appl. Ser. No. 60/267,724, filed Feb. 12, 2001.
FIELD OF THE INVENTION
The present invention relates to the field of optical communications systems and particularly to a method for reduction or elimination of timing jitter and amplitude jitter occurring in transmission of Return-to-Zero (RZ) modulated pulses by use of optimum amount of pre-chirp.
BACKGROUND OF THE INVENTION
Transmission of optical pulses based on RZ modulation is emerging as the best choice in high bit rate and/or long distance systems. However, the pulses suffer from nonlinear intra-channel effects, which lead to timing jitter and amplitude jitter. Timimg jitter and amplitude jitter weaken the performance and limit the maximum capacity of each channel.
SUMMARY OF THE INVENTION
Dispersion describes how a signal is distorted due to the various frequency components of the signal having different propagation characteristics. Specifically, dispersion is the degree of scattering in the light beam as it travels along a fiber span. Dispersion can also be caused by the frequency dependence of the group velocity of a light signal propagating inside a fiber.
The intricate interplay of nonlinearity and dispersion acting on pulses in optical fibers continues to challenge the conventional wisdom and established intuition. One example is the idea that short duty-cycle RZ transmission in dispersive fibers is able to combat the detrimental effects of fiber nonlinearity. Due to their short width, the pulses disperse rapidly, spreading in time over hundreds or thousands of bits. Theory, simulations and experiments in the prior art uniformly show that with shorter pulses the nonlinear impairments are reduced. This may seem somewhat counter-intuitive since the reduction of the pulse width is inevitably accompanied by an increase in the pulse peak power and an increase in the impact of self-phase modulation (SPM) may be expected. SPM causes compression in the pulse. The reason for the reduction is not merely that the individual peak power is reduced by dispersion. In a random bit sequence the intensity pattern of the interfering pulses contains spikes that are of the same order of magnitude as the input peak power. The reduced peak power is, therefore, not a viable explanation. Rather, the mechanism for the tolerance towards nonlinear impairments relies on the fact that the intensity pattern changes very rapidly. Thus, the accumulated effect of the instantaneous nonlinearity tends to get averaged out and SPM and nonlinear pulse interaction is reduced even though the pulses spread over hundreads of neighboring time slots. The concept of spreading the pulses as far as possible and as quickly as possible in the time domain, creating a rapidly varying intensity pattern, in order to combat the impact of nonlinearity, represent such a big shift from standard dispersion managed approaches that a specific term “tedon-transmission” has been coined to represent this scheme.
System penalties are generated in the form of timing and amplitude jitter, which limit the performance of such systems. It may be useful to note that the scheme presented herein is fundamentally different from schemes, which rely on soliton transmission where the pulses usually do not spread over more than tens of bits.
Analysis of the nonlinear pulse interaction in systems based on highly dispersed optical pulses provides estimates of timing and amplitude jitter. The pulse streams are both coherent and non-coherent. Analysis of the nonlinear intra-channel effects indicate that the non-linear effects possess a symmetry when pre-chirped pulses are launched. System penalties reduce montonically with decreasing pulse width and with increasing fiber dispersion. Proper dispersion pre-compensation can result in a significant reduction of the nonlinear impairments. Optimal pre-compensation can be determined analytically.
It is, therefore, an object of the present invention to minimize timing jitter by injecting the proper amount of pre-chirp into the communications link.
A further object of the present invention is to minimize amplitude jitter by injecting the proper amount of pre-chirp into the communications link.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is best described with reference to the detailed description and the following figures, where:
FIG. 1 a shows the timing jitter as a function of position along the link with 4 dBm average input power.
FIG. 1 b shows the effect of pre-compensation on timing jitter at the link output for average input powers of 4 dBm, 7 dBm and 10 dBm.
FIG. 1 c shows the amplitude jitter at the link output as a function of the pre-compensation parameter with the average input powers of 4 dBm and 7 dBm.
FIG. 1 d shows the mean energy in the time slots corresponding to logical zeroes for average input powers of 4 dBm and 7 dBm.
FIG. 2 (top) illustrates timing jitter versus link length and (bottom) shows eye diagrams captured at points marked in the top of the figure.
FIG. 3 is a simple flowchart of the steps to reduce timing and amplitude jitter.
FIG. 4 is a simple block diagram of an exemplary implementation of a system for reducing or eliminating timing and amplitude jitter.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention concentrates on timing and amplitude jitter as well as the energy of pulses generated in time slots corresponding to logical zeroes. Analytical estimates of timing and amplitude jitter in systems based on highly dispersed optical pulses can be obtained. System penalties reduce monotonically with decreasing pulse width and with increasing chromatic dispersion. There is a qualitative difference between the phase coherent case, when there is a fixed relationship with the pulse stream, and the incoherent case, where the phase relation between pulses is random. The two cases are equivalent in terms of the timing jitter but differ significantly in terms of the amplitude jitter and the noise of the zeroes. In the coherent case there is a larger noise on zeroes but the amplitude jitter can be minimized by quasi-symmetric dispersion compensation. In the incoherent case, the noise on zeroes is lower but no improvement in the amplitude jitter can be obtained by manipulating the dispersion compensation scheme.
In the case of RZ modulation with Gaussian shaped pulses propagating in a sequence of lossy, dispersive fiber spans with periodic amplification and further assuming highly dispesive pulses for 40 Gbits/s over 800 km conventional single mode fiber, where the dispersion compensation is applied at the receiver as opposed to span by span the expressions for timing and amplitude jitter can be derived. The derivations of the expressions for the timing and amplitude jitter rely only on the assumptions that are inherent to the perturbational approach. Assuming a random sequence of Gaussian shaped pulses at the system input
∑ n = - ∞ ∞ m n u n ( 0 , t ) ,
where m n is equal to 0 or 1 with probability of 0.5, and where u n (0,t)=A 0 exp(−0.5(t−nT) 2 /τ 2 ) with T=1/B, B being the data rate and averaging over all possible two-pulse interactions yields the following result:
std ( t 1 ) B=C 1 γP av τ 3/2 √{square root over ( B/|B 2 |)} (1)
where std(t 1 ) denotes the standard deviation of the temporal pulse position, defined as the position of the center of mass of the pulse t 1 =(1/E 1 )∫t|u n (L,t)| 2 dt, E 1 =√{square root over (π)}A 0 2 τ is the energy of the pulses, P av =E 1 B/2 is the average power of the signal, γ is the nonlinearity coefficient, τis the full width at half maximum of the pulse and B 2 is the dispersion coefficient. Because of the linearization approximation, and of the large number of pulses interacting with any given one, the temporal pulse position is also found to be Gaussian distributed. The term C 1 , which is a cumbersome function of both the chirp parameter of the injected pulses and of the fiber loss coefficient, is a proportionality coefficient given by:
C 1 2 = 2 2 π I 1 ( 2 )
where
I 1 = ∫ - z * L - z * ⅆ z ∫ - z * L - z * ⅆ z ′ zf ( z + z * ) z ′ f ( z ′ + z * ) ( z 2 + z ′2 ) 3 / 2
f(z) is the ratio of the average power at z and the power at the input of the line and L is the link length. The term z* denotes the portion of the fiber length whose dispersion is pre-compensated for at the transmitter side. The reason for including only two pulse interactions in the averaging that led to equation (1) is that, as shown in the prior art, only cross phase modulation contributes to timing jitter. An analytical expression for C 1 can be obtained in the simplified case of a lossless fiber, where f(z)=1 so that C 1 2 =2√{square root over (2/π)}[2√{square root over ((L−z*) 2 )}+z* 2 −√{square root over (2)}(|L−z*|+|z*|)]. This expression can be used in equation (1) after replacing P av with the path averaged optical power to obtain an order-of-magnitude estimate of the timing jitter. This suggests that the growth of the timing jitter is approximately proportional to the square root of the length of the link. Note the strong dependence of timing jitter on the launched pulse width, which stresses the advantage of using short pulses. Additionally, the dependence on the dispersion coefficient exposes the advantage of high dispersion fibers in this transmission scheme. That is, in order to minimize the timing jitter, the optimum amount of pre-chirp is found by means of minimizing, by variation of z*, the integral I 1 , which is defined above.
Since timing jitter is generated by cross-phase modulation, which is an incoherent process, equations (1) and (2) hold regardless of the phase relationship between the transmitted pulses. In order to analyze intensity impairments the cases of phase coherence and phase incoherence need to be explicitly separated. The phase coherent case occurs when the pulses originate from a single mode locked laser or from a continuous wave (CW) laser whose intensity is externally modulated. This applies to most cases of electrical time-division multiplexing (ETDM). The phase incoherent case prevails typically when the launched pulse stream originates from more than one source laser as in the case of optical time-division multiplexing (OTDM).
In the case of phase coherence, equally spaced pulses have an equal phase difference between them. The standard deviation of the pulse energy divided by the mean energy of ones, which are referred to as amplitude jitter, is obtained from the following expression:
std ( E 1 ) E 1 = C 2 γ P av τ , ( 3 )
where C 2 is a proportionality coefficient depending only on B, z* and the fiber parameters and not on the average power P av , nor on the pulse width τ. The proportionality coefficient may be obtained as an average over the tranmsitted message of all three pulse interactions yielding a cumbersome expression. An appropriate expression can be obtained in the asymptotic case where |B 2 |LB 2 >>1, yielding
C 2 2 ≅ 8 log ( B 2 LB 2 ) 3 B 2 I 2 , ( 4 )
where
I 2 = ∫ 0 L ⅆ z f ( z ) 2 - ∫ - z * L - z * ⅆ z f w ( z + z * ) f w ( - z + z * )
and f w (z)=f(z)rect(z;0, L), with rect(z;0, L) being a function which is 1 for 0≦z≦L and zero elsewhere. The approximation leading to equation (4) involves the disregard of the correlation between contributions of different three pulse interactions to amplitude jitter. This disregard is justified by the large number of interacting pulses in this scheme. Similarly to the timing jitter, the amplitude jitter decreases with increasing dispersion or decreasing pulse width. Its dependence on pulse width is, however, more moderate. The approximate expression for C 2 allows for optimization of the pre-compensation parameter z* for the minimization of the amplitude jitter.
That is, in order to minimize the amplitude jitter, the optimum amount of pre-chirp is found by means of minimizing, by variation of z*, the integral I 2 , which is defined above.
The minimization of these integrals (I 1 and I 2 ) can be performed accurately and quickly with standard numerical techniques. Heuristic, simplifying approximations are also available. It is beneficial to use any amount of pre-chirp in a range around the optimum amount. In systems with symmetric power evolutions, the optimum amount of pre-chirp is close to half of the total dispersion in the link. Since, however, it may be shown by numerical evaluations of I 1 and I 2 that I 2 is more sensitive to the amount of pre-chirp and that with the amount of pre-chirp that minimizes I 2 the quantity I 1 is also very close to its minimum value, the optimization of the link for that concerns both amplitude and timing jitter is performed by using the amount of pre-chirp that minimizes I 2 .
In the particular case of a link made of n lossy fiber segments of length z 0 (L=nz 0 ) and lumped amplification with Erbium amplifiers, the procedure of the present invention can be followed analytically. In this case, f(z)=exp[−α mod(z,z 0 )], where α is the fiber loss coefficient and mod(z, z 0 ) is the remainder of the division of z by z 0 , and the minimum value for C 2 is obtained for
z opt * = nz 0 2 - n ( α z 0 - 1 ) + ( n - 1 ) exp ( - α z 0 ) 2 α [ n - ( n - 1 ) exp ( - α z 0 ) ] . ( 5 )
For the above expression to be valid, z opt *≦(nz 0 )/2 should be consistently verified that it is large enough and that αz 0 is realistic. The point of zero accumulation dispersion z opt * always precedes the center of the line by less than half a span length. An evaluation of C 1 , shows that the timing jitter for z*=z opt * is also very close to its minimum.
Similarly, the mean energy of the echo pulses appearing in the time slots corresponding to logical zeroes (in the phase coherent case) can be expressed as
mean ( E 0 ) E 1 = ( C 3 + C 4 ) γ 2 P av 2 τ 2 , ( 6 )
where once again the terms C 3 and C 4 are proportionality coefficients depending only on B, z* and the fiber dispersion parameters. Using the same approximations as in the derivation of (6) in the asymptotic regime |B 2 |LB 2 >>1, C 3 and C 4 are given by
C 3 ≅ π 3 12 B 2 [ ∫ 0 L ⅆ zf ( z ) ] 2 ,
C 4 ≅ 4 log ( B 2 LB 2 ) 3 B 2 ∫ 0 L ⅆ z f ( z ) 2 .
The power of the echo pulses is independent, within the variability of the approximations, of the pre-compensation, z*, whereas both timing and ampitude jitter strongly depend on it.
In the phase incoherent case in which the phase of the transmitted pulses is random, there is a random phase relation between the contribution of the nonlinear interaction and the transmitted pulse at a given time slot. A general relation between the amplitude jitter and the average power of the echo pulses at the position where a logical zero is transmitted is found as follows:
std ( E 1 ) E 1 = 2 3 [ mean ( E 0 ) E 1 ] . ( 9 )
Asymptotically, for |B 2 |LB 2 >>1, the energy of the echo pulses is still described by equation (6), only with C 3 =0, as certain phase sensitive contributions are averaged out. Since C 3 >0 this implies that the energy of the echo pulses at zeroes is always smaller in the phase incoherent case. To understand the amplitude jitter of ones, equation (6) with C 3 =0 can be inserted into equation (9) which shows that the amplitude jitter is given exactly by equations (3) and (4), only without the second integral in the square brackets of equation (4). Since the value of this integral is always non-negative the amplitude jitter in the incoherent case is equal to or larger than in the case of phase coherent pulses. Based on the above, the pre-compensation of the signal in the incoherent case has no effect either on the amplitude jitter or on the average energy of zeroes.
To confirm the theoretical results a comprehensive series of simulations have been performed and are presented herein using a 40 Gb/s Pseudo Random Bit Sequence (PRBS) consisting of 2.5 ps wide Gaussian shaped pulses is injected into 10×80 km spans of standard single mode fiber (SMF) with B 2 =−21.67 ps 2 /km, γ=1.2W −1 km −1 and α=0.048 km −1 . The simulations were performed with a time window equivalent to 2048 symbols. This large time window was necessary, since with the parameters the number of overlapping pulses was as large as 1500. Other simulations using a shorter time frame consisting only of 512 symbols led to deviations on the order of 30% in the computation of the timing jitter. FIG. 1 a shows the timing jitter as a function of position along the link with 4 dBm average input power. Both the theoretical expression (1) and the simulation results are displayed for two values of pre-compensation z*=0 and z*=z opt *=370 km. There is a noticeable large advantage of optimal pre-compensation, leading to a reduction by a factor of 4.55 in the resulting timing jitter. The effect of pre-compensation on timing jitter at the link output is shown in FIG. 1 b for average input powers of 4 dBm, 7 dBm and 10 dBm. The results are normalized to the average launched power. The fact that the points obtained with the three powers nearly overlap in the figure confirms the validity of the pertubational approach up to these powers. The amplitude jitter at the link output is shown as a function of the pre-compensation parameter in FIG. 1 c with the average input powers of 4 dBm and 7 dBm. The theoretical prediction for z opt * in the coherent case is in agreement with the simulation results. In the incoherent case there is a larger amplitude jitter and its value is practically independent of the pre-compensation parameter. The mean energy in the time slots corresponding to logical zeroes for average input powers of 4 dBm and 7 dBm is plotted in FIG. 1 d . Its dependence on the value of pre-compensation is negligible as expected, and its value is smaller in the incoherent case.
The effect of pre-dispersion, which is at the root of the present invention, is most clearly observed and understood when the power profile along the fiber is symmetric about the center of the link. This symmetry can be obtained, at least approximately, by introducing Raman amplification with a counter-propagating pump (or pumps). In such cases both the timing and amplitude jitter can be canceled out by equally splitting the dispersion compensation between the input and output of the optical link, as it can be shown that both I 1 , and I 2 are zero for z*=z opt *=L/2. It has been shown that the present invention, however, permits optimization of the amount of predispersion to yield a significant reduction of the transmission penalties in more realistic cases when the power profile is not perfectly symmetric.
To demonstrate this effect FIG. 2 shows three different sets of simulations, where we used 4 ps pulses with an average power of 7 dBm. In the top figure only the timing jitter is plotted against the link length. The amplitude jitter has a similar evolution. The triangles show the timing jitter in a lossy link with Raman amplified fiber spans of 80 km, and without pre-dispersion. The Raman pump power was chosen such that the fiber losses were compensated in each span. The asterisks show the timing jitter for the same link, but where the pulses are pre-dispersed by −2720 ps/nm. In this case, the pulses are transform-limited at 160 km where the penalties are maximal and after 320 km the penalties are minimized. The circles demonstrate the exact cancellation of the timing jitter in a lossless fiber link and after pre-dispersion by 2720 ps/nm. The power in the lossless case was set to the average power in the Raman amplified cases.
In the three cases eye-diagrams have been detected at 320 km. These are indicated in FIG. 2 (at points marked 1 – 3 ). It is clear that the penalties are eliminated in the ideal lossless case and that the penalties in the Raman amplified link are reduced because of the pre-dispersion.
The simulations presented in FIG. 2 herein assumed a single Raman pump. Multiple pumps can, in principle, further improve the symmetry of the link so that better cancellation of the penalties can be expected. Note the similarity with the cancellation of the impairments due to optical nonlineadties obtained by mid-span spectral inversion. Both require a symmetric power profile. It is, however, surprising that in the present case this result is obtained only by a proper dispersion management of the link.
Analytical formulae, simulations and a method for overcoming timing and amplitude jitter in systems based on ultra short pulse transmission have been presented. Additionally, it has been shown that the system penalties reduce monotonically with increasing fiber dispersion as well as with decreasing pulse width. Further, it has been shown that the combination of counterpropagating Raman amplification and proper predispersion of the optical pulses enables a significant reduction of the impairments. The method works equally well without Raman amplifier, permitting the reduction of timing and amplitude jitter also when lumped amplification with Erbium amplifiers is used.
In summary, nonlinear impairments due to intrachannel interactions in schemes involving ultrashort pulse (tedon) transmission with random bit sequences have been studied. The amount of timing jitter, amplitude jitter of logical ones and the mean noise on the level of logical zeroes have been presented. The analysis shows the advantage of using short pulse widths and fibers with large chromatic dispersion. It has been further shown that optimal pre-compensation allows significant reduction of timing and amplitude jitter in phase coherent cases.
FIG. 3 is a simple flowchart of the steps to follow to reduce or eliminate timing and amplitude jitter. Means for measuring total dispersion of a transmission fiber link and are known in the art. Computing devices including processors and system as well as Application Specific Integrated Circuits (ASICs), Field programmbale Gate Arrays (FPGAs), Reduced Instruction Set Computers (RISCs), or any combination thereof or any similar device designed for performing the computations specified herein, can be used to implement the computation of the optimal pre-chirp and therefore, provides a means for performing the computation. The specified computation of optimal pre-chirp may even be computed using a high-end pocket calculator or computer. Two devices are used, one at the input of the transmission fiber and the other at the output of the transmission fiber. Dispersion is added to the signal opposite in sign to the dispersion of the transmission fiber. The two devices may be fibers, gratings or any other device used for this purpose. The two devices for dispersion compensation should, however, be designed such that the device at the input adds dispersion −z opt *B 2 and the device at the output adds −(1−z opt *)B 2 , where B 2 is the total dispersion of the link.
FIG. 4 represents a simple block diagram of an exemplary implementation of a system to reduce or eliminate timing and amplitude jitter. The box to the far left with a “T” represent a transmitter. The trnasmission fiber, which may have a plurality of in-line amplifiers, is represent by the letters “TF”. The box to the far right with the letter “R” represents the receiver. The dispersion compensation devices are represented by “(a)” and “(b)”, with “(a)” being the dispersion compensation device at the input of the transmission fiber and with “(b)” being the dispersion compensating device at the output of the transmission fiber. The amounts of dispersion to be added to the input and the output of the tranmission fiber is as specified above in the description of FIG. 3 .
The present invention may be implemented in hardware, software or firmware as well as Application Specific Integrated Circuits (ASICs) or Field Programmable Gate Arrays (FPGAs) or any other menas by which the functions and process disclosed herein can be effectively and efficiently accomplished or any combination thereof. The above means for implementation should not be taken to be exhaustive but merely exemplary and therefore, not limit the means by which the present invention may be practiced.
It should be clear from the foregoing that the objectives of the invention have been met. While particular embodiments of the present invention have been described and illustrated, it should be noted that the invention is not limited thereto since modifications may be made by persons skilled in the art. The present application contemplates any and all modifications within the spirit and scope of the underlying invention disclosed and claimed herein. | A system and method for reducing timing and amplitude jitter in trnasmission of Retrun-to-Zero modulated pulses is described. In the reduction of amplitude jitter the modulated pulses must be phase coherent. The method comprises the steps of measuring a total dispersion of a transmission fiber link, computing an optimal amount of pre-chirp to be added at an input of said transmission fiber link, computing an optimal amount of pre-chirp to be added at an output of said transmission fiber link, adding said optimal amount of pre-chirp to said input of said tranmisssion fiber link and adding said optimal amount of pre-chirp to said output of said tranmisssion fiber link. The system for reducing timing jitter in transmission of Return-to-Zero modulated pulses comprises means for measuring a total dispersion of a transmission fiber link, means for computing an optimal amount of pre-chirp to be added at an input of said transmission fiber link, means for computing an optimal amount of pre-chirp to be added at an output of said transmission fiber link, means for adding said optimal amount of pre-chirp to said input of said transmission fiber link and means for adding said optimal amount of pre-chirp to said output of said transmission fiber link. | 7 |
This application is a continuation of application Ser. No. 07/529,996, filed May 3, 1990, now abandoned.
FIELD OF THE INVENTION
The present invention relates to a power steering system for an outboard motor, and more particularly to a system having an improved power unit for applying a steering assist force to a manual steering system, and for suitably controlling the steering assist force.
BACKGROUND OF THE INVENTION
A conventional manually operative steering system of an outboard motor exhibits a significant problem, such as, for example, the fact that the steering load increases, which may result in difficulty in performance of the steering operation, in accordance with navigation conditions, such as, for example, wind or wave conditions, hull speed, trim angle of the outboard motor body and the like.
In order to obviate the problem encountered with the conventional manual steering system, a hydraulic power steering system has been proposed.
The proposed hydraulic power steering system is generally composed of the manual power steering system and a power unit equipped with a hydraulic pump for generating a steering assist force. The power unit applies the steering assist force to the manual power steering system.
However, the hydraulic power steering system described above utilizes the power source of the outboard motor itself as the power source of the hydraulic pump. Accordingly, the steering assist force generated by means of the hydraulic pump is changed in response to the revolutions per minute of the engine, that is, the engine speed, mounted upon the outboard motor, which may not be suitably controlled according to the navigation conditions.
OBJECTS OF THE INVENTION
An object of this invention is to substantially eliminate the defects or drawbacks of the conventional technology and to provide a power steering system for an outboard motor which is capable of easily and suitably steering an outboard motor body by means of a small steering load which is free from the changes of the navigation conditions.
Another object of this invention is to provide a power steering system for the outboard motor which is capable of reducing the necessary space of the power steering system required within the hull so as to thereby render the system applicable to a small sized hull.
SUMMARY OF THE INVENTION
These and other objects can be achieved according to the present invention, in accordance with one aspect thereof, by providing a power steering system for an outboard motor for steering the outboard motor body of the outboard motor disposed outside of a rear portion of the hull and provided with an engine and a propeller driven by means of the engine, the power steering system comprising a manual steering system mounted upon the hull for operating a steering element so as to manually steer the outboard motor body, a power unit operatively connected to the manual steering system and including an electric motor for applying a steering assist force to the manual steering system, a sensor means for detecting navigation conditions of the hull and the outboard motor, and control means for controlling the electric motor of the power unit so as to generate the steering assist force in accordance with the navigation conditions detected by the sensor means.
In accordance with preferred embodiments of the present invention, the sensor means operatively connected to the control means is provided with a steering torque sensor for detecting steering torque during operation of the manual steering system, an engine speed sensor for detecting engine speed and a steering sensor for detecting steering angle and steering direction of the outboard motor body steered by means of the manual steering system.
The control means controls the electric motor of the power unit so as to determine the power assist force required in response to the steering torque detected by means of the steering torque sensor and then converts or refines the determined force into a final applied force in response to the engine speed and the steering angle respectively detected by means of the engine speed sensor and the steering angle sensor.
The sensor means comprises a thrust sensor operatively connected to the control means for detecting the thrust force generated by means of the propeller of the outboard motor.
The control means controls the electric motor of the power unit so as to generate the steering assist force in proportion to the thrust force detected by means of the thrust sensor.
The outboard motor is provided with a power trim-tilt system for automatically trimming and tilting the outboard motor body and the thrust sensor directly detects the pressure of the pressurized oil operating the power trim-tilt system so as to indirectly detect the thrust generated by means of the propeller.
In accordance with another aspect of the present invention, there is provided a power steering system for an outboard motor for steering an outboard motor body of the outboard motor disposed outside of a rear portion of the hull, the power steering system comprising a manual steering system mounted upon the hull for operating a steering element so as to manually steer the outboard motor body and a power unit operatively connected to the manual steering system and including an electric motor for applying a steering assist force to the manual steering system and a transmission means for transmitting the power generated by means of the electric motor, the electric motor being accommodated within a motor box means located outside the hull.
In preferred embodiments, the transmission means is accommodated within a transmission box means located outside the hull. The hull is provided with a transom at the rear portion thereof and the transmission means comprises reduction gears, a rack and a pinion, the reduction gears being accommodated within a gear box located outside the hull, the rack and pinion being accommodated within a rack box located above a surface of the transom.
According to the present invention having the characteristics and structures described above, the power steering system of the outboard motor comprises a control means which sets the steering assist force applied to the manual steering system in accordance with the engine speed and the steering angle respectively detected by means of the engine speed sensor and the steering angle sensor as well as the steering torque detected by means of the steering torque sensor, so that the steering assist force can be suitably controlled in accordance with or regardless of the navigation conditions of the hull.
In addition, the control means sets the steering assist force so as to be proportional to the thrust force generated by means of the propeller of the outboard motor and affect the steering load, so that the steering assist force can be controlled so as to correspond to the fluctuation of the steering load. Thus, the power steering system can easily and suitably steer the outboard motor body by means of a small load which is free from the navigation conditions, thereby improving the steering feeling and operation.
Furthermore, according to the present invention, the power steering system comprises the motor box in which the electric motor of the power unit is accommodated and the transmission box in which the transmission means for transmitting the steering assist force generated by means of the electric motor to the manual steering system is accommodated. The motor box and the transmission box are located outside the rear portion of the hull at which position the outboard motor is disposed, thereby reducing the location space of the power steering system required within the hull and, hence, the power steering system can be applied to a small sized craft so as to improve the usage thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
For a better understanding of the present invention and to show how the same is carried out, reference is now made to, by way of preferred embodiments, the accompanying drawings, in which like reference characters designate like or corresponding parts throughout the several views, and wherein:
FIG. 1 is a block diagram mainly representing a controller of a power steering system of an outboard motor of the first embodiment according to the present invention;
FIG. 2 is a side view of the outboard motor to which the power steering system provided with the controller shown in FIG. 1 is applied;
FIG. 3 is a front view of the power steering system of the first embodiment;
FIG. 4 is a longitudinal sectional view of the power steering system shown in FIG. 3;
FIG. 5 is an enlarged perspective view of a portion of the power steering system enclosed by means of the circle designated by means of the reference character 5 as shown in FIG. 4;
FIG. 6 is an illustration representing an arrangement of a steering angle sensor shown in FIG. 4;
FIG. 7 is a sectional view representing a gear tooth of a pinion shown in FIG. 6;
FIG. 8 is a flowchart representing control conditions of the controller shown in FIG. 1;
FIG. 9 is a graph representing the relationship between the steering torque and the current value supplied to a motor, which is memorized within the ROM shown in FIG. 1;
FIG. 10 is a graph representing the relationship between the engine speed, the steering angle and the current value to the motor, which are memorized within the RAM shown in FIG. 1;
FIG. 11A is a plan view representing the arrangement of a detecting gear comprising one modification of the first embodiment;
FIG. 11B is an enlarged sectional view of the portion enclosed by means of the circle designated 11B as shown in FIG. 11A;
FIG. 12 is a block diagram mainly representing a controller of a power steering system of the second embodiment according to the present invention;
FIG. 13 is a perspective view of the power steering system including the controller shown in FIG. 12;
FIG. 14 is a front view of the power steering system of the second embodiment shown in FIG. 12;
FIG. 15 is a longitudinal sectional view of the power steering system shown in FIG. 14;
FIG. 16 is a front view of a power trim-tilt system accommodated within the outboard motor body shown in FIG. 14;
FIG. 17 is a side view of the power trim-tilt system shown in FIG. 16;
FIG. 18 is a front view of a thrust sensor of the power trim-tilt system shown in FIGS. 12 and 16;
FIG. 19 is a schematic sectional view of the power trim-tilt system shown in FIGS. 16 and 17;
FIG. 20 is a graph generally representing the relationship between the engine speed and the thrust force generated by means of a propeller;
FIG. 21 is a partial perspective view of the power steering system of the third embodiment according to the present invention;
FIG. 22 is a longitudinal sectional view partially representing the power steering system shown in FIG. 21;
FIG. 23 is a side view of the outboard motor including the power steering system shown in FIGS. 21 and 22;
FIG. 24 is a perspective view of a conventional manual steering system; and
FIG. 25 is a side view representing the tilt-up and tilt-down conditions of the outboard motor body shown in FIG. 24.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In advance of the detailed description of the preferred embodiments of the present invention, the conventional art will be described hereunder with reference to FIGS. 24 and 25.
Referring to FIG. 24 showing a manual steering system for an outboard motor, when an operator controls steering wheel 2 disposed at a driving station within a hull 1, a gear within a gear box 4 is rotated through means of a steering shaft 3. In response to the rotation of the gear, an inner cable 6 of a steering cable 5 is reciprocated axially forwardly or backwardly (push-pull motion). The steering cable 5 comprises an outer cable 7 and the inner cable 6 coaxially located therein.
The front end of the inner cable 6 extends slightly beyond the front end of the outer cable 7 and is connected to one end of a drag link 9 of a link mechanism 8. The drag link 9 has an L-shaped configuration and has the other end thereof connected to one end of a steering bracket 10 which is pivotable. The other end of the steering bracket 10 is secured to a body 12 of the outboard motor 11.
As shown in FIG. 25, the outboard motor body 12 comprises a drive shaft housing 13 including a drive shaft, not shown. The outboard motor body 12 is supported by means of a swivel bracket 14 through means of a pilot shaft, not shown, which is secured to the drive shaft housing 13 so as to be horizontally rotatable or steerable around the pilot shaft. The swivel bracket 14 is supported so as to be rotatable, that is, tiltable, in a vertical direction by means of a clamp bracket shaft 15 which is horizontally mounted between a laterally spaced pair of clamp brackets 16 and 16, by means of which a transom la of the hull 1 thereby mounts the outboard motor body 12 to the hull 1. Accordingly to the structure described above, the outboard motor body 12 is horizontally bilaterally swung about the pilot shaft by means of the push-pull motion of the inner cable 6 by the steering cable 5 through means of the link mechanism 8, whereby the outboard motor body 12 is able to be steered.
However, with respect to the manual steering system of the conventional type described above, the maneuvering of the outboard motor 11 may involve much labor as a result of an increase of the steering load applied thereto during the steering operation due to the navigation conditions, such as, for example, wind or wave conditions, hull speed, trim angle of the outboard motor 11, or the like.
In order to obviate the defect of the conventional manual steering system and, hence, to reduce the steering load applied thereto, conventional technology provides a hydraulic power steering system for the outboard motor. However, the hydraulic power steering system of the prior art utilizes a power source of the outboard motor itself as a power source for driving a hydraulic pump of the hydraulic power steering system. Accordingly, the steering assist force generated by means of the hydraulic pump is changed in response to changes in the revolutions per minute of the drive shaft of the outboard motor and may not be suitably controlled in accordance with the navigation conditions.
A power steering system according to the present invention conceived for substantially eliminating the defects or drawbacks encountered within the prior art described above will now be described hereunder with reference to FIGS. 1 to 23.
Referring to FIGS. 1 to 10 representing the first embodiment according to the present invention, FIG. 3 shows a front view of a power steering system 20 of one embodiment of the present invention. Referring to FIG. 3, the power steering system 20 comprises a manual steering system 21 and a power unit 22 wherein the manual steering system 21 is of the type substantially the same as that shown in FIGS. 24 and 25, so that the like reference numerals are used to designate elements or members corresponding to those shown in FIGS. 24 and 25 and the details thereof are now omitted herefrom.
The power unit 22 acts to apply a steering assist force directed in the same direction as the manual steering force of the manual steering system 21 to an input end of the link mechanism 8 so as to thereby reduce the steering load. The power unit 22 comprises a motor box 23 in which a motor, not shown, is accommodated, a gear box 24 in which a reduction gear is accommodated and a sensor box 25 in which a torque sensor, not shown, is incorporated.
As shown in FIG. 4, the motor box 23 and the gear box 24 are integrally coupled with a rack box 27 in which a rack 26 is accommodated and the integral structure is secured to an upper portion of the swivel bracket 14 of the outboard motor 11 by means of bolts.
The sensor box 25 is secured to one of the paired clamp brackets 16 through means of a support arm 28 and slidably accommodates a sensor rod, not shown, therein. The sensor rod has one end secured to a terminal end of the outer cable 7 by means of a stationary arm 28a. The other end of the sensor rod is operatively connected to a potentiometer, not shown, accommodated within the sensor box 25. The potentiometer and the sensor rod described above constitute a steering torque sensor 32 as shown in FIG. 1.
When the inner cable 6 is pushed or pulled with respect to the outer cable 7 by means of the manual operation of the steering wheel 2, the reaction force applied to the outer cable 7 by means of the push or pull motion of the inner cable 6, that is, the steering load, is transmitted to the sensor rod through means of the stationary arm 28a. The displacement of the sensor rod is detected by means of the potentiometer disposed within the sensor box 25 and a signal, that is, a steering torque signal, representing the displacement detected by means of the potentiometer is transmitted to a controller 29 described later herein and shown in FIG. 1.
As shown in FIG. 4, the rack box 27 has axial ends to which shrinkable cylindrical bellows 31 and 31 are coaxially secured and the rack 26 is accommodated within the rack box 27 in an axially reciprocating and liquid-tight manner. The rack 26 has one axial end (right end as viewed in FIG. 4) secured to a stay 26a and, as shown in FIG. 5, the stay 26a is connected to a bent end 9a of the drag link 9 which is disposed in a direction normal to link 9 by means of a washer 33 and a nut 34. The rack 26 is engaged with a pinion 30 at an intermediate portion thereof, which is fixed to a pinion shaft 30a. The pinion shaft 30a is operatively connected to the motor shaft 37 of the motor 38, shown in FIG. 1, through means of reduction gears 35 and 36 which are in the form of bevel gears and are engaged with each other. Accordingly, when the motor 38 is driven, the pinion 30 is rotated through means of the reduction gears 35 and 36 so as to thereby move the rack 26 in the linear direction thereof, whereby the rotating power of the motor 38 is transmitted to the link mechanism 8 as the steering assist force for reducing the steering load so as to thereby easily steer the outboard motor body 12.
Referring to FIG. 1, an engine speed sensor 39 detects the revolutions per minute of the engine (that is, the engine speed), not shown, mounted within the outboard motor body 12 and transmits a signal representing the engine speed, that is, an engine speed signal, to the controller 29.
A steering angle sensor 40 utilizes a non-contact electromagnetic sensor and is arranged so as to be disposed opposite to the pinion 30 as shown in FIG. 6. When an operator operates the steering wheel 2 so as to move the inner cable 6 of the steering cable 5 and to rotate the pinion 30 through means of the stay 26a and rack 26, the steering angle sensor 40 counts the number of gear teeth 41 of the pinion 30 so as to thereby detect the steering angle of the outboard motor body 12. Referring to FIG. 7, each of the gear teeth 41 of the pinion 30 has a top land 42 upon which a cutout portion 43 is formed in such a manner so as not to decrease or adversely affect the strength of the pinion 30. The cutout portion 43 is formed so as to be disposed in an asymmetrical manner such that the position of the cutout portion 43 is disposed such that the ends thereof are at distances L and M respectively from bilateral ends of the top land 42. Accordingly, when the steering angle sensor 40 detects this asymmetrical cutout portion 43, detected voltage waveforms of the gear teeth 41 of the pinion 30 are asymmetrical, thus detecting the direction of rotation of the pinion 30, that is, the steering direction of the outboard motor body 12. The steering angle sensor 40 transmits signals representing these steering angles and steering directions described above as steering angle-direction signals to the controller 29.
Referring to FIG. 1, the controller 29 is composed of a central processing unit (CPU) 44, memory units comprising a read only memory (ROM) 45 and a random access memory (RAM) 46 and signal converters comprising an analog-to-digital converter (A-D converter) 47 and a digital-to-analog converter (D-A converter) 48.
The ROM 45 has a data-table, as shown in FIG. 9, representing the relationship between the steering torque T and the current value A supplied to the motor 38. The steering assist force applied to the link mechanism 8 from the power unit 22 is determined in accordance with the current value A supplied to the motor 38. Referring to FIG. 8, CPU 44 reads the steering torque signal and the engine speed signal from the steering torque sensor 32 and the engine speed sensor 39 respectively through means of the A-D converter 47 when the START switch is ON, and then determines the current value A to be supplied to the motor 38 for generating the steering assist force corresponding to the steering torque T represented by means of the steering torque signal with reference to the data-table memorized within the ROM45.
The RAM 46 has a data-table, as shown in FIG. 10, representing the relationship between the steering angle Θ, the engine speed R and the current values A' and A" supplied to the motor 38. Referring to the FIG. 8, the CPU 44 continually reads the steering angle Θ through means of the A-D converter 47 during the operation of a shift device accommodated within the outboard motor body 12. The CPU 44 then transits the steering angle Θ data to the RAM 46 and simultaneously calculates the proper current value so as to the adjust the current A as determined by means of the data-table memorized within the ROM 45.
Namely, the characteristics of the current values A' and A" memorized within RAM 46, as shown in FIG. 10, are different in accordance with the engine speed R even for the same steering angle Θ. The CPU 44 selects one of these characteristics of the current values A' and A" in accordance with the engine speed signal transmitted from the engine speed sensor 39 and, for example, selects a characteristic curve represented by means of a full line P as viewed in FIG. 10 in the case where the engine speed R is more than 5500 r.p.m. This characteristic curve represented by means of the full line P designates the supplied current value A determined by means of the data-table as shown in FIG. 9 in the case where the steering angles is less than the steering angle α (Θ<α), the designates the supplied current value A' determined by means of the formula described such as, for example,
A'=A-X(Θ-α)
in the case where the steering angles is more than the steering angle α and less than a steering angle β (α<Θ<β; α<β), thus reducing the steering assist force determined by means of the supplied current value A'. The letter X represents a gradient of the full line P as shown in FIG. 10 for the condition wherein α<Θ<β. The characteristic curve represented by means of the full line P thus designates the supplied current value A" determined by means of the formula described such as, for example,
A"=A-X (β-α)
in the case where the steering angles is more than the steering angle β (Θ>β). As this supplied current value A" is constant, the steering assist force determined by means of the current value A" is also constant. According to the characteristics described above, when the engine speed R is high and the steering angle Θ is large, the controller 29 operates to reduce the current value supplied to the motor 38, thus avoiding a turn-over, for example, of the hull 1.
Referring to FIG. 1, the current value A, A' or A" supplied to the motor 38 is transmitted to a driver 49 through means of the D-A converter 48, which amplifies the current value from the controller 29 so as to drive the motor 38 and then conducts the amplified current to the motor 38.
According to the described first embodiment, the controller 29 adjusts the supplied current value A to the motor as determined by means of the steering torque T as derived from the steering torque sensor 32 in accordance with the engine speed R and the steering angle θ respectively detected by means of the engine speed sensor 39 and the steering angle sensor 40. In the case where the engine speed R is high, the controller 29 preferably supplies to the motor 38 a current value less than the supplied current value A as determined by means of the steering torque T so as to reduce the steering assist force, so that the steering assist force can be suitably controlled in accordance with the navigation conditions. Thus, the power steering system of the outboard motor can easily and suitably steer the outboard motor body with a small steering load.
FIG. 11A is a fragmentary plan view of one modification according to the first embodiment. In this first modification, the pinion 30 and a detecting gear 50 are coaxially located with respect to the pinion shaft 30a, and the detecting gear 50 has gear teeth 41 provided with the cutout portion 43 as shown in FIG. 7 so as to detect the direction of rotation of the pinion 30 or has gear teeth 51, as shown in FIG. 11B, respectively provided with stepped cutout portions 52 so as to similarly detect the direction of rotation of the pinion. The shapes of the teeth of the detecting gear 50 provided with the cutout portion 43 or 52 is detected by means of the steering angle sensor 40. According to this modification, these cutout portions 43 and 52 are formed without adversely affecting the strength of the pinion 30, thus correctly detecting the steering direction of the outboard motor body 12 by means of a voltage wave of the detecting gear 50.
In another modification of the first embodiment, the steering sensor 40 may be arranged so as to directly detect the rotation of the motor 38 so as to detect the steering direction of the outboard motor body 12.
Referring to FIGS. 12 to 20 representing the second embodiment according to the present invention, FIG. 13 is a perspective view of a power steering system 60 of the second embodiment of the present invention, in which like reference numerals designate portions or members corresponding to those used for the first embodiment shown in FIGS. 1 to 10 and, consequently, a detailed description thereof is now omitted herefrom.
In the second embodiment, the power steering system 60 is applied to the outboard motor 11 in which a power trim-tilt system 62 is accommodated, as shown in FIGS. 16 and 17, and comprises the manual steering system 21 and a power unit 61.
The power unit 61 comprises a thrust sensor 63 as shown in FIGS. 12, 16 and 18, the motor box 23, as shown in FIGS. 13 to 15, in which a motor 38 for generating the steering assist force is accommodated, the gear box 24 in which the reduction gears 35 and 36 for transmitting a turning force are accommodated, and the rack box 27 in which the rack 26 and pinion 30 for transmitting the turning force from the gears 35 and 36 to the drag link 9 of the link mechanism 8 through means of the stay 26a are incorporated.
The trust sensor 63, as described later in detail, detects the thrust of the propeller 64, as shown in FIG. 2, of the outboard motor 11 and transmits a trust signal representing the thrust to controller 65 as shown in FIGS. 12 and 13.
Referring to FIG. 12, the controller 65 is composed to an arithmetic unit 66, an output unit 67 for the torque control signal and a motor control unit 68, wherein the arithmetic unit 66 calculates and determines the steering assist force in proportion, for example, to the thrust represented by means of the trust signal and transmits an assist force control signal representing the steering assist force to the motor control unit 68 through means of the output unit 67 as an output member. The motor control unit 68 manipulates, and preferably amplifies the assist force control signal and transmits the amplified signal to the motor 38. Thus the controller 65 controls the rotation of the motor 38 so as to generate the suitable steering assist force.
Namely, the steering load applied to the steering wheel 2 during the steering operation is generally affected by means of the trust force generated by means of the propeller 64 and the force applied to the outboard motor body 12 in the direction of the axis of the propeller 64 or the moment around the pivot shaft, not shown, applied to the outboard motor body 12. The applied force and the moment respectively described above are proportional to the thrust force generated by means of the propeller 64. Accordingly, the controller 65 controls the steering assist force generated by means of the motor 38 so as to be proportional to the thrust force to propeller 64, thus adjusting the steering assist force in accordance with fluctuations of the steering load, whereby the steering feeling can be improved.
Referring to FIG. 20 in a running craft such as, for example, a motor boat, the thrust force generated by means of the propeller 64 during the engine operation is a maximum before the water-borne operation of the craft and is constant during the water-borne operation of the craft. In this case, the controller 65 controls the steering assist force generated by means of the motor 38 so as to rapidly increase before the water-borne operation of the craft and to be constant during the water-borne operation of the craft in response to the thrust force generated by means of the propeller 64 described above.
As shown in FIGS. 16 and 17, the power trim-tilt system is composed of a pair of trim cylinders 69a and 69b accommodated within the outboard motor body 12, a tilt cylinder 70 arranged between the trim cylinders 69a and 69b within the outboard motor body 12, and an oil pump 71 located outside the outboard motor body 12. Referring to FIG. 19, the oil pump 71 supplies pressurized oil and an inner upper chamber and an inner lower chamber of the tilt cylinder 70 through means of a tilt-down tube 72 and a tilt-up tube 73 respectively, so as to thereby move a piston rod 74 incorporated within the tilt cylinder 70 downwardly and upwardly, whereby the outboard motor body 12 can be automatically tilted downwardly and upwardly, respectively. The oil pump 71 also supplies the pressurized oil to an inner upper chamber and an inner lower chamber of trim cylinders 69a and 69b through means of a trim-down tube 75 and a trim-up tube 76 respectively, so as to thereby move piston rods 77a and 77b respectively incorporated within the trim cylinders 69a and 69b downwardly and upwardly. Thus, the outboard motor body 12 can be automatically trimmed downwardly and upwardly within the range of the tilt angle.
The trim-up tube 76 is interposed between an output end of the oil pump 71 and the inner lower chambers of the trim cylinders 69a and 69b so as to supply the pressurized oil within the oil pump 71 into the inner lower chambers of the trim cylinders 69a and 69b. The thrust sensor 63 is disposed within the flow line of the trim-up tube 76 and, as shown in FIG. 18, is composed of a pressure sensor 78 and a sensor body 79 which comprises a liquid-tight hollow box structure secured t the trim-up tube 76. The pressure sensor 78 is accommodated within the sensor body 79 and is adapted to detect the pressure of the pressurized oil within the trim-up tube 76 and then transmit an electric signal representing the detected pressure to the arithmetic unit 66 of the controller 65 through means of a signal cable 80. The pressurized oil within the trim-up tube 76 therefore effectively applies to the outboard motor body 12 a force, which is substantially the same as that of the thrust force generated by means of the propeller 65, in a direction opposite to the thrust force direction so as to thereby hold the hull 1 in a predetermined navigation state with the bow thereof lifted upwardly. Accordingly, the thrust force generated by means of the propeller 65 can be indirectly detected by means of the thrust sensor 63 which directly detects the pressure of the pressurized oil within the trim-up tube 76.
The arithmetic unit 66 of the controller 65, as shown in FIG. 12, has a data-table representing the relationship between the pressure of the pressurized oil within the trim-up tube 76 and the trust force generated by means of the propeller 64, and the arithmetic unit 66 reads the thrust force corresponding to the detected signal from the thrust sensor 63 according to the data-table. The arithmetic unit 66, furthermore, calculates and determines the steering assist force proportional to the trust force read in the described manner and transmits the assist fore control signal representing the steering assist force determined in the described manner to the motor control unit 68 through means of the output unit 67. The motor control unit 68 manipulates and preferably amplifies the assist force control signal and then transmits the amplified signal to the motor 38, whereby the controller 65 enables the motor 38 to generate the suitable steering assist force corresponding to the fluctuation of the steering load.
According to the described second embodiment, the controller 65 enables the motor 38 to generate the suitable steering assist force corresponding to the fluctuation of the steering load which is generally affected by means of the thrust force generated by means of the propeller 64 and the like force, thus reducing the steering load applied to the steering wheel 2 and, hence, the steering feeling can ge improved by means of the suitable steering assist force corresponding to the fluctuation of the steering load.
In addition, the thrust sensor 63 indirectly detects the thrust force generated by means of the propeller 64 in such a manner by directly detecting the pressure of the pressurized oil within the trim-up tube 76 of the existing opwer trim-tilt system 62, so that the thrust sensor 63 can be made compact and simplified with reduced cost.
In accordance with a first modification of the second embodiment, the thrust sensor 63 may be disposed within the tilt-up tube 73 of the power trim-tilt system 62 so as to thereby directly determine the pressure of the pressurized oil within the tilt-up tube 73, thus indirectly detecting the thrust force generated by means of the propeller 64, because the pressurized oil is also supplied to the tilt cylinder 70 as well as the trim cylinders 69a and 69b during the trim-up operation.
In accordance with a second modification of the second embodiment, the power trim-tilt system 62 is composed of a single hydraulic cylinder for attaining both the power trim effect and the power tilt effect. The thrust sensor may be mounted within a tube through which the pressurized oil is supplied from the oil pump 71 to the inner chamber of the hydraulic cylinder described above, thus indirectly detecting the thrust force generated by means of the propeller 64.
Referring to FIGS. 21 and 23 representing the third embodiment according to the present invention, FIG. 21 is a partial perspective view of a power steering system 90 of the third embodiment of the present invention, in which like reference numerals are used to designate portions or members corresponding to those used for the first embodiment shown in FIGS. 1 to 10 and, consequently, a detailed description thereof is now omitted herefrom.
In the third embodiment, the power steering system 90 comprises the manual steering system 21 and a power unit 91. Referring to FIGS. 21 and 22, the power unit 91 is provided with a motor box 92 within which a motor 38 is accommodated, a gear box 93 in which the reduction gears 35 and 36 are accommodated, a rack box 94 in which a rack 97 and a pinion 96 are incorporated, and a sensor box 95 in which a potentiometer and a sensor rod constituting the steering torque sensor 32 are accommodated. The reduction gears 35 and 36, the rack 97 and the pinion 96 are constructed as a transmission means for transmitting the steering assist force generated by means of the motor 38 to the link mechanism 8 of the manual steering system 21. The motor box 92 and the gear box 93 are located outside the transom 1a of the hull, and the rack box 94 is disposed above, as viewed, an upper end surface of the transom 1a in parallel relationship with respect thereto. The sensor box 95 is coaxially mounted with respect to the inner cable 6 of the steering cable 5.
Namely, the motor box 92 is arranged outside the transom in such a manner that the longitudinal direction of the motor box 92 corresponds to the upward and downward direction as viewed, and the gear box 93 is integrally secured to the upper, as viewed, portion of the motor box 92. The reduction gear 35 secured to the motor shaft, not shown, is substantially perpendicularly engaged with the reduction gear 36 secured to the pinion shaft 96a extending horizontally as viewed, whereby the rotation force of the motor 38 changes to the horizontal direction from the vertical direction as shown in FIG. 21.
The rack box 94 which accommodates a pinion shaft 96a as well as the rack 97 and the pinion 96 is mounted to one of the clamp brackets 16 in a coaxial relationship with respect to the clamp bracket shaft 15 interposed between the clamp brackets 16 and 16. One of the bellows 31 is attached to the rack box 94 and the other bellow is attached to the end portion of the clamp bracket shaft 15 in such a manner as to extend outwardly beyond the other one of the clamp brackets 16. The rack 97 is coaxially accommodated within the rack box 94 and the hollow clamp bracket shaft 15 in an axially reciprocating manner and both axial ends of the rack 97 are incorporated in the bellows 31. The most outward end portion 97a, that is, the most rightward end as viewed in FIG. 22, of the rack 97 extends outside bellow 31 and is perpendicularly connected to the stay 26a through means of a free joint device 98 so as to thereby transmit the axial reciprocation of the rack 97 to the outboard motor body 12 through means of the link mechanism 8, whereby the outboard motor 12 can be steered in the bilateral direction.
According to the third embodiment described above, the motor box 92 and the gear box 93 are located outside the transom 1a of the hull 1 and the rack box 94 is disposed above the transom 1a and rearwardly of the steering cable 5, so that the power unit 91 composed of the motor box 92, the gear box 93, the rack box 94 and the like members is not mounted inside the hull 1, thus eliminating any reduction of the space of the hull 1. Accordingly, the power steering system 90 is able to be applied to a small sized craft, for example a small sized motor board, which normally or otherwise would not have sufficient space to accommodate such a power steering system, thereby improving the utility of the power steering system 90.
It is to be understood by persons skilled in the art that the present invention is not limited to the described embodiments and many other modifications and changes may be made without departing from the spirit and scope of the appended claims. It is therefore to be understood that within the scope of the appended claims, the present invention may be practiced otherwise than as specifically disclosed herein. | A power steering system for an outboard motor for steering an outboard motor disposed outside of a rear portion of a hull and usually including a manual steering system mounted upon the hull for operating a steering element so as to manually steer the outboard motor body, is disclosed. A power unit is operatively connected to the manual steering system and includes an electric motor for applying a steering assist force to the manual steering system. The power unit is located at the portion of the hull capable of effectively utilizing the inner space of the hull and the electric motor of the power unit is controlled by means of a control unit in accordance with the navigation conditions of the hull and the operating conditions of the outboard motor as detected by means of suitable sensors. The sensors comprise various sensors such as, for example, a steering torque sensor and an engine speed sensor. | 5 |
FIELD OF THE INVENTION
This invention relates to internal combustion engines, and, more particularly, to a method and associated control system for determining the duration of the fuel injection pulse in each cylinder of a multi-cylinder internal combustion engine.
BACKGROUND OF THE INVENTION
In the feedforward part of an SI (Spark Ignition) engine Air/Fuel control system, the in-cylinder mass air flow rate should be accurately estimated in order to determine the amount of fuel to be injected. Generally, this evaluation is performed either with a dedicated physical sensor (MAF sensor) or more often through an indirect evaluation.
To meet strict emission regulations, automobile gasoline engines are equipped with a three-way catalytic converter (TWC). A precise control of the air-fuel ratio (A/F) to maintain it as close as possible to the stoichiometric value is necessary to achieve a high efficiency of the TWC converter in the conversion of the toxic exhaust gases (CO, NOx, HC) into less harmful products (CO 2 , H 2 O, N 2 ). Typically, in a spark-ignition engine, this control is performed through a so-called lambda sensor. The lambda sensor generates a signal representative of the value of the ratio
λ = Air / Fuel Air / Fuel stoichiometric
from the amount of oxygen detected in the exhaust gas mixture. If λ<1 the mixture is rich of fuel, while if λ>1 the mixture is lean of fuel.
To keep the air/fuel ratio (AFR) as close as possible to unity, the lambda sensor is introduced in the conduit or stream of exhaust gases for monitoring the amount of oxygen present in the exhaust gas mixture. The signal generated by the lambda sensor is input to the controller of the engine that adjusts the injection times and thus the fuel injected during each cycle for reaching the condition λ=1.
Traditional Air/Fuel control systems include a feed-forward part, in which the amount of fuel to be injected is calculated on the basis of the in-cylinder mass air flow, and a feedback part that uses the signal of the oxygen sensor (lambda sensor) in the exhaust gas stream, to ensure that the Air/Fuel remain as close as possible to the stoichiometric value (e.g. Heywood, J.B., -“Internal combustion engine fundamentals”-McGraw-Hill Book Co., 1988.).
FIG. 1 shows a block diagram of a traditional Air/Fuel control system. Generally, the feedback part of the Air/Fuel control system is fully active only in steady-state conditions. Moreover, the lambda sensor signal is made available only after this sensor has reached a certain operating temperature. In transients and under cold start conditions, the feedback control is disabled, thus the feedforward part of Air/Fuel control becomes particularly important.
As mentioned above, air flow estimation is often the basis for calculating the amount of injected fuel in the feedforward part of Air/Fuel control system.
A conventional technique for estimating a cylinder intake air flow in a SI (Spark Ignition) engine involves the so-called “speed-density” equation:
m . ap = η ( p m , N ) · V d · N · p a 120 · R · T m
where {dot over (m)} ap is the inlet mass air flow rate, V d is the engine displacement and N is the engine speed; T m and p m are the average manifold temperature and pressure and η is the volumetric efficiency of the engine. This is a nonlinear function of engine speed (N) and manifold pressure (p m ), that may be experimentally mapped in correspondence with different engine working points.
A standard method is to map the volumetric efficiency and compensate it for density variations in the intake manifold.
One of the drawbacks in using the “speed-density” equation for the in-cylinder air flow estimation is the uncertainty in the volumetric efficiency. Generally, the volumetric efficiency is calculated in the calibration phase with the engine under steady state conditions. However variations in the volumetric efficiency due, for example, to engine aging and wear, combustion chamber deposit buildup etc., may introduce errors in the air flow estimation.
The low-pass characteristic of commercial sensors (Manifold Absolute Pressure or MAP sensors) used for the determination of the manifold pressure p m , introduces a delay that, during fast transients, causes significant errors in the air flow determination.
This problem is not solved by using a faster sensor because in this case the sensor detects also pressure fluctuations due to the valve and piston motion (e.g. Barbarisi, et al., “An Extended kalman Observer for the In-Cylinder Air Mass Flow Estimation”, MECA 02 International Workshop on Diagnostics in Automotive Engines and Vehicles, 2001).
In engines equipped with an EGR (Exhaust Gas Recirculation) valve, the MAP (Manifold Absolute Pressure) sensor cannot distinguish between fresh air (of known oxygen content) and inert exhaust gas in the intake manifold. Therefore, in this case the speed-density equation (1) cannot be used and the air charge estimation algorithm should provide a method for separating the contribution of recycled exhaust gas to the total pressure in the intake manifold (e.g. Jankovic, M., Magner, S.W., “Air Charge Estimation and Prediction in Spark Ignition Internal Combustion Engines”, Proceedings of the American Conference, San Diego, California, June 1999).
An alternative method for the air charge determination is to use a dedicated Mass Air Flow (MAF) physical sensor, located upstream the throttle, that directly measures the inlet mass air flow. The main advantages of a direct air flow measurement are: automatic compensation for engine aging and for all other factors that modify engine volumetric efficiency; improved idling stability; and lack of sensibility of the system to EGR (Exhaust Gas Recirculation) since only the fresh air flow is measured.
Anyway, air flow measurement by means of a MAF sensor (which is generally a hot wire anemometer) accurately estimates the mass flow in the cylinder only in steady state because during transients the intake manifold filling/empting dynamics play a significant role (e.g. Grizzle, J.W., Cookyand, J.A., and Milam, W.P., “Improved Cylinder Air Charge Estimation for Transient Air Fuel Ratio Control”, Proceedings of American Control Conference, 1994; and Stotsky, I., Kolmanovsky, A., “Application of input estimation and control in automotive engines” Control Engineering Practice 10, pp. 1371-1383, 2002).
Moreover, for commercial automotive applications, the fact that a MAF sensor has a relatively high cost compared to the cost of MAP (Manifold Absolute Pressure) sensor used with the “speed density” evaluation approach, should be taken into account.
SUMMARY OF THE INVENTION
Test carried out by the applicants have unexpectedly shown that the amount of fuel to be injected in each cylinder of a multi-cylinder spark ignition internal combustion engine may be determined with enhanced precision if the fuel injection durations are determined as a function of the sensed mass air flow in all the cylinders of the engine, instead of considering only the air flow in the same cylinder.
This surprising finding has led the applicants to devise a more efficient method of controlling a multi-cylinder spark ignition internal combustion engine and an innovative feedforward control system.
The feedforward control system may be embodied in a feedforward-and-feedback control system of a multi-cylinder spark ignition engine, including a lambda sensor, that effectively keeps the composition of the air/fuel ratio of the mixture that is injected into the combustion chamber of each cylinder at a pre-established value.
Experimental tests carried out by the applicants demonstrated that the feedforward-and-feedback control system of this invention is effective in controlling the engine such to keep the lambda value as close as possible to any pre-established reference value.
BRIEF DESCRIPTION OF THE DRAWINGS
Preferred embodiments of the invention will be described referring to the attached drawings, wherein:
FIG. 1 is a block diagram illustrating a conventional air/fuel control system for an internal combustion engine as in the prior art;
FIG. 2 is a block diagram illustrating a feedforward injection control system in accordance with the present invention; and
FIG. 3 is a schematic diagram illustrating an injection control system of the present invention for an internal combustion engine with N cylinders.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The amount of fuel to be injected in each cylinder of a spark ignition (SI) internal combustion engine having N cylinders is determined by a feedforward fuel injection control system as that surrounded by the broken line perimeter in FIG. 3 .
The block A IR -C YLINDER generates signals MAF 1 , . . . , MAF N representative of the Mass Air Flow aspired by each cylinder of the engine. This block may be easily realized by juxtaposing N mass air flow sensors.
The block I NJECTION C ONTROL M APS has as inputs the signals MAF 1 , . . . , MAF N and a signal representing the speed of the engine, and generates as a function thereof a feedforward signal I FF1 , . . . , I FFN for each cylinder.
According to an innovative aspect of this invention, each feedforward signal is determined as a function of the speed of the engine and of all the Mass Air Flow values MAF 1 , . . . , MAF N of all the cylinders. The feedforward signals I FF1 , . . . , I FFN are generated in this case by pointing to respective locations of a look-up table that is established during a test phase of the engine.
Tests carried out by the applicants have demonstrated that generating each feedforward signal I FFi for a certain cylinder as a function of all the mass air flow values detected or estimated for all the cylinders of the engine, enhances the apparent correctness of the composition of the air/fuel mixture that is injected into each cylinder of the engine.
This unpredictable result may be explained by the fact that there is an apparent non-homogeneous air filling for the different cylinders of the engine. This phenomenon is induced by air backflow in the intake manifold and air turbulences. For this reason, even if each cylinder of the engine is maintained nominally to the stoichiometric condition, the global exhaust gas could not have the oxygen content needed to guarantee the maximum efficiency of the three-way catalytic converter. For this reason, it appears that the injected fuel amount for each cylinder of the engine should be dependent not only by the related mass air flow value but also by the mass air flow incoming into the other cylinders.
According to a preferred embodiment of this invention, the amount of fuel to be injected in each cylinder of an internal combustion engine having N cylinders is determined with a feedforward-and-feedback fuel injection control system as depicted in FIG. 3 .
A lambda sensor, introduced in the outlet conduit of exhaust gases for monitoring the amount of oxygen in the exhaust gases, determines whether the lambda ratio is above or below unity from the amount of oxygen detected in the exhaust gas mixture. The lambda sensor provides a signal representative of the value of the ratio:
λ
=
Air
/
Fuel
Air
/
Fuel
stoichiometric
If λ<1 the mixture is rich of fuel, while if λ>1 the mixture is lean of fuel.
The feedback-and-feedforward control system comprises an array of controllers CONTROLLERB 1 , . . . , CONTROLLERB N each input with a respective feedforward signal I FFi and with an error signal Δ LAMBDA representing the difference between the actual lambda ratio L AMBDA - VALUE and a reference value L AMBDA - REF . Each controller adjusts the injection duration I 1 , . . . , I N of a respective cylinder and thus the amount of fuel that is injected during each cycle in the respective cylinder for eventually reach the condition L AMBDA - VALUE =L AMBDA - REF .
LAMBDA-VALUE=LAMBDA-REF. The lambda sensor may be preferably a virtual lambda sensor of the type described in the cited prior European Patent application No. 05,425,121.0.
According to a preferred embodiment of this invention, each controller CONTROLLERB i is realized using a Fuzzy Inference System properly set in a preliminary calibration phase of the system, according to a common practice.
Preferably, each mass air flow sensor is a soft-computing mass air flow estimator, of the type disclosed in the European patent application No. 06,110,557.3 in the name of the same applicants and shown in FIG. 2 . This estimator is capable of estimating both in a steady state and in transient conditions the in-cylinder mass air flow of a single-cylinder SI engine, basically using a combustion pressure signal of the cylinder. A learning machine, such as for example a MLP (Multi-Layer Perceptron) neural network, trained on the experimental data acquired in different operating conditions of a gasoline engine, may be used for realizing the inlet mass air flow estimator.
A traditional combustion pressure piezoelectric transducer, or any other low-cost pressure sensor, may provide the required raw information. As disclosed in the cited European Patent application, the cylinder combustion pressure is correlated with the inlet mass air flow of the cylinder, thus a signal produced by a combustion pressure sensor is exploited for producing through a soft-computing processing that utilizes information on throttle opening, speed and angular position, a signal representative of the inlet mass air flow.
REFERENCES
1. Heywood, J. B.,—“Internal combustion engine fundamentals”—McGraw-Hill Book Co., 1988.
2. Barbarisi, O., Di Gaeta, A., Glielmo, L., and Santini, S., “An Extended Kalman Observer for the In-Cylinder Air Mass Flow Estimation”, MECA02 International Workshop on Diagnostics in Automotive Engines and Vehicles, 2001.
3. Grizzle, J. W., Cookyand, J. A., and Milam, W. P., “Improved Cylinder Air Charge Estimation for Transient Air Fuel Ratio Control”, Proceedings of American Control Conference, 1994.
4. Jankovic, M., Magner, S. W., “Air Charge Estimation and Prediction in Spark Ignition Internal Combustion Engines”, Proceedings of the American Conference, San Diego, Calif., June 1999.
5. Stotsky, I., Kolmanovsky, A., “Application of input estimation and control in automotive engines” Control Engineering Practice 10, pp. 1371–1383, 2002. | The amount of fuel to be injected in each cylinder of a multi-cylinder spark ignition internal combustion engine may be determined with enhanced precision if the fuel injection durations are determined as a function of the sensed mass air flow in all the cylinders of the engine, instead of considering only the air flow in the same cylinder. This finding has led to the realization of a more efficient approach of controlling a multi-cylinder spark ignition internal combustion engine and a feedforward control system. | 5 |
TECHNICAL FIELD
The present embodiments relate to network communications.
BACKGROUND
A computer network, often simply referred to as a network, typically includes a group of interconnected computers and devices that facilitate communication between users and allows users to share resources. Adapters, switches and other devices are typically used during network communication. Continuous efforts are being made to improve network communication.
SUMMARY
The various embodiments of the present system and methods have several features, no single one of which is solely responsible for their desirable attributes. Without limiting the scope of the present embodiments as expressed by the claims that follow, their more prominent features now will be discussed briefly. After considering this discussion, and particularly after reading the section entitled “Detailed Description” one will understand how the features of the present embodiments provide various advantages.
In one embodiment, a machine implemented method for a first network device and a second network device, where the first network device and the second network device communicate with each other via a first network link and a second network link is provided. The method includes identifying a network packet field for applying a hashing technique for selecting either the first network link or the second network link to transmit the network packet; and exchanging a hashing parameter between the first network device and the second network device, prior to applying the hashing technique for selecting the first network link and the second network link.
In another embodiment, a machine implemented method for a first network device and a second network device, where the first network device and the second network device communicate with each other via a first network link and a second network link is provided. The method includes negotiating a network packet field for applying a hashing technique for selecting either the first network link or the second network link to transmit the network packet; identifying the hashing technique applied on the network packet field for selecting the first network link and the second network link; and exchanging a hashing parameter between the first network device and the second network device, prior to applying the hashing technique for selecting the first network link and the second network link.
In yet another embodiment, a system is provided. The system includes a first network device and a second network device, where the first network device and the second network device communicate with each other via a first network link and a second network link. The first network device and the second network device are configured to negotiate a network packet field for applying a hashing technique for selecting either the first network link or the second network link to transmit the network packet; identify the hashing technique applied on the network packet field for selecting the first network link and the second network link; and exchange a hashing parameter to select the first network link and the second network link for transmitting the network packet.
This brief summary has been provided so that the nature of the disclosure may be understood quickly. A more complete understanding of the disclosure can be obtained by reference to the following detailed description of the embodiments thereof concerning the attached drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The various present embodiments relating to selectable initialization for adapters now will be discussed in detail with an emphasis on highlighting the advantageous features. These novel and non-obvious embodiments are depicted in the accompanying drawings, which are for illustrative purposes only. These drawings include the following figures, in which like numerals indicate like parts:
FIG. 1A is a functional block diagram of a system, used according to one embodiment;
FIG. 1B shows an example of linking, according to one embodiment; and
FIG. 2 is a process flow diagram, according to one embodiment.
DETAILED DESCRIPTION
The following detailed description describes the present embodiments with reference to the drawings. In the drawings, reference numbers label elements of the present embodiments. These reference numbers are reproduced below in connection with the discussion of the corresponding drawing features.
As a preliminary note, any of the embodiments described with reference to the figures may be implemented using software, firmware, hardware (e.g., fixed logic circuitry), manual processing, or a combination of these implementations. The terms “logic”, “module”, “component”, “system”, and “functionality”, as used herein, generally represent software, firmware, hardware, or a combination of these elements. For instance, in the case of a software implementation, the terms “logic”, “module”, “component”, “system”, and “functionality” represent machine executable code that performs specified tasks when executed on a processing device or devices (e.g., hardware based central processing units). The program code can be stored in one or more computer readable memory devices.
More generally, the illustrated separation of logic, modules, components, systems, and functionality into distinct units may reflect an actual physical grouping and allocation of software, firmware, and/or hardware, or can correspond to a conceptual allocation of different tasks performed by a single software program, firmware program, and/or hardware unit. The illustrated logic, modules, components, systems, and functionality may be located at a single site (e.g., as implemented by a processing device), or may be distributed over a plurality of locations. The term “machine-readable media” and the like refers to any kind of medium for retaining information in any form, including various kinds of storage devices (magnetic, optical, static, etc.).
The embodiments disclosed herein, may be implemented as a computer process (method), a computing system, or as an article of manufacture, such as a computer program product or computer-readable media. The computer program product may be computer storage media, readable by a computer device, and encoding a computer program of instructions for executing a computer process. The computer program product may also be readable by a computing system, and encoding a computer program of instructions for executing a computer process.
FIG. 1A is a block diagram of a system 10 configured for use with the various embodiments. System 10 includes a computing system 12 (may also be referred to as “host system 12 ”) coupled to an adapter 14 that interfaces with a network 16 for communicating with network devices 54 and 56 . The network may include, for example, additional computing systems, servers, storage systems and other devices.
The computing system 12 may include one or more processors 18 , also known as a hardware-based, central processing unit (CPU). The processor 18 executes computer-executable process steps out of a memory 28 and interfaces with an interconnect 20 , which may also be referred to as a computer bus 20 . Processor 18 may be, or may include, one or more programmable general-purpose or special-purpose microprocessors, digital signal processors (DSPs), programmable controllers, application specific integrated circuits (ASICs), programmable logic devices (PLDs), or the like, or a combination of such hardware devices.
The computer bus 20 may be, for example, a system bus, a Peripheral Component Interconnect (PCI) bus (or PCI Express bus), a HyperTransport or industry standard architecture (ISA) bus, a SCSI bus, a universal serial bus (USB), an Institute of Electrical and Electronics Engineers (IEEE) standard 1394 bus (sometimes referred to as “Firewire”), or any other kind of interconnect.
An adapter interface 22 enables computing system 12 to interface with adapter 14 , as described below. The computing system 12 also includes other devices and interfaces 24 , which may include a display device interface, a keyboard interface, a pointing device interface, etc. The details of these components are not germane to the inventive embodiments.
The computing system 12 may further include a storage device 26 , which may be for example a hard disk, a CD-ROM, a non-volatile memory device (flash or memory stick) or any other device. Storage 26 may store operating system program files, application program files, and other files. Some of these files are stored on storage 26 using an installation program. For example, the processor 18 may execute computer-executable process steps of an installation program so that the processor 18 can properly execute the application program.
Memory 28 interfaces to the computer bus 20 to provide processor 18 with access to memory storage. Memory 28 may include random access main memory (RAM). When executing stored computer-executable process steps from storage 26 , the processor 18 may store and execute the process steps out of RAM. Read only memory (ROM, not shown) may also be used to store invariant instruction sequences, such as start-up instruction sequences or basic input/output system (BIOS) sequences for operation of a keyboard (not shown).
With continued reference to FIG. 1A , a link 30 and the adapter interface 22 couple the adapter 14 to the computing system 12 . The adapter 14 may be configured to send and receive network traffic complying with one or more protocols/standards, for example, Ethernet, Gigabit Ethernet, Transmission Control Protocol (TCP), Internet Protocol(IP) and others.
The adapter 14 interfaces with the computing system 12 via a host interface 32 . In one embodiment, the host interface may be a Peripheral Component Interconnect (PCI) Express interface coupled to a PCI Express link (for example, link 30 ).
In one embodiment, adapter 14 includes an offload module 48 that is used to perform certain functions that are typically performed by a host system. As an example, offload module 48 may execute a network protocol stack, for example, a TCP/IP protocol stack for processing TCP/IP packets that are sent and received from other devices. In one embodiment, offload module 48 is a dedicated hardware resource for performing the offloaded function.
Adapter 14 may also include a processor 34 that executes firmware instructions out of memory 36 to control overall adapter 14 operations. Memory 36 may also store the process steps as described below, according to one embodiment.
The adapter 14 may also include storage 46 , which may be for example non-volatile memory, such as flash memory, or any other device. The storage 46 may store executable instructions and operating parameters that can be used for controlling adapter operations.
The adapter 14 includes a network interface 52 (also referred to and shown as port 52 ) that interfaces with a link 50 for sending and receiving network traffic. In one embodiment, port 52 includes logic and circuitry for handling network packets, for example, Ethernet or any other type of network packets. Port 52 may include memory storage locations, referred to as memory buffers (not shown) to temporarily store information received from or transmitted to other network devices.
FIG. 1B shows an example of using link aggregation in system 10 . The term link as used herein includes communication link used by network devices to send and receive information.
Link aggregation is typically used in networks to increase available bandwidth between two network nodes, for example, between computing system 12 and network device 54 ( FIG. 1B ). Certain standards, for example, IEEE 802.3ad provide a mechanism for pairing two network links (for example, 60 A/ 60 B and 60 C/ 60 D). Each network node distributes traffic among links/network ports by using certain techniques, for example, by executing a machine-executable hashing technique that uses one or more fields of a network packet header to select a link/port to send or receive a network packet. The following example illustrates link aggregation with respect to FIG. 1B .
FIG. 1B shows computing system 12 (may also be referred to as network node) communicating with another network device 54 (may also be referred to as computing system or network node) via a switching device 56 . Computing system 12 may include two adapters 14 a and 14 b (similar to adapter 14 described above), each coupled to switching device 56 via links 60 A and 60 B. Switching device 56 is coupled to network device 54 via links 60 C and 60 D. Details of switching device 56 are not provided since they are not germane to the inventive embodiments.
When computing system 12 sends a message to network device 54 , the hashing process executed by computing system 12 and/or one of adapters 14 a / 14 b may select link 60 A. However, the response from network device 54 may be received by computing system 12 via link 60 B.
If adapters 14 a and 14 b use an offload module (for example, 48 , FIG. 1A ), then sending a packet via 60 A and receiving the response via 60 B at adapter 14 b can cause problems. Typically, offload module 48 uses flow information per connection for sending and receiving packets. The packets are mapped to the same physical ports so that the offload module 48 can process a received packet. When return traffic ends up at adapter 14 b having a different physical port, offload module 48 at adapter 14 b is not able to process the packet because it does not maintain connection information of adapter 14 a and hence, the offload operation may fail. It is desirable to use offload module 48 and take advantage of linking between communicating network nodes. The embodiments disclosed herein provide one such solution, as described below with respect to FIG. 2 .
FIG. 2 shows a process flow diagram of a process 200 that uses linking and an offload module between communicating nodes, according to one embodiment. Process 200 begins in block S 202 when communicating devices (or nodes), for example, computing system 12 and network device 54 , negotiate to establish certain protocols and parameters for communication. In block 5204 , both nodes may negotiate and agree on one or more parameters (hash-type) that can be used to identify a connection/flow and on which a hashing technique is performed to select a link.
The type of parameter may depend on a protocol type. For example, for Ethernet based communication, the EtherType field may be used. An Ethernet frame includes a preamble, a destination Media Access Control (MAC) address field, a source MAC address field, an Ether type field, a payload and cyclic redundancy code (CRC). The Ether type field may be a two-octet field in an Ethernet used to indicate which protocol is encapsulated in the PayLoad of an Ethernet Frame.
For Fibre Channel over Ethernet packets, the fields may be a destination identifier (D_ID) or source identifier (S ID). For TCP packets, SRC-SKT (source socket number) or SRC-DST (destination socket number) may be used for identifying a flow.
It is noteworthy that the examples provided above are used to illustrate the adaptive embodiments, which are not limited to using any specific field for defining a connection flow, and on which a hashing technique is implemented.
In block 5206 , a hashing algorithm that is used to select a link is identified and agreed upon by the communicating nodes. In one embodiment, the hashing algorithm generates an “n”-bit hash value where “n” may correspond to a number of physical ports within a link aggregation group. Various hashing algorithms are available and may be used. For example, “xor_nibble” algorithm that may use the MAC address for a destination or a source may be used to select a link. Another example may be the (a) Bit x=XOR (upper bits of each digit of M_DA (Destination MAC address in an Ethernet header) and M_SA (Source MAC address in an Ethernet header) may be used to select a link; or (b) Bit y=XOR (lower bits of each digit of M_DA and M_SA) may be used to select a link.
Hashing parameters are then exchanged in block S 208 . In one embodiment, the hashing algorithm, the hash type, and a “hash scope” may be hard coded and stored at a memory location available to both the communicating nodes 12 and 54 . Hash scope in this context means the number of ports that are a part of a link aggregate. For example, if links 60 A and 60 B are aggregated, then two ports (for example, at adapters 14 a and 14 b ) may be the hash scope.
In one embodiment, the hash type, hash scope and the hashing algorithm may be statically stored by an administrator (not shown) that configures the networking nodes. In another embodiment, the hash type, hash scope and algorithm may be dynamically exchanged, using a special packet while the nodes 12 and 54 are communicating.
In block S 210 , nodes 12 and 54 start packet transmission. The links for packet transmission are selected based on information exchanged in block S 208 .
In one embodiment, because the communicating nodes 12 and 54 agree on the hash type and the hash algorithm, the selected links are consistent and hence in an environment similar to FIG. 1B , one always receives packets via the same link that the packets are transmitted. Thus, the embodiments disclosed herein allow one to aggregate links, use multiple adapters and effectively use an offload module.
Although the present disclosure has been described with reference to specific embodiments, these embodiments are illustrative only and not limiting. Many other applications and embodiments of the present invention will be apparent in light of this disclosure and the following claims. References throughout this specification to “one embodiment” or “an embodiment” means that a particular feature, structure or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention. Therefore, it is emphasized and should be appreciated that two or more references to “an embodiment” or “one embodiment” or “an alternative embodiment” in various portions of this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures or characteristics being referred to may be combined as suitable in one or more embodiments of the invention, as will be recognized by those of ordinary skill in the art. | Method and system for a first network device and a second network device is provided. The first network device and the second network device communicate with each other via a plurality of network links. A network packet field for applying a hashing technique for selecting one of the network links to transmit the network packet is negotiated between the first network device and the second network device. The hashing technique is identified for selecting the selected network link. The first network device and the second network device, prior to applying the hashing technique exchange hashing parameters. | 8 |
CROSS-REFERENCE TO RELATED APPLICATION
This application is a 35 USC 371 application of PCT/EP2009/052954 filed on Mar. 13, 2009.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a machine tool, in particular a handheld power tool, having an electrical drive motor.
2. Description of the Prior Art
For cooling the motor, handheld power tools with an electrical drive motor, such as angle sanders, have a fan wheel in the housing, which is driven by the motor and generates a cooling air flow that is guided through the housing of the handheld power tool. Since in operation of the handheld power tool in machining a workpiece, abrasive dirt particles are created that are carried via the cooling air flow into the interior of the housing, there is the risk of soiling of the drive motor as well as other parts of the machine tool that are located in the housing. The abrasive particles can become deposited in the housing and lead to wear at pole piece winding overhangs of the electrical drive motor, for instance, which can trip a short circuit with an attendant functional failure. Moreover, the dirt particles increase friction and impair the cooling capacity of the cooling air flow, thus reducing the heat dissipation.
OBJECT AND ADVANTAGES OF THE INVENTION
It is the object of the invention to ensure the functional capability of a machine tool over a long period of operation.
The embodiment according to the invention is suitable for use in machine tools, in particular in handheld power tools, having an electrical drive motor, preferably electric handheld tools, which are used for sanding or some other metal-cutting machining operation. An alternating current motor, in particular a series-wound motor is preferably used as the electrical drive motor. Optionally, a direct current motor, such as a permanently excited motor, may also be used. The electrical drive motor has pole pieces for improved guidance of the magnetic field; the drive motor is furthermore assigned a fan wheel, which is driven by the armature shaft of the drive motor and by way of which a cooling air flow is generated for cooling the motor as well as other components of the machine tool. The cooling air flow is introduced into the housing of the machine tool, carried past the drive motor, and guided back out of the housing again via outflow openings.
According to the invention, in the housing an air guide element is provided, which is preferably disposed on a face end of the electric motor and forms a portion of the flow course of the cooling air flow inside the housing. The air guide element covers the pole pieces at least partially, so that the applicable portion of the pole pieces is located outside the flow course of the cooling air flow.
This embodiment has the advantage that the pole pieces are protected against the abrasive dirt particles that are entrained with the cooling air flow. The abrasive dust cannot become deposited on the pole pieces, particularly on winding overhangs of the pole pieces. The pole pieces are protected mechanically against soiling by the air guide element.
A further advantage resides in the optimized flow course, particularly in the vicinity of the pole pieces, since the air guide element, for protecting the pole pieces, additionally also forms a part of the flow course of the cooling air flow, and by way of the shape of the air guide element, an influence can be exerted on the flow. Moreover, air eddies are avoided in the vicinity of the pole pieces, which are disposed on the side of the air guide element remote from the flow course. Since interfering influences on the flow course, which are associated with pressure differences, are eliminated or at least reduced, a more tolerable noise pattern is also achieved, since no high frequencies and only slight amplitudes are generated in the flow.
In addition, noise shielding of the rotor of the electrical drive motor is also attained, so that less motor noise reaches the outside. Finally, there is less power loss in the electrical drive motor, because less turbulence, which draws mechanical energy from the drive motor as a result of pressure fluctuations, occurs.
In a preferred refinement, the air guide element has a pole piece receiving portion that receives the face end of the pole pieces and is located outside the flow course of the cooling air flow. The air guide element is preferably embodied as an air guide ring, and the pole piece receiving portion expediently forms an annular chamber which is located radially outside a cylindrical air guide stub that is a component of the air guide ring. The air guide stub, on one side, defines the flow course of the cooling air flow, and on the opposite side of its wall it defines the pole pieces, which are covered by the stub. Advantageously, the pole pieces are located radially outside the flow course, so that the pole piece receiving portion, embodied as an annular chamber, in the air guide ring is likewise located outside the flow course. Accordingly, the cooling air flow is carried axially through the motor between the armature of the electric motor, preferably embodied as an internal rotor motor, and the stator. With this air guidance, not only the stator parts but also the armature or rotor parts of the electric motor are cooled.
It may be expedient, in the air guide element disposed on an axial face end of the electric motor, to provide additional flow elements, such as at least one flow scoop protruding into the flow course and oriented in particular radially to the flow course, for the sake of achieving an improved or in a certain way desired flow guidance. The flow scoop can then be a fixed, invariable component of the air guide ring, or in an alternative version, it can be retained movably on the air guide element, for instance by way of a film hinge or the like.
The flow stub in the air guide ring serves in particular to receive the fan wheel, which is disposed coaxially to the armature or rotor shaft of the electric motor and is connected to the rotor in a manner fixed against relative rotation. The flow stub here communicates with the receiving chamber in the air guide element, in which the fan wheel is rotatably supported. The air guide element and the fan wheel thus form a structural unit, creating a so-called impeller, or in other words an encapsulated propeller.
BRIEF DESCRIPTION OF THE DRAWINGS
Further advantages and expedient embodiments can be learned from the further claims, the description of the drawings, and the drawings. In the drawings:
FIG. 1 is a schematic illustration of an electric handheld power tool;
FIG. 2 is a perspective view of an electric motor in the handheld power tool, having an air guide ring disposed on an axial face end of the motor;
FIG. 3 shows the electric motor including the air guide ring in a further perspective view;
FIG. 4 is a section through the electric motor including the air guide ring;
FIG. 5 shows the air guide ring in an individual perspective view; and
FIG. 6 shows the air guide ring in a further version, with additional flow scoops, oriented radially to the flow course.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the drawings, identical components are identified by the same reference numerals.
The handheld power tool 1 shown in general fashion in FIG. 1 has, in a housing 2 , an electrical drive motor 3 , which is embodied in particular as an alternating current motor, preferably as a series-wound motor, but a direct current motor can also be considered. The rotor shaft or armature shaft 11 of the drive motor 3 has an axis 4 and is rotationally coupled to a tool shaft 5 supported rotatably in the housing and drives that shaft. A tool 6 for machining a workpiece is located on the tool shaft 5 .
As can be seen from FIGS. 2 and 3 , the electrical drive motor 3 has pole pieces 7 , which are embodied in particular as winding overhangs and form a component of the stator of the drive motor. A magnetic return part 8 annularly surrounding the pole pieces 7 is also present and may optionally have permanent magnets as well.
On a face end of the electrical drive motor 3 , an air guide ring 9 is located coaxially to the rotor shaft or armature shaft 11 of the drive motor, and in this ring 9 , a fan wheel 10 shown only symbolically revolves rotatably and is coupled to the shaft 11 in a manner fixed against relative rotation. The air guide ring 9 embraces the fan wheel 10 , and the two components together form an impeller.
As can be seen from FIG. 3 , the air guide ring 9 has a radially tapered, axially extending air guide stub 12 , which is embodied in one piece with the air guide ring and is preferably made from a plastic. The air guide stub 12 serves the purpose of flow guidance of cooling air that is guided through the housing of the handheld power tool and in particular is guided axially through the radial region between the armature and the stator of the electric motor. The air guide stub 12 forms a part of the flow course for the cooling air flow. The outside of the air guide stub 12 , conversely, defines the axial face end of the pole pieces 7 .
As can be seen from the sectional view in FIG. 4 , radially outside the cylindrical air guide stub 12 , an annular chamber 13 is formed in the air guide ring 9 , for receiving the face end of the pole pieces 7 . The annular chamber 13 forms a pole piece receiving portion and is defined radially on the inside by the wall of the air guide stub 12 and radially on the outside by a further wall 14 , which is embodied in one part or in one piece with the air guide ring 9 .
Radially between the armature 16 and the radially embracing stator parts, such as the magnetic return part 8 , an axially extending flow course 15 through the drive motor 3 is formed for the cooling air that is aspirated into the housing by the revolution of the fan wheel. The flow course 15 discharges into the air guide stub 12 of the air guide ring 9 . In this way, the cooling air flow flows through the drive motor 3 over its axial length and is guided out of the air guide ring 9 axially via the open face end located facing the air guide stub 12 .
In FIG. 5 , the air guide ring 9 is shown again in an individual perspective view. The air guide stub 12 can be seen, which has approximately half the diameter of the outer diameter of the air guide ring 9 . In the axial direction, the air guide stub 12 occupies at most half the length of the entire axial length of the air guide ring 9 .
In FIG. 6 , an air guide ring 9 is shown in a modified version. Two diametrically opposed, radially outward-opening flow scoops 17 are formed in one part with the air guide stub 12 ; they form a component of the wall of the air guide stub 12 , but opposite the cylinder wall are widened with a radial component and extend outward. The flow scoops 17 open in the direction of the annular chamber 13 , which serves to receive the pole pieces. Thus a flow course is opened between the interior of the air guide stub 12 , as a component of the flow course, and the annular chamber 13 , so that a partial flow of the cooling air flow can enter the annular chamber 13 radially via the opened flow scoops 17 and ensures an additional cooling of the pole scoops.
The flow scoops 17 are optionally embodied movably and are meant to be adjusted between the open position, shown, and a closed position, in which positions the flow scoops 17 are located in the wall of the air guide stub 12 , so that a radial crossover of cooling air is not possible. The pivotability of the flow scoops 17 can be formed for instance via a film hinge, by way of which the flow guide scoops are connected to the wall of the air guide stub 12 . Fundamentally, however, a fixed, immovable embodiment of the flow scoops 17 is also possible.
The foregoing relates to the preferred exemplary embodiments of the invention, it being understood that other variants and embodiments thereof are possible within the spirit and scope of the invention, the latter being defined by the appended claims. | A machine tool, in particular a powered hand tool, has an electric drive motor to which pole shoes are assigned in order to conduct a magnetic field. Furthermore, a fan wheel is provided in order to produce a stream of cooling air. In the housing, an air-guiding element forms a portion of the flow path for the stream of cooling air. According to the invention, the air-guiding element at least partially covers the pole shoes. | 1 |
This is a continuation of application Ser. No.: 09/284,223, filed Apr. 9, 1999, which is a 371 of PCT/US97/18272, filed Oct. 9, 1997; which claims the benefit of Provisional application No. 60/028,459, filed Oct. 9, 1996.
FIELD OF THE INVENTION
The present invention relates to a new method of treatment using compounds which are dual non-selective β-adrenoceptor and α 1 -adrenoceptor antagonists, in particular the carbazolyl-(4)-oxypropanolamine compounds of Formula I, preferably carvedilol, for inhibiting stress-activated protein kinases (SAPKs). This invention also relates to a method of treatment using compounds which are dual non-selective β-adrenoceptor and α 1 -adrenoceptor antagonists, in particular the carbazolyl-(4)-oxypropanolamine compounds of Formula I, preferably carvedilol, for treating diseases mediated by stress-activated protein kinases.
BACKGROUND OF THE INVENTION
Cells respond to extracellular stimuli by activating signal transduction pathways, which culminate in gene expression. A critical component of eukaryotic signal transduction is the activation of protein kinases, which phosphorylate a host of cellular substrates. Certain protein serine/threonine kinases transduce signals to the nucleus of cells in response to cellular stresses. These kinases are known as stress-activated protein kinases (SAPKs), or, alternately, c-Jun N-terminal (amino-terminal kinases (JNKs), and likely play a role in the genetic response of many components of the cardiovascular system to disease processes [Force, et al., Circulation Research, 78(6): 947-953 (1996)]. Stress-activated protein kinases activate genes responsible for apoptosis (cell death); SAPK activation precedes the onset of apoptosis.
Surprisingly, it has been found that carvedilol, a dual non-selective β-adrenoceptor and α 1 -adrenoceptor antagonist, inhibits stress-activated protein kinases. This inhibition means that carvedilol and related Formula I compounds are useful in treating diseases mediated by stress-activated protein kinases. Importantly, this inhibition means that carvedilol and related Formula I compounds are useful for treating SAPK-initiated apoptosis. This inhibition also means that carvedilol and related Formula I compounds are useful for treating cardiovascular diseases, such as ischemia, atherosclerosis, heart failure, and restenosis.
SUMMARY OF THE INVENTION
The present invention provides a new method of treatment using compounds which are dual non-selective β-adrenoceptor and a α 1 -adrenoceptor antagonists, in particular the carbazolyl-(4)-oxypropanolamine compounds of Formula I, preferably carvedilol, for inhibiting stress-activated protein kinases, in mammals, particularly humans. The present invention also provides a method of treatment using said compounds for treating diseases mediated by stress-activated protein kinases. Additionally, this invention provides a method for treating SAPK-initiated apoptosis using the compounds of Formula I. This invention further provides a method of treatment using dual non-selective β-adrenoceptor and α 1 -adrenoceptor antagonists, in particular carvedilol, in the treatment of cardiovascular disorders, such as ischemia, atherosclerosis, heart failure, and restenosis following angioplasty.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides a new method for inhibiting stress-activated protein kinases using compounds which are dual non-selective β-adrenoceptor and α 1 -adrenoceptor antagonists. Preferably, this invention provides a new method for inhibiting stress-activated protein kinases using compounds of Formula I:
wherein:
R 7 -R 13 are independently —H or —OH; and
A is a moiety of Formula II:
wherein:
R 1 is hydrogen, lower alkanoyl of up to 6 carbon atoms or aroyl selected from benzoyl and naphthoyl;
R 2 is hydrogen, lower alkyl of up to 6 carbon atoms or arylalkyl selected from benzyl, phenylethyl and phenylpropyl;
R 3 is hydrogen or lower alkyl of up to 6 carbon atoms;
R 4 is hydrogen or lower alkyl of up to 6 carbon atoms, or when X is oxygen, R 4 together with R 5 can represent —CH 2 —0—;
X is a single bond, —CH 2 , oxygen or sulfur;
Ar is selected from phenyl, naphthyl, indanyl and tetrahydronaphthyl;
R 5 and R 6 are individually selected from hydrogen, fluorine, chlorine, bromine, hydroxyl, lower alkyl of up to 6 carbon atoms, a —CONH 2 — group, lower alkoxy of up to 6 carbon atoms, benzyloxy, lower alkylthio of up to 6 carbon atoms, lower alkysulphinyl of up to 6 carbon atoms and lower alkylsulphonyl of up to 6 carbon atoms; or
R 5 and R 6 together represent methylenedioxy; and pharmaceutically acceptable salts thereof.
More preferably, the present invention provides a new method for inhibiting stress-activated protein kinases using compounds of Formula III:
wherein:
R 1 is hydrogen, lower alkanoyl of up to 6 carbon atoms or aroyl selected from benzoyl and naphthoyl;
R 2 is hydrogen, lower alkyl of up to 6 carbon atoms or arylalkyl selected from benzyl, phenylethyl and phenylpropyl;
R 3 is hydrogen or lower alkyl of up to 6 carbon atoms;
R 4 is hydrogen or lower alkyl of up to 6 carbon atoms, or when X is oxygen, R 4 together with R 5 can represent —CH 2 —0—;
X is a valency bond, —CH 2 , oxygen or sulfur,
Ar is selected from phenyl, naphthyl, indanyl and tetrahydronaphthyl;
R 5 and R 6 are individually selected from hydrogen, fluorine, chlorine, bromine, hydroxyl, lower alkyl of up to 6 carbon atoms, a —CONH 2 — group, lower alkoxy of up to 6 carbon atoms, benzyloxy, lower alkylthio of up to 6 carbon atoms, lower alkysulphinyl of up to 6 carbon atoms and lower alkylsulphonyl of up to 6 carbon atoms; or
R 5 and R 6 together represent methylenedioxy; and pharmaceutically acceptable salts thereof.
Most preferably, the present invention provides a new method for inhibiting stress-activated protein kinases using a compound of Formula IV, better known as carvedilol or (1-(carbazol-4-yloxy-3-[[2-(o-methoxyphenoxy)ethyl]amino]-2-propanol):
The compounds of the present invention are novel multiple action drugs useful in the treatment of mild to moderate hypertension. Carvedilol is known to be both a competitive non-selective β-adrenoceptor antagonist and a vasodilator, and is also a calcium channel antagonist at higher concentrations. The vasodilatory actions of carvedilol result primarily from α 1 -adrenoceptor blockade, whereas the β-adrenoceptor blocking activity of the drug prevents reflex tachycardia when used in the treatment of hypertension. These multiple actions of carvedilol are responsible for the antihypertensive efficacy of the drug in animals, particularly in humans. See Willette, R. N., Sauermelch, C. F. & Ruffolo, R. R., Jr. (1990) Eur. J. Pharmacol., 176, 237-240; Nichols, A. J., Gellai, M. & Ruffolo, R. R., Jr. (1991) Fundam. Clin. Pharmacol., 5, 25-38; Ruffolo, R. R., Jr., Gellai, M., Hieble, J. P., Willette, R. N. & Nichols, A. J. (1990) Eur. J. Clin. PharmacoL, 38, S82-S88; Ruffolo, R. R., Jr., Boyle, D. A., Venuti, R. P. & Lukas, M. A. (1991) Drugs of Today, 27, 465-492; and Yue, T. -L., Cheng, H., Lysko, P. G., Mckenna, P. J., Feuerstein, R., Gu, J., Lysko, K. A., Davis, L. L. & Feuerstein, G. (1992) J. Pharmacol. Exp. Ther., 263, 92-98.
The antihypertensive action of carvedilol is mediated primarily by decreasing total peripheral vascular resistance without causing the concomitant reflex changes in heart rate commonly associated with other antihypertensive agents. Willette, R. N., et al. supra; Nichols, A. J., et al. supra; Ruffolo. R. R., Jr., Gellai, M., Hieble, J. P., Willette, R. N. & Nichols, A. J. (1990) Eur. J. Clin. Pharmacol., 38, S82-S88 . . . Carvedilol also markedly reduces infarct size in rat, canine and porcine models of acute myocardial infarction, Ruffolo, R. R., Jr., et al., Drugs of Today, supra, possibly as a consequence of its antioxidant action in attenuating oxygen free radical-initiated lipid peroxidation. Yue, T.-L., et al. sapra.
Recently, it has been discovered that compounds which are dual non-selective β-adrenoceptor and α 1 -adrenoceptor antagonists, in particular the compounds of Formula I, preferably carvedilol, inhibit stress-activated protein kinases. Based on this mechanism of action, the instant compounds can be used to treat diseases wherein inhibition of stress-activated protein kinases is indicated. In particular, the compounds of the present invention, preferably carvedilol, can be used for blocking SAPK-induced apoptosis, particularly in cardiac cells or in neuronal cells. Therefore, the compounds of Formula I are useful in treating cardiovascular diseases and neurodegenerative disorders.
Some of the compounds of Formula I are known to be metabolites of carvedilol. Certain preferred compounds of the present invention, that is, the compounds of Formula I wherein A is the moiety of Formula II wherein R1 is —H, R2 is —H, R3 is —H, R4 is —H, X is O, Ar is phenyl, R5 is ortho —OH, and R6 is —H, and one of R 7 , R 9 , or R 10 is —OH, are metabolites of carvedilol.
Compounds of Formula I may be conveniently prepared as described in U.S. Pat. No. 4,503,067. Reference should be made to said patent for its full disclosure, the entire disclosure of which is incorporated herein by reference.
Pharmaceutical compositions of the compounds of Formula I, including carvedilol, may be administered to patients according to the present invention in any medically acceptable manner, preferably orally. For parenteral administration, the pharmaceutical composition will be in the form of a sterile injectable liquid stored in a suitable container such as an ampoule, or in the form of an aqueous or nonaqueous liquid suspension. The nature and composition of the pharmaceutical carrier, diluent or excipient will, of course, depend on the intended route of administration, for example whether by intravenous or intramuscular injection Pharmaceutical compositions of the compounds of Formula I for use according to the present invention may be formulated as solutions or lyophilized powders for parenteral administration. Powders may be reconstituted by addition of a suitable diluent or other pharmaceutically acceptable carrier prior to use. The liquid formulation is generally a buffered, isotonic, aqueous solution. Examples of suitable diluents are normal isotonic saline solution, standard 5% dextrose in water or buffered sodium or ammonium acetate solution. Such formulation is especially suitable for parenteral administration, but may also be used for oral administration or contained in a metered dose inhaler or nebulizer for insufflation. It may be desirable to add excipients such as ethanol, polyvinyl-pyrrolidone, gelatin, hydroxy cellulose, acacia, polyethylene glycol, mannitol, sodium chloride or sodium citrate.
Alternatively, these compounds may be encapsulated, tableted or prepared in a emulsion or syrup for oral administration. Pharmaceutically acceptable solid or liquid carriers may be added to enhance or stabilize the composition, or to facilitate preparation of the composition. Liquid carriers include syrup, peanut oil, olive oil, glycerin, saline, ethanol, and water. Solid carriers include starch, lactose, calcium sulfate dihydrate, terra alba, magnesium stearate or stearic acid, talc, pectin, acacia, agar or gelatin. The carrier may also include a sustained release material such as glyceryl monostearate or glyceryl distearate, alone or with a wax. The amount of solid carrier varies but, preferably, will be between about 20 mg to about 1 g per dosage unit. The pharmaceutical preparations are made following the conventional techniques of pharmacy involving milling, mixing, granulating, and compressing, when necessary, for tablet forms; or milling, mixing and filling for hard gelatin capsule forms. When a liquid carrier is used, the preparation will be in the form of a syrup, elixir, emulsion or an aqueous or non-aqueous suspension. Such a liquid formulation may be administered directly p.o. or filled into a soft gelatin capsule.
Dosing in humans for the treatment of disease according to the present invention should not exceed a dosage range of from about 3.125 to about 50 mg of the compounds of Formula I, particularly carvedilol, preferably given twice daily. As one of ordinary skill in the art will readily comprehend, the patient should be started on a low dosage regimen of the desired compound of Formula I, particularly carvedilol, and monitered for well-known symptoms of intolerance, e.g., fainting, to such compound. Once the patient is found to tolerate such compound, the patient should be brought slowly and incrementally up to the maintenance dose. The choice of initial dosage most appropriate for the particular patient is determined by the practitioner using well-known medical principles, including, but not limited to, body weight. In the event that the patient exhibits medically acceptable tolerance of the compound for two weeks, the dosage is doubled at the end of the two weeks and the patient is maintained at the new, higher dosage for two more weeks, and observed for signs of intolerance. This course is continued until the patient is brought to a maintenance dose
It will be appreciated that the actual preferred dosages of the compounds being used in the compositions of this invention will vary according to the particular composition formulated, the mode of administration, the particular site of administration and the host being treated.
No unacceptable toxicological effects are expected when the compounds of Formula I, including the compound of Formula II, are used according to the present invention.
The experimentals which follow are not intended to limit the scope of this invention, but are provided to illustrate how to use the compounds of this invention. Many other embodiments will be readily apparent to those skilled in the art.
Experimental
Heart perfusion and tissue extraction
Male New Zealand white rabbits (2.5-3.1 kg) were anesthetized with sodium pentobarbital, 10 mgc/kg, and the hearts removed rapidly and placed in cold Krebs-Henseleit bicarbonate-buffered saline supplemented with 10 mM glucose and equilibrated with 95% O 2 /5% CO 2 . The temperature of the perfusates and the hearts was maintained at 37° C. After equilibration (20 min), the perfusion was interrupted for 30 min unless otherwise indicated by switching off the perfusion pump, and the hearts were thus rendered globally ischemic. Reperfusion was initiated by restarting the pump. Carvedilol or propranolol was infused via a syringe pump to give a final concentration of 10 μM or a concentration indicated when reperfusion was started. Control hearts were perfused for up to 50 minutes after the preequilibration without interruption to the perfusate flow. At the end of the perfusion period, hearts ventricles were “freeze-clamped” using aluminum tongs precooled in liquid N 2 and pulverized under liquid N.. The powders were resuspended in ice-cold lysis buffer. Extracts were incubated for 5 min at 4° C. The detergent-soluble supernatant fractions were retained, and protein content was measured.
Stress-activated protein kinase (SAPK/JNK) assay
Fusion protein, GST-c-Jun (1-81) was made according to the method described by Hibi et al (14). The cDNA clone with a sequence encoding human c-Jun amino acids 1-81 was provided by Human Genome Sciences (HGS)(Gaithesberg, MD) and subcloned into a pGEX 4T-3 which contains a DNA sequence encoding glutathione-S-transferase (GST). The GST-cJun expression Vector, pGEX4T-3/c-Jun, was transformed into E.Coli. Expression of GST-c-Jun (1-81) fusion protein was induced by isopropyl-β-thiogalactoside (IPTG). E.Coli were lysed and centrifuged. The fusion protein, GST-c-Jun (1-81) was purified by glutathione-Sepharose chromatography.
SAPK/JNK assay
For analysis of protein kinases that bind c-Jun (“pull-down” assays), detergent-soluble extracts (100 μL, 0.5 mg protein) were added to 4 μ of GST-c Jun 1-81 . After incubation (4° C., 1 hour), glutathione-Sepharose was added, and the incubation was continued with mixing (4° C., 1 hour). Pellets were washed in lysis buffer A containing 75 mmol/L NaCl, then in buffer A (mmol/L: HEPES 20, MgCl 2 2.5, ED)TA 0.1, and β-glycerophosphate 20, pH 7.7) containing 75 mrmnol/L NaCl and 0.05% (vol/vo/) Triton X-100, and finally in buffer A alone. Phosphorylation of GST-c Jun 1-81 , by JNK/SAPKs was initiated with 30 μL of kinase assay buffer (mmol/L: HEPES 20, MgCl 2 20,β-glycerophosphate 20, DTT 2, and Na 3 VO 4 0.1, pH 7.6) containing 20 μmol/L ATP and 1 to 2 μCi [y- 32 P] ATP (Amersham International). After 20 minutes at 30° C., the reaction was terminated by centrifugation. The pellet was washed in cold buffer A containing 75 mmolnL NaCl and 0.05% (vol/vol) Triton X-100. Phosphorylated proteins in the pellet were eluted by boilingin SDS-PAGE sample buffer and then separated by SDS-PAGE. Gels were stained with Coomassie blue to identifythe 46-kD GST-c-Jun 1-81 . After autoradiography phosplorlmager was used to quantify the band intensities of c-Jun 1-81 .
Results
Ischemia-reperfusion activated SAPK in a time-dependent manner and peaked at 20 min after reprefusion as shown in FIG. 1 .
Carvedilol, administered at the beginning of reperfusion reduced the activation of SAPK by 51.2% and 30.7% at 1 and 10 μM, respectively. Under the same condition, propranolol, at 10 μM, had no effect on SAPK activation by ischemia-reperfusion as shown in FIG. 2 .
The foregoing is illustrative of the use of the compounds of this invention. This invention, however, is not limited to the precise embodiment described herein, but encompasses all modifications within the scope of the claims which follow. | This invention relates to a method for inhibiting stress-activated protein kinases (SAPKs) which comprises administering to a mammal in need thereof an effective amount of a compound which is a dual non-selective β-adrenoceptor and α 1 -adrenoceptor antagonist. | 0 |
RELATED APPLICATIONS
[0001] This application is a divisional of application Ser. No. 11/319,975, filed Dec. 29, 2005, which claims the benefit of provisional application Ser. No. 60/640,510, filed on Dec. 30, 2004, and application Ser. No. 11/034,737, filed on Jan. 13, 2005, the teachings and contents all of which are hereby incorporated by reference.
SEQUENCE LISTING
[0002] This application contains a sequence listing in paper format and in computer readable format, the teachings and content of which are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
[0003] 1. Field of the Invention
[0004] One aspect of the present invention is concerned with the recovery of a protein expressed by open reading frame 2 (ORF2) of porcine circovirus type 2 (PCV2). More particularly, the protein is a recombinant protein expressed by a transfected virus containing recombinant coding sequences for porcine circovirus type 2, open reading frame 2. Still more particularly, the transfected virus is permitted to infect cells in growth media and the protein expressed by open reading frame 2 is recovered in the supernate, rather than from inside the cells. Even more particularly, the method involves the steps of amplifying the open reading frame 2 gene from porcine circovirus type 2, cloning this amplified portion into a first vector, excising the open reading frame 2 portion from this first vector and cloning it into a transfer vector, cotransfecting the transfer vector with a viral vector into cells in growth media, causing the cells to become infected by the viral vector and thereby express open reading frame 2, and recovering the expressed recombinant protein coded for by open reading frame 2 in the supernate.
[0005] In another aspect, the present invention is concerned with an immunogenic composition effective for inducing an immune response against PCV2, and methods for producing those immunogenic compositions. More particularly, the present invention is concerned with an immunological composition effective for providing an immune response that protects an animal receiving the composition and reduces, or lessens the severity, of the clinical symptoms associated with PCV2 infection. Still more particularly, the present invention is concerned with a protein-based immunological composition that confers effective protection against infection by PCV2. Even more particularly, the present invention is concerned with an immunological composition comprising ORF2 of PCV2, wherein administration of PCV2-ORF2 results in protection against infection by PCV2. Most particularly, the present invention is concerned with an immunological composition effective for conferring effective immunity to a swine receiving the immunological composition, and wherein the composition comprises the protein expressed by ORF2 of PCV2.
[0006] 2. Description of the Prior Art
[0007] Porcine circovirus type 2 (PCV2) is a small (17-22 nm in diameter), icosahedral, non-enveloped DNA virus, which contains a single-stranded circular genome. PCV2 shares approximately 80% sequence identity with porcine circovirus type 1 (PCV1). However, in contrast with PCV1, which is generally non-virulent, swine infected with PCV2 exhibit a syndrome commonly referred to as Post-weaning Multisystemic Wasting Syndrome (PMWS). PMWS is clinically characterized by wasting, paleness of the skin, unthriftiness, respiratory distress, diarrhea, icterus, and jaundice. In some affected swine, a combination of all symptoms will be apparent while other swine will only have one or two of these symptoms. During necropsy, microscopic and macroscopic lesions also appear on multiple tissues and organs, with lymphoid organs being the most common site for lesions. A strong correlation has been observed between the amount of PCV2 nucleic acid or antigen and the severity of microscopic lymphoid lesions. Mortality rates for swine infected with PCV2 can approach 80%. In addition to PMWS, PCV2 has been associated with several other infections including pseudorabies, porcine reproductive and respiratory syndrome (PRRS), Glasser's disease, streptococcal meningitis, salmonellosis, postweaning colibacillosis, dietetic hepatosis, and suppurative bronchopneumonia.
[0008] Open reading frame 2 (ORF2) protein of PCV2, having an approximate molecular weight of 30 kDa when run on SDS-PAGE gel, has been utilized in the past as an antigenic component in vaccines for PCV2. Typical methods of obtaining ORF2 for use in such vaccines generally consist of amplifying the PCV2 DNA coding for ORF2, transfecting a viral vector with the ORF2 DNA, infecting cells with the viral vector containing the ORF2 DNA, permitting the virus to express ORF2 protein within the cell, and extracting the ORF2 protein from the cell via cell lysis. These procedures generally take up to about four days after infection of the cells by the viral vector. However, these procedures have a disadvantage in that the extraction procedures are both costly and time-consuming. Additionally, the amount of ORF2 recovered from the cells is not very high; consequently, a large number of cells need to be infected by a large number of viral vectors in order to obtain sufficient quantities of the recombinant expressed protein for use in vaccines and the like.
[0009] Current approaches to PCV2 immunization include DNA-based vaccines, such as those described in U.S. Pat. No. 6,703,023. However, such vaccines have been ineffective at conferring protective immunity against PCV2 infection and the clinical signs associated therewith.
[0010] Accordingly, what is needed in the art is a method of obtaining ORF2 protein, which does not require extraction of the ORF2 protein from within infected cells. What is further needed are methods of obtaining recombinant ORF2 protein in quantities sufficient for efficiently preparing vaccine compositions. What is still further needed are methods for obtaining ORF2 protein which do not require the complicated and labor-intensive methods required by the current ORF2 protein extraction protocols. Finally, with respect to compositions, what is needed in the art is an immunogenic composition which does confer protective immunity against PCV2 infection and lessens the severity of or prevents the clinical signs associated therewith.
SUMMARY OF THE INVENTION
[0011] The present invention overcomes the problems inherent in the prior art and provides a distinct advance in the state of the art. Specifically, one aspect of the present invention provides improved methods of producing and/or recovering recombinant PCV2 ORF2 protein, i) by permitting infection of susceptible cells in culture with a recombinant viral vector containing PCV2 ORF2 DNA coding sequences, wherein ORF2 protein is expressed by the recombinant viral vector, and ii) thereafter recovering the ORF2 in the supernate. It has been unexpectedly discovered that ORF2 is released into the supernate in large quantities if the infection and subsequent incubation of the infected cells is allowed to progress past the typical prior PCV 2 ORF2 recovery process, which extracts the PCV2 ORF2 from within cells. It furthermore has been surprisingly found, that PCV ORF2 protein is robust against prototypical degradation outside of the production cells. Both findings together allow a recovery of high amounts of PCV2 ORF2 protein from the supernate of cell cultures infected with recombinant viral vectors containing a PCV2 ORF2 DNA and expressing the PCV2 ORF2 protein. High amounts of PCV2 ORF2 protein means more than about 20 μg/mL supernate, preferably more than about 25 μg/mL, even more preferred more than about 30 μg/mL, even more preferred more than about 40 μg/mL, even more preferred more than about 50 μg/mL, even more preferred more than about 60 μg/mL, even more preferred more than about 80 μg/mL, even more preferred more than about 100 μg/mL, even more preferred than about 150 μg/mL, most preferred than about 190 μg/mL. Those expression rates can also be achieved for example by the methods as described in Examples 1 to 3.
[0012] Preferred cell cultures have a cell count between about 0.3-2.0×10 6 cells/mL, more preferably from about 0.35-1.9×10 6 cells/mL, still more preferably from about 0.4-1.8×10 6 cells/mL, even more preferably from about 0.45-1.7×10 6 cells/mL, and most preferably from about 0.5-1.5×10 6 cells/mL. Preferred cells are determinable by those of skill in the art. Preferred cells are those susceptible for infection with an appropriate recombinant viral vector, containing a PCV2 ORF2 DNA and expressing the PCV2 ORF2 protein. Preferably the cells are insect cells, and more preferably, they include the insect cells sold under the trademark Sf+ insect cells (Protein Sciences Corporation, Meriden, Conn.).
[0013] Appropriate growth media will also be determinable by those of skill in the art with a preferred growth media being serum-free insect cell media such as Excell 420 (JRH Biosciences, Inc., Lenexa, Kans.) and the like. Preferred viral vectors include baculovirus such as BaculoGold (BD Biosciences Pharmingen, San Diego, Calif.), in particular if the production cells are insect cells. Although the baculovirus expression system is preferred, it is understood by those of skill in the art that other expression systems will work for purposes of the present invention, namely the expression of PCV2 ORF2 into the supernatant of a cell culture. Such other expression systems may require the use of a signal sequence in order to cause ORF2 expression into the media. It has been surprisingly discovered that when ORF2 is produced by a baculovirus expression system, it does not require any signal sequence or further modification to cause expression of ORF2 into the media. It is believed that this protein can independently form virus-like particles (Journal of General Virology Vol. 81, pp. 2281-2287 (2000) and be secreted into the culture supernate. The recombinant viral vector containing the PCV2 ORF2 DNA sequences has a preferred multiplicity of infection (MOI) of between about 0.03-1.5, more preferably from about 0.05-1.3, still more preferably from about 0.09-1.1, and most preferably from about 0.1-1.0, when used for the infection of the susceptible cells. Preferably the MOIs mentioned above relates to one mL of cell culture fluid. Preferably, the method described herein comprises the infection of 0.35-1.9×10 6 cells/mL, still more preferably of about 0.4-1.8×10 6 cells/mL, even more preferably of about 0.45-1.7×10 6 cells/mL, and most preferably of about 0.5-1.5×10 6 cells/mL with a recombinant viral vector containing a PCV2 ORF2 DNA and expressing the PCV2 ORF protein having a MOI (multiplicity of infection) of between about 0.03-1.5, more preferably from about 0.05-1.3, still more preferably from about 0.09-1.1, and most preferably from about 0.1-1.0.
[0014] The infected cells are then incubated over a period of up to ten days, more preferably from about two days to about ten days, still more preferably from about four days to about nine days, and most preferably from about five days to about eight days. Preferred incubation conditions include a temperature between about 22-32° C., more preferably from about 24-30° C., still more preferably from about 25-29° C., even more preferably from about 26-28° C., and most preferably about 27° C. Preferably, the Sf+ cells are observed following inoculation for characteristic baculovirus-induced changes. Such observation may include monitoring cell density trends and the decrease in viability during the post-infection period. It was found that peak viral titer is observed 3-5 days after infection and peak ORF2 release from the cells into the supernate is obtained between days 5 and 8, and/or when cell viability decreases to less than 10%.
[0015] Thus, one aspect of the present invention provides an improved method of producing and/or recovering recombinant PCV2 ORF2 protein, preferably in amounts described above, by i) permitting infection of a number of susceptible cells (see above) in culture with a recombinant viral vector with a MOI as defined above, ii) expressing PCV2 ORF2 protein by the recombinant viral vector, and iii) thereafter recovering the PCV2 ORF2 in the supernate of cells obtained between days 5 and 8 after infection and/or cell viability decreases to less then 10%. Preferably, the recombinant viral vector is a recombinant baculovirus containing PCV2 ORF2 DNA coding sequences and the cells are Sf+ cells. Additionally, it is preferred that the culture be periodically examined for macroscopic and microscopic evidence of contamination or for atypical changes in cell morphology during the post-infection period. Any culture exhibiting any contamination should be discarded. Preferably, the expressed ORF2 recombinant protein is secreted by the cells into the surrounding growth media that maintains cell viability. The ORF2 is then recovered in the supernate surrounding the cells rather than from the cells themselves.
[0016] The recovery process preferably begins with the separation of cell debris from the expressed ORF2 in media via a separation step. Preferred separation steps include filtration, centrifugation at speeds up to about 20,000×g, continuous flow centrifugation, chromatographic separation using ion exchange or gel filtration, and conventional immunoaffinity methods. Those methods are known to persons skilled in the art for example by (Harris and Angel (eds.), Protein purification methods—a practical approach, IRL press Oxford 1995). The most preferred separation methods include centrifugation at speeds up to about 20,000×g and filtration. Preferred filtration methods include dead-end microfiltration and tangential flow (or cross flow) filtration including hollow fiber filtration dead-end micro filtration. Of these, dead-end microfiltration is preferred. Preferred pore sizes for dead-end microfiltration are between about 0.30-1.35 μm, more preferably between about 0.35-1.25 μm, still more preferably between about 0.40-1.10 μm, and most preferably between about 0.45-1.0 μm. It is believed that any conventional filtration membrane will work for purposes of the present invention and polyethersulfone membranes are preferred. Any low weight nucleic acid species are removed during the filtration step.
[0017] Thus, one further aspect of the present invention provides an improved method of producing and/or recovering recombinant PCV2 ORF2 protein, preferably in amounts described above, by i) permitting infection of a number of susceptible cells (see above) in culture with a recombinant viral vector with a MOI as defined above, ii) expressing PCV ORF2 protein by the recombinant viral vector, iii) recovering the PCV2 ORF2 in the supernate of cells obtained between days 5 and 8 after infection and/or cell viability decreases to less then 10%, and, iv) separating cell debris from the expressed PCV2 ORF2 via a separation step. Preferably, the recombinant viral vector is a baculovirus containing ORF2 DNA coding sequences and the cells are SF+ cells. Preferred separation steps are those described above. Most preferred is a dead-end microfiltration using a membrane having a pore size between about 0.30-1.35 μm, more preferably between about 0.35-1.25 μm, still more preferably between about 0.40-1.10 μm, and most preferably between about 0.45-1.0 μm.
[0018] For recovery of PCV2 ORF2 that will be used in an immunogenic or immunological composition such as a vaccine, the inclusion of an inactivation step is preferred in order to inactivate the viral vector. An “immunogenic or immunological composition” refers to a composition of matter that comprises at least one antigen which elicits an immunological response in the host of a cellular and/or antibody-mediated immune response to the composition or vaccine of interest. Usually, an “immunological response” includes but is not limited to one or more of the following effects: the production or activation of antibodies, B cells, helper T cells, suppressor T cells, and/or cytotoxic T cells and/or yd T cells, directed specifically to an antigen or antigens included in the composition or vaccine of interest. Preferably, the host will display either a therapeutic or protective immunological response such that resistance to new infection will be enhanced and/or the clinical severity of the disease reduced. Such protection will be demonstrated by either a reduction or lack of symptoms normally displayed by an infected host, a quicker recovery time and/or a lowered viral titer in the infected host. Thus, the present invention also relates to method of producing and/or recovering recombinant PCV2 ORF2 protein, preferably in amounts described above, by i) permitting infection of a number of susceptible cells (see above) in culture with a recombinant viral vector with a MOI as defined above, ii) expressing PCV ORF2 protein by the recombinant viral vector, iii) recovering the PCV2 ORF2 in the supernate of cells obtained between days 5 and 8 after infection and/or cell viability decreases to less then 10%, iv) separating cell debris from the expressed PCV2 ORF2 via a separation step, and v) inactivating the recombinant viral vector.
[0019] Preferably, this inactivation is done either just before or just after the filtration step, with after the filtration step being the preferred time for inactivation. Any conventional inactivation method can be used for purposes of the present invention. Thus, inactivation can be performed by chemical and/or physical treatments. In preferred forms, the volume of harvest fluids is determined and the temperature is brought to between about 32-42° C., more preferably between about 34-40° C., and most preferably between about 35-39° C. Preferred inactivation methods include the addition cyclized binary ethylenimine (BEI), preferably in a concentration of about 1 to about 20 mM, preferably of about 2 to about 10 mM, still more preferably of about 2 to about 8 mM, still more preferably of about 3 to about 7 mM, most preferably of about 5 mM. For example the inactivation includes the addition of a solution of 2-bromoethyleneamine hydrobromide, preferably of about 0.4M, which has been cyclized to 0.2M binary ethylenimine (BEI) in 0.3N NaOH, to the fluids to give a final concentration of about 5 mM BEI. Preferably, the fluids are then stirred continuously for 72-96 hours and the inactivated harvest fluids can be stored frozen at −40° C. or below or between about 1-7° C. After inactivation is completed a sodium thiosulfate solution, preferably at 1.0M is added to neutralize any residual BEI. Preferably, the sodium thiosulfate is added in equivalent amount as compared to the BEI added prior to for inactivation. For example, in the event BEI is added to a final concentration of 5 mM, a 1.0M sodium thiosulfate solution is added to give a final minimum concentration of 5 mM to neutralize any residual BEI.
[0020] Thus, one further aspect of the present invention relates to a method of producing recombinant PCV2 ORF2 protein, preferably in amounts described above, by i) permitting infection of a number of susceptible cells (see above) in culture with a recombinant viral vector with a MOI as defined above, ii) expressing PCV ORF2 protein by the recombinant viral vector, iii) recovering the PCV2 ORF2 in the supernate of cells obtained between days 5 and 8 after infection and/or cell viability decreases to less then 10%, iv) separating cell debris from the expressed PCV2 ORF2 via a separation step, and v) inactivating the recombinant viral vector. Preferably, the recombinant viral vector is a baculovirus containing ORF2 DNA coding sequences and the cells are SF+ cells. Preferred separation steps are those described above, most preferred is the filtration step. Preferred inactivation steps are those described above. Preferably, inactivation is performed between about 35-39° C. and in the presence of 2 to 8 mM BEI, still more preferred in the presence of about 5 mM BEI. It has been surprisingly found, that higher concentrations of BEI negatively affect the PCV2 ORF2 protein.
[0021] According to one further aspect of the present invention, the method described above also includes an neutralization step after step v). This step vi) comprises adding of an equivalent amount of an agent that neutralizes the inactivation agent within the solution. Preferably, if the inactivation agent is BEI, addition of sodium thiosulfate to an equivalent amount is preferred. Thus, according to a further aspect, step vi) comprises adding of a sodium thiosulfate solution to a final concentration of about 1 to about 20 mM, preferably of about 2 to about 10 mM, still more preferably of about 2 to about 8 mM, still more preferably of about 3 to about 7 mM most preferably of about 5 mM, when the inactivation agent is BEI.
[0022] In preferred forms and especially in forms that will use the recombinant PCV2 ORF2 protein in an immunogenic composition such as a vaccine, each lot of harvested ORF2 will be tested for inactivation by passage in the anchorage dependent, baculovirus susceptible Sf+ cells. In a preferred form of this testing, 150 cm 2 of appropriate cell culture monolayer is inoculated with 1.0 mL of inactivated PCV2 fluids and maintained at 25-29° C. for 14 days with at least two passages. At the end of the maintenance period, the cell monolayers are examined for cytopathogenic effect (CPE) typical of PCV2 ORF2 baculovirus. Preferably, positive virus controls are also used. Such controls can consist of one culture of Sf+ cells inoculated with a non-inactivated reference PCV2 ORF2 baculovirus and one flask of Sf+ cells that remain uninoculated. After incubation and passage, the absence of virus-infected cells in the BEI treated viral fluids would constitute a satisfactory inactivation test. The control cells inoculated with the reference virus should exhibit CPE typical of PCV2 ORF2 baculovirus and the uninoculated flask should not exhibit any evidence of PCV2 ORF2 baculovirus CPE. Alternatively, at the end of the maintenance period, the supernatant samples could be collected and inoculated onto a Sf+ 96 well plate, which has been loaded with Sf+ cells, and then maintained at 25-29° C. for 5-6 days. The plate is then fixed and stained with anti-PCV2 ORF2 antibody conjugated to FITC. The absence of CPE and ORF2 expression, as detected by IFA micoscopy, in the BEI treated viral fluids constitutes a satisfactory inactivation test. The control cells inoculated with the reference virus should exhibit CPE and IFA activity and the uninoculated flask should not exhibit any evidence of PCV2 ORF2 baculovirus CPE and contain no IFA activity.
[0023] Thus a further aspect of the present invention relates to an inactivation test for determining the effectiveness of the inactivation of the recombination viral vector, comprises the steps: i) contacting at least a portion of the culture fluid containing the recombinant viral vector with an inactivating agent, preferably as described above, ii) adding a neutralization agent to neutralize the inactivation agent, preferably as described above, and iii) determining the residual infectivity by the assays as described above.
[0024] After inactivation, the relative amount of recombinant PCV2 ORF2 protein in a sample can be determined in a number of ways. Preferred methods of quantitation include SDS-PAGE densitometry, ELISA, and animal vaccination studies that correlate known quantities of vaccine with clinical outcomes (serology, etc.). When SDS-PAGE is utilized for quantitation, the sample material containing an unknown amount of recombinant PCV2 ORF2 protein is run on a gel, together with samples that contain different known amounts of recombinant PCV2 ORF2 protein. A standard curve can then be produced based on the known samples and the amount of recombinant PCV2 ORF2 in the unknown sample can be determined by comparison with this standard curve. Because ELISAs are generally recognized as the industry standard for antigen quantitation, they are preferred for quantitation.
[0025] Thus, according to a further aspect, the present invention also relates to an ELISA for the quantification of recombinant PCV2 ORF2 protein. A preferred ELISA as provided herewith will generally begin with diluting the capture antibody 1:6000 or an appropriate working dilution in coating buffer. A preferred capture antibody is Swine anti-PCV2 PAb Prot. G purified, and a preferred coating buffer is 0.05M Carbonate buffer, which can be made by combining 2.93 g NaHCO 3 (Sigma Cat. No. S-6014, or equivalent) and 1.59 g NaCO 3 (Sigma Cat. No. S-6139, or equivalent). The mixture is combined with distilled water, or equivalent, to make one liter at a pH of 9.6±0.1. Next, the capture antibody is diluted 1:6000, or any other appropriate working dilution, in coating buffer. For example, for four plates, one would need 42 mLs of coating buffer and seven μL of capture antibody. Using a reverse pipetting method, 100 μL of diluted capture antibody is added to all of the wells. In order to obtain an even coating, the sides of each plate should be gently tapped. The plates are then sealed with plate sealers, prior to stacking the plates and capping the stack with an empty 96-well plate. The plates are incubated overnight (14-24 hours) at 35-39° C. Each plate is then washed three times with wash buffer using the ultra wash plus micro titer plate washer set at 250 μL/wash with three washes and no soak time. After the last wash, the plates should be tapped onto a paper towel. Again, using the reverse pipetting technique, 250 μL of blocking solution should be added to all of the wells. The test plates should be sealed and incubated for approximately one hour (±five minutes) at 35-37° C. Preferably, the plates will not be stacked after this step. During the blocking step, all test samples should be pulled out and thawed at room temperature. Next, four separate dilution plates should be prepared by adding 200 μL of diluent solution to all of the remaining wells except for row A and row H, columns 1-3. Next, six test tubes should be labeled as follows, low titer, medium titer, high titer, inactivated/filtered (1:240), inactivated/filtered (1:480), and internal control. In the designated tubes, an appropriate dilution should be prepared for the following test samples. The thawed test samples should be vortexed prior to use. For four plates, the following dilutions will be made: A) the low titer will not be pre-diluted: 3.0 mLs of low titer; B) negative control at a 1:30 dilution (SF+ cells): 3.77 mLs of diluent+130 μL of the negative control; C) medium titer at a 1:30 dilution (8 μg/mL): 3.77 mLs of diluent+130 μL of the medium titer; D) high titer at a 1:90 dilution (16 μg/mL): 2.967 mLs of diluent+33 μL of high titer; E) inactivated/filtered at a 1:240 dilution: 2.39 mLs of diluent+10 μL of inactivated/filtered sample; F) inactivated/filtered at a 1:480 dilution: 1.0 mL of diluent+1.0 mL of inact/filtered (1:240) prepared sample from E above; G) internal control at 1:30 dilution: 3.77 mLs of diluent+130 μL of the internal control. Next, add 300 μL of the prepared samples to corresponding empty wells in the dilution plates for plates 1 through 4. The multichannel pipettor is then set to 100 μL, and the contents in Row A are mixed by pipetting up and down for at least 5 times and then 100 μL is transferred to Row B using the reverse pipetting technique. The tips should be changed and this same procedure is followed down the plate to Row G. Samples in these dilution plates are now ready for transfer to the test plates once the test plates have been washed 3 times with wash buffer using the ultrawash plus microtiter plate washer (settings at 250 μL/wash, 3 washes, no soak time). After the last wash, the plates should be tapped onto a paper towel. Next, the contents of the dilution plate are transferred to the test plate using a simple transfer procedure. More specifically, starting at row H, 100 μL/well is transferred from the dilution plate(s) to corresponding wells of the test plate(s) using reverse pipetting technique. After each transfer, the pipette tips should be changed. From Row G, 100 μL/well in the dilution plate(s) is transferred to corresponding wells of the test plate(s) using reverse pipetting technique. The same set of pipette tips can be used for the remaining transfer. To ensure a homogenous solution for the transfer, the solution should be pipetted up and down at least 3 times prior to transfer. Next, the test plate(s) are sealed and incubated for 1.0 hour±5 minutes at 37° C.±2.0° C. Again, it is preferable not to stack the plates. The plates are then washed 3 times with wash buffer using the ultrawash plus microtiter plate washer (settings at 250 μL/wash, 3 washes, and no soak time). After the last wash, the plates are tapped onto a paper towel. Using reverse pipetting technique, 100 μL of detection antibody diluted 1:300, or appropriate working dilution, in diluent solution is added to all of the wells of the test plate(s). For example, for four plates, one will need 42 mLs of diluent solution with 140 μL of capture antibody. The test plate(s) are then sealed and incubated for 1.0 hour±5 minutes at 37° C.±2.0° C. Again, the plates are washed 3 times with wash buffer using the ultrawash plus microtiter plate washer (settings at 250 μL/wash, 3 washes, and no soak time). After the last wash, the plates are tapped onto a paper towel. Next, the conjugate diluent is prepared by adding 1% normal rabbit serum to the diluent. For example, for four plates, 420 μL of normal rabbit serum is added to 42 mL of diluent. The conjugate antibody is diluted to 1:10,000, or any other appropriate working dilution, in a freshly prepared conjugate diluent solution to all wells of the test plate(s). Using a reverse pipetting technique, 100 μL of this diluted conjugate antibody is added to all the wells. The test plate(s) are then sealed and incubated for 45±5 minutes at 37° C.±2.0° C. Preferably, the plates are not stacked. The plates are then washed 3 times with wash buffer using the ultrawash plus microtiter plate washer (settings at 250 μL/wash, 3 washes, and no soak time). After the last wash, the plates are tapped onto a paper towel. Next, equal volumes of TMB Peroxidase Substrate (Reagent A) with Peroxidase Solution B (Reagent B) are mixed immediately prior to use. The amount mixed will vary depending upon the quantity of plates but each plate will require 10 mL/plate+2 mLs. Therefore, for 4 plates, it will be 21 mL of Reagent A+21 mL of Reagent B. Using a reverse pipetting technique, 100 μL of substrate is added to all wells of the test plate(s). The plates are then incubated at room temperature for 15 minutes±15 seconds. The reaction is stopped by the addition of 100 μL of 1N HCl solution to all wells using a reverse pipetting technique. The ELISA plate reader is then turned on and allowed to proceed through its diagnostics and testing phases in a conventional manner.
[0026] A further aspect of the invention relates to a method for constructing a recombinant viral vector containing PCV2 ORF2 DNA and expressing PCV2 ORF2 protein in high amounts, when infected into susceptible cells. It has been surprisingly found that the recombinant viral vector as provided herewith expresses high amounts, as defined above, of PCV2 ORF2 after infecting susceptible cells. Therefore, the present invention also relates to an improved method for producing and/or recovering of PCV2 ORF2 protein, preferably comprises the step: constructing a recombinant viral vector containing PCV2 ORF2 DNA and expressing PCV2 ORF2 protein. Preferably, the viral vector is a recombinant baculorvirus. Details of the method for constructing recombinant viral vectors containing PCV2 ORF2 DNA and expressing PCV2 ORF2 protein, as provided herewith, are described to the following: In preferred forms the recombinant viral vector containing PCV2 ORF 2 DNA and expressing PCV2 ORF2 protein used to infect the cells is generated by transfecting a transfer vector that has had an ORF2 gene cloned therein into a viral vector. Preferably, only the portion of the transfer vector is transfected into the viral vector, that contains the ORF2 DNA. The term “transfected into a viral vector” means, and is used as a synonym for “introducing” or “cloning” a heterologous DNA into a viral vector, such as for example into a baculovirus vector. The viral vector is preferably but not necessarily a baculovirus.
[0027] Thus, according to a further aspect of the present invention, the recombinant viral vector is generated by recombination between a transfer vector containing the heterologous PCV2 ORF2 DNA and a viral vector, preferably a baculorvirus, even more preferably a linearized replication-deficient baculovirus (such as Baculo Gold DNA). A “transfer vector” means a DNA molecule, that includes at least one origin of replication, the heterologous gene, in the present case PCV2 ORF2, and DNA sequences which allows the cloning of said heterologous gene into the viral vector. Preferably the sequences which allow cloning of the heterologous gene into the viral vector are flanking the heterologous gene. Even more preferably those flanking sequences are at least homologous in parts with sequences of the viral vector. The sequence homology then allows recombination of both molecules, the viral vector and the transfer vector to generate a recombinant viral vector containing the heterologous gene. One preferred transfer vector is the pVL1392 vector (BD Biosciences Pharmingen), which is designed for co-transfection with the BaculoGold DNA into the preferred Sf+ cell line. Preferably, said transfer vector comprises a PCV2 ORF2 DNA. The construct co-transfected is approximately 10,387 base pairs in length.
[0028] In more preferred forms, the methods of the present invention will begin with the isolation of PCV2 ORF2 DNA. Generally, this can be from a known or unknown strain as the ORF2 DNA appears to be highly conserved with at least about 95% sequence identity between different isolates. Any PCV2 ORF2 gene known in the art can be used for purposes of the present invention as each would be expressed into the supernate. The PCV ORF2 DNA is preferably amplified using PCR methods, even more preferred together with the introduction of a 5′ flanking Kozak's consensus sequence (CCGCCAUG) (SEQ ID NO 1) and/or a 3′ flanking EcoR1 site (GAATTC) (SEQ ID NO 2). Such introduction of a 5′ Kozak's consensus preferably removes the naturally occurring start codon AUG of PCV2 ORF2. The 3′ EcoR1 site is preferably introduced downstream of the stop codon of the PCV2 ORF2. More preferably it is introduced downstream of a poly A transcription termination sequence, that itself is located downstream of the PCV2 ORF2 stop codon. It has been found, that the use of a Kozak consensus sequence, in particular as described above, increases the expression level of the subsequent PCV2 ORF2 protein. The amplified PCV2 ORF2 DNA, with these additional sequences, is cloned into a vector. A preferred vector for this initial cloning step is the pGEM-T-Easy Vector (Promega, Madison, Wis.). The PCV2 ORF2 DNA including some pGEM vector sequences (SEQ ID NO: 7) is preferably excised from the vector at the Not1 restriction site. The resulting DNA is then cloned into the transfer vector.
[0029] Thus, in one aspect of the present invention, a method for constructing a recombinant viral vector containing PCV2 ORF2 DNA is provided. This method comprises the steps: i) cloning a recombinant PCV2 ORF2 into a transfer vector; and ii) transfecting the portion of the transfer vector containing the recombinant PCV2 ORF2 into a viral vector, to generate the recombinant viral vector. Preferably, the transfer vector is that described above or is constructed as described above or as exemplarily shown in FIG. 1 . Thus according to a further aspect, the transfer vector, used for the construction of the recombinant viral vector as described herein, contains the sequence of SEQ ID NO: 7.
[0030] According to a further aspect, this method further comprises prior to step i) the following step: amplifying the PCV2 ORF2 DNA in vitro, wherein the flanking sequences of the PCV2 ORF2 DNA are modified as described above. In vitro methods for amplifying the PCV2 ORF2 DNA and modifying the flanking sequences, cloning in vitro amplified PCV2 ORF2 DNA into a transfer vector and suitable transfer vectors are described above, exemplarily shown in FIG. 1 , or known to a person skilled in the art. Thus according to a further aspect, the present invention relates to a method for constructing a recombinant viral vector containing PCV2 ORF2 DNA and expressing PCV2 ORF2 protein comprises the steps of: i) amplifying PCV2 ORF2 DNA in vitro, wherein the flanking sequences of said PCV2 ORF2 DNA are modified, ii) cloning the amplified PCV2 ORF2 DNA into a transfer vector; and iii) transfecting the transfer vector or a portion thereof containing the recombinant PCV2 ORF2 DNA into a viral vector to generate the recombinant viral vector. Preferably, the modification of the flanking sequences of the PCV2 ORF2 DNA is performed as described above, e.g. by introducing a 5′ Kozak sequence and/or a EcoR 1 site, preferably as described above.
[0031] According to a further aspect, a method of producing and/or recovering recombinant protein expressed by open reading frame 2 of PCV2 is provided. The method generally comprises the steps of: i) cloning a recombinant PCV2 ORF2 into a transfer vector; ii) transfecting the portion of the transfer vector containing the recombinant PCV2 ORF2 into a virus; iii) infecting cells in media with the transfected virus; iv) causing the transfected virus to express the recombinant protein from PCV2 ORF2; v) separating cells from the supernate; and vi) recovering the expressed PCV2 ORF2 protein from the supernate.
[0032] Methods of how to clone a recombinant PCV2 ORF2 DNA into a transfer vector are described above. Preferably, the transfer vector contains the sequence of SEQ ID NO:3, SEQ ID NO:4, SEQ ID NO:7. However, the transfer vector can contain any PCV2 ORF2 DNA, unmodified or modified, as long as the PCV2 ORF2 DNA, when transfected into a recombinant viral vector, is expressed in cell culture. Preferably, the recombinant viral vector comprises the sequence of SEQ ID NO:8. Moreover, methods of how to infect cells, preferably how to infect insect cells with a defined number of recombinant baculovirus containing PCV2 ORF2 DNA and expressing PCV2 ORF2 protein are described above in detail. Moreover, steps of separating cells from the supernate as well as steps for recovering the expressed PCV2 ORF2 protein are also described above in detail. Any of these specific process steps, as described herein, are part of the method of producing and/or recovering recombinant protein expressed by open reading frame 2 of PCV2 as described above. Preferably, the cells are SF+ cells. Still more preferably, cell cultures have a cell count between about 0.3-2.0×10 6 cells/mL, more preferably from about 0.35-1.9×10 6 cells/mL, still more preferably from about 0.4-1.8×10 6 cells/mL, even more preferably from about 0.45-1.7×10 6 cells/mL, and most preferably from about 0.5-1.5×10 6 cells/mL. Preferably, the recombinant viral vector containing the PCV2 ORF2 DNA has a preferred multiplicity of infection (MOI) of between about 0.03-1.5, more preferably from about 0.05-1.3, still more preferably from about 0.09-1.1, still more preferably from about 0.1-1.0, and most preferably to about 0.5, when used for the infection of the susceptible cells. Preferably, recovering of the PCV2 ORF2 protein in the supernate of cells obtained between days 5 and 8 after infection and/or cell viability decreases to less then 10%. Preferably, for producing PCV2 ORF2 protein, cells are cultivated at 25 to 29° C. Preferably, the separation step is a centrifugation or a filtration step.
[0033] Optionally, this method can include the step of amplifying the PCV2 ORF2 DNA from a strain of PCV2 prior to cloning the PCV2 ORF2 DNA into the transfer vector. In preferred forms, a 5′ Kozak's sequence, a 3′ EcoR1 site, and combinations thereof can also be added to the amplified sequence, preferably prior to or during amplification. A preferred 5′ Kozak's sequence comprises SEQ ID NO: 1. A preferred 3′ EcoR1 site comprises SEQ ID NO: 2. Preferred PCV2 ORF2 DNA comprises the nucleotide sequence Genbank Accession No. AF086834 (SEQ ID NO: 3) and SEQ ID NO: 4. Preferred recombinant PCV2 ORF2 protein comprises the amino acid sequence of SEQ ID NO: 5, which is the protein encoded by SEQ ID NO: 3 (Genbank Accession No. AF086834) and SEQ ID No: 6, which is the protein encoded by SEQ ID NO: 4. A preferred media comprises serum-free insect cell media, still more preferably Excell 420 media. When the optional amplification step is performed, it is preferable to first clone the amplified open reading frame 2 into a first vector, excise the open reading frame 2 from the first vector, and use the excised open reading frame for cloning into the transfer vector. A preferred cell line for cotransfection is the SF+ cell line. A preferred virus for cotransfection is baculovirus. In preferred forms of this method, the transfected portion of the transfer vector comprises SEQ ID NO: 8. Finally, for this method, it is preferred to recover the PCV2 open reading frame 2 (ORF2) protein in the cell culture supernate at least 5 days after infecting the cells with the virus.
[0034] Thus, a further aspect of the invention relates to a method for producing and/or recovering the PCV2 open reading frame 2, comprises the steps: i) amplifying the PCV2 ORF2 DNA in vitro, preferably by adding a 5′ Kozak sequence and/or by adding a 3′ EcoR1 restriction site, ii) cloning the amplified PCV2 ORF2 into a transfer vector; iii) transfecting the portion of the transfer vector containing the recombinant PCV2 ORF2 into a virus; iv) infecting cells in media with the transfected virus; v) causing the transfected virus to express the recombinant protein from PCV2 ORF2; vi) separating cells from the supernate; and vii) recovering the expressed PCV2 ORF2 protein from the supernate.
[0035] A further aspect of the present invention relates to a method for preparing a composition comprising PCV2 ORF2 protein, and inactivated viral vector. This method comprises the steps: i) cloning the amplified PCV2 ORF2 into a transfer vector; ii) transfecting the portion of the transfer vector containing the recombinant PCV2 ORF2 into a virus; iii) infecting cells in media with the transfected viral vector; iv) causing the transfected viral vector to express the recombinant protein from PCV2 ORF2; v) separating cells from the supernate; iv) recovering the expressed PCV2 ORF2 protein from the supernate; and vii) inactivating the recombinant viral vector. Preferably, the recombinant viral vector is a baculovirus containing ORF2 DNA coding sequences and the cells are SF+ cells. Preferred separation steps are those described above, most preferred is the filtration step. Preferred inactivation steps are those described above. Preferably, inactivation is performed between about 35-39° C. and in the presence of 2 to 8 mM BEI, still more preferred in the presence of about 5 mM BEI. It has been surprisingly found, that higher concentrations of BEI negatively affect the PCV2 ORF2 protein, and lower concentrations are not effective to inactivate the viral vector within 24 to 72 hours of inactivation. Preferably, inactivation is performed for at least 24 hours, even more preferred for 24 to 72 hours.
[0036] According to a further aspect, the method for preparing a composition comprising PCV2 ORF2 protein, and inactivated viral vector, as described above, also includes an neutralization step after step vii). This step viii) comprises adding of an equivalent amount of an agent that neutralizes the inactivation agent within the solution. Preferably, if the inactivation agent is BEI, addition of sodium thiosulfate to an equivalent amount is preferred. Thus, according to a further aspect, step viii) comprises adding of a sodium thiosulfate solution to a final concentration of about 1 to about 20 mM, preferably of about 2 to about 10 mM, still more preferably of about 2 to about 8 mM, still more preferably of about 3 to about 7 mM, most preferably of about 5 mM, when the inactivation agent is BEI.
[0037] According to a further aspect, the method for preparing a composition comprising PCV2 ORF2 protein, and inactivated viral vector, as described above, comprises prior to step i) the following step: amplifying the PCV2 ORF2 DNA in vitro, wherein the flanking sequences of the PCV2 ORF2 DNA are modified as described above. In vitro methods for amplifying the PCV2 ORF2 DNA and modifying the flanking sequences, cloning in vitro amplified PCV2 ORF2 DNA into a transfer vector and suitable transfer vectors are described above, exemplarily shown in FIG. 1 , or known to a person skilled in the art. Thus according to a further aspect, this method comprises the steps: i) amplifying PCV2 ORF2 DNA in vitro, wherein the flanking sequences of said PCV2 ORF2 DNA are modified, ii) cloning the amplified PCV2 ORF2 DNA into a transfer vector; and iii) transfecting the transfer vector or a portion thereof containing the recombinant PCV2 ORF2 DNA into a viral vector to generate the recombinant viral vector, iv) infecting cells in media with the transfected virus; v) causing the transfected virus to express the recombinant protein from PCV2 ORF2; vi) separating cells from the supernate; vii) recovering the expressed PCV2 ORF2 protein from the supernate; viii) inactivating the recombinant viral vector, preferably, in the presence of about 1 to about 20 mM BEI, most preferred in the presence of about 5 mM BEI; and ix) adding of an equivalent amount of an agent that neutralizes the inactivation agent within the solution, preferably, adding of a sodium thiosulfate solution to a final concentration of about 1 to about 20 mM, preferably of about 5 mM, when the inactivation agent is BEI.
[0038] In another aspect of the present invention, a method for preparing a composition, preferably an antigenic composition, such as for example a vaccine, for invoking an immune response against PCV2 is provided. Generally, this method includes the steps of transfecting a construct into a virus, wherein the construct comprises i) recombinant DNA from ORF2 of PCV2, ii) infecting cells in growth media with the transfected virus, iii) causing the virus to express the recombinant protein from PCV2 ORF2, iv) recovering the expressed ORF2 protein from the supernate, v) and preparing the composition by combining the recovered protein with a suitable adjuvant and/or other pharmaceutically acceptable carrier.
[0039] “Adjuvants” as used herein, can include aluminum hydroxide and aluminum phosphate, saponins e.g., Quil A, QS-21 (Cambridge Biotech Inc., Cambridge Mass.), GPI-0100 (Galenica Pharmaceuticals, Inc., Birmingham, Ala.), water-in-oil emulsion, oil-in-water emulsion, water-in-oil-in-water emulsion. The emulsion can be based in particular on light liquid paraffin oil (European Pharmacopea type); isoprenoid oil such as squalane or squalene; oil resulting from theoligomerization of alkenes, in particular of isobutene or decene; esters of acids or of alcohols containing a linear alkyl group, more particularly plant oils, ethyl oleate, propylene glycol di-(caprylate/caprate), glyceryl tri-(caprylate/caprate) or propylene glycol dioleate; esters of branched fatty acids or alcohols, in particular isostearic acid esters. The oil is used in combination with emulsifiers to form the emulsion. The emulsifiers are preferably nonionic surfactants, in particular esters of sorbitan, of mannide (e.g. anhydromannitol oleate), of glycol, of polyglycerol, of propylene glycol and of oleic, isostearic, ricinoleic or hydroxystearic acid, which are optionally ethoxylated, and polyoxypropylene-polyoxyethylene copolymer blocks, in particular the Pluronic products, especially L121. See Hunter et al., The Theory and Practical Application of Adjuvants (Ed. Stewart-Tull, D. E. S.). John Wiley and Sons, NY, pp 51-94 (1995) and Todd et al., Vaccine 15:564-570 (1997).
[0040] For example, it is possible to use the SPT emulsion described on page 147 of “Vaccine Design, The Subunit and Adjuvant Approach” edited by M. Powell and M. Newman, Plenum Press, 1995, and the emulsion MF59 described on page 183 of this same book.
[0041] A further instance of an adjuvant is a compound chosen from the polymers of acrylic or methacrylic acid and the copolymers of maleic anhydride and alkenyl derivative. Advantageous adjuvant compounds are the polymers of acrylic or methacrylic acid which are cross-linked, especially with polyalkenyl ethers of sugars or polyalcohols. These compounds are known by the term carbomer (Phameuropa Vol. 8, No. 2, June 1996). Persons skilled in the art can also refer to U.S. Pat. No. 2,909,462 which describes such acrylic polymers cross-linked with a polyhydroxylated compound having at least 3 hydroxyl groups, preferably not more than 8, the hydrogen atoms of at least three hydroxyls being replaced by unsaturated aliphatic radicals having at least 2 carbon atoms. The preferred radicals are those containing from 2 to 4 carbon atoms, e.g. vinyls, allyls and other ethylenically unsaturated groups. The unsaturated radicals may themselves contain other substituents, such as methyl. The products sold under the name Carbopol; (BF Goodrich, Ohio, USA) are particularly appropriate. They are cross-linked with an allyl sucrose or with allyl pentaerythritol. Among then, there may be mentioned Carbopol 974P, 934P and 971P. Most preferred is the use of Cabopol 971P. Among the copolymers of maleic anhydride and alkenyl derivative, the copolymers EMA (Monsanto) which are copolymers of maleic anhydride and ethylene. The dissolution of these polymers in water leads to an acid solution that will be neutralized, preferably to physiological pH, in order to give the adjuvant solution into which the immunogenic, immunological or vaccine composition itself will be incorporated.
[0042] Further suitable adjuvants include, but are not limited to, the RIBI adjuvant system (Ribi Inc.), Block co-polymer (CytRx, Atlanta Ga.), SAF-M (Chiron, Emeryville Calif.), monophosphoryl lipid A, Avridine lipid-amine adjuvant, heat-labile enterotoxin from E. coli (recombinant or otherwise), cholera toxin, IMS 1314 or muramyl dipeptide among many others.
[0043] Preferably, the adjuvant is added in an amount of about 100 μg to about 10 mg per dose. Even more preferred the adjuvant is added in an amount of about 100 μg to about 10 mg per dose. Even more preferred the adjuvant is added in an amount of about 500 μg to about 5 mg per dose. Even more preferred the adjuvant is added in an amount of about 750 μg to about 2.5 mg per dose. Most preferred the adjuvant is added in an amount of about 1 mg per dose.
[0044] Thus, according to a further aspect, the method for preparing an antigenic composition, such as for example a vaccine, for invoking an immune response against PCV2 comprises i) preparing and recovering PCV2 ORF2 protein, and ii) admixing this with a suitable adjuvant. Preferably, the adjuvant is Carbopol 971P. Even more preferred, Carbopol 971P is added in an amount of about 500 μg to about 5 mg per dose, even more preferred in an amount of about 750 μg to about 2.5 mg per dose and most preferred in an amount of about 1 mg per dose. Preferably, the process step i) includes the process steps as described for the preparation and recovery of PCV2 ORF2. For example, in preferred forms of this method, the construct comprising PCV2 ORF2 DNA is obtained in a transfer vector. Suitable transfer vectors and methods of preparing them are described above. Optionally, the method may include the step of amplifying the ORF2 from a strain of PCV2 through PCR prior to cloning the ORF2 into the transfer vector. Preferred open reading frame sequences, Kozak's sequences, 3′ EcoR1 site sequences, recombinant protein sequences, transfected construct sequences, media, cells, and viruses are as described in the previous methods. Another optional step for this method includes cloning the amplified PCV2 ORF2 DNA into a first vector, excising the ORF2 DNA from this first vector, and using this excised PCV2 ORF2 DNA for cloning into the transfer vector. As with the other methods, it is preferred to wait for at least 5 days after infection of the cells by the transfected baculovirus prior to recovery of recombinant ORF2 protein from the supernate. Preferably, the recovery step of this method also includes the step of separating the media from the cells and cell debris. This can be done in a variety of ways but for ease and convenience, it is preferred to filter the cells, cell debris, and growth media through a filter having pores ranging in size from about 0.45 μM to about 1.0 μM. Finally, for this method, it is preferred to include a virus inactivation step prior to combining the recovered recombinant PCV2 ORF2 protein in a composition. This can be done in a variety of ways, but it is preferred in the practice of the present invention to use BEI.
[0045] Thus according to a further aspect, this method comprises the steps: i) amplifying PCV2 ORF2 DNA in vitro, wherein the flanking sequences of said PCV2 ORF2 DNA are modified, ii) cloning the amplified PCV2 ORF2 DNA into a transfer vector; and iii) transfecting the transfer vector or a portion thereof containing the recombinant PCV2 ORF2 DNA into a viral vector to generate the recombinant viral vector, iv) infecting cells in media with the transfected virus; v) causing the transfected virus to express the recombinant protein from PCV2 ORF2; vi) separating cells from the supernate; vii) recovering the expressed PCV2 ORF2 protein from the supernate; viii) inactivating the recombinant viral vector, preferably, in the presence of about 1 to about 20 mM BEI, most preferred in the presence of about 5 mM BEI; ix) adding of an equivalent amount of an agent that neutralizes the inactivation agent within the solution, preferably, adding of a sodium thiosulfate solution to a final concentration of about 1 to about 20 mM, preferably of about 5 mM, when the inactivation agent is BEI, and x) adding a suitable amount of an adjuvant, preferably adding Carbopol, more preferably Carbopol 971P, even more preferred in amounts as described above (e.g. of about 500 μg to about 5 mg per dose, even more preferred in an amount of about 750 μg to about 2.5 mg per dose and most preferred in an amount of about 1 mg per dose).
[0046] Additionally, the composition can include one or more pharmaceutical-acceptable carriers. As used herein, “a pharmaceutical-acceptable carrier” includes any and all solvents, dispersion media, coatings, stabilizing agents, diluents, preservatives, antibacterial and antifungal agents, isotonic agents, adsorption delaying agents, and the like. Most preferred, the composition provided herewith, contains PCV2 ORF2 protein recovered from the supernate of in vitro cultured cells, wherein said cells were infected with a recombinant viral vector containing PCV2 ORF2 DNA and expressing PCV2 ORF2 protein, and wherein said cell culture were treated with about 2 to about 8 mM BEI, preferably with about 5 mM BEI to inactivate the viral vector, and an equivalent concentration of a neutralization agent, preferably sodium thiosulfate solution to a final concentration of about 2 to about 8 mM, preferably of about 5 mM, Carbopol, more preferably Carbopol 971P, preferably in amounts of about 500 μg to about 5 mg per dose, even more preferred in an amount of about 750 μg to about 2.5 mg per dose and most preferred in an amount of about 1 mg per dose, and physiological saline, preferably in an amount of about 50 to about 90% (v/v), more preferably to about 60 to 80% (v/v), still more preferably of about 70% (v/v).
[0047] Thus, a further aspect relates to a method for preparing an antigenic composition, such as for example a vaccine, for invoking an immune response against PCV2 comprising the steps: i) amplifying PCV2 ORF2 DNA in vitro, wherein the flanking sequences of said PCV2 ORF2 DNA are modified, ii) cloning the amplified PCV2 ORF2 DNA into a transfer vector; and iii) transfecting the transfer vector or a portion thereof containing the recombinant PCV2 ORF2 DNA into a viral vector to generate the recombinant viral vector, iv) infecting cells in media with the transfected virus; v) causing the transfected virus to express the recombinant protein from PCV2 ORF2; vi) separating cells from the supernate; vii) recovering the expressed PCV2 ORF2 protein from the supernate; viii) inactivating the recombinant viral vector, preferably, in the presence of about 2 to about 20 mM BEI, most preferred in the presence of about 5 mM BEI; ix) adding of an equivalent amount of an agent that neutralize the inactivation agent within the solution, preferably, adding of a sodium thiosulfate solution to a final concentration of about 0.5 to about 20 mM, preferably of about 5 mM, when the inactivation agent is BEI, x) adding a suitable amount of an adjuvants, preferably adding Carbopol, more preferably Carbopol 971P, still more preferred in amounts as described above (e.g. of about 500 μg to about 5 mg per dose, even more preferred in an amount of about 750 μg to about 2.5 mg per dose and most preferred in an amount of about 1 mg per dose); and xi) adding physiological saline, preferably in an amount of about 50 to about 90% (v/v), more preferably to about 60 to 80% (v/v), still more preferably of about 70% (v/v). Optionally, this method can also include the addition of a protectant. A protectant as used herein, refers to an anti-microbiological active agent, such as for example Gentamycin, Merthiolate, and the like. In particular adding of a protectant is most preferred for the preparation of a multi-dose composition. Those anti-microbiological active agents are added in concentrations effective to prevent the composition of interest for any microbiological contamination or for inhibition of any microbiological growth within the composition of interest.
[0048] Moreover, this method can also comprise addition of any stabilizing agent, such as for example saccharides, trehalose, mannitol, saccharose and the like, to increase and/or maintain product shelf-life. However, it has been surprisingly found, that the resulting formulation is immunologically effective over a period of at least 24 months, without adding any further stabilizing agent.
[0049] A further aspect of the present invention relates to the products result from the methods as described above. In particular, the present invention relates to a composition of matter comprises recombinantly expressed PCV2 ORF2 protein. Moreover, the present invention also relates to a composition of matter that comprises recombinantly expressed PCV2 ORF2 protein, recovered from the supernate of an insect cell culture. Moreover, the present invention also relates to a composition of matter comprises recombinantly expressed PCV2 ORF2 protein, recovered from the supernate of an insect cell culture. Preferably, this composition of matter also comprises an agent suitable for the inactivation of viral vectors. Preferably, said inactivation agent is BEI. Moreover, the present invention also relates to a composition of matter that comprises recombinantly expressed PCV2 ORF2 protein, recovered from the supernate of an insect cell culture, and comprises an agent, suitable for the inactivation of viral vectors, preferably BEI and a neutralization agent for neutralization of the inactivation agent. Preferably, that neutralization agent is sodium thiosulfate, when BEI is used as an inactivation agent.
[0050] In yet another aspect of the present invention, an immunogenic composition that induces an immune response and, more preferably, confers protective immunity against the clinical signs of PCV2 infection, is provided. The composition generally comprises the polypeptide, or a fragment thereof, expressed by Open Reading Frame 2 (ORF2) of PCV2, as the antigenic component of the composition.
[0051] PCV2 ORF2 DNA and protein, as used herein for the preparation of the compositions and also as used within the processes provided herein is a highly conserved domain within PCV2 isolates and thereby, any PCV2 ORF2 would be effective as the source of the PCV ORF2 DNA and/or polypeptide as used herein. A preferred PCV2 ORF2 protein is that of SEQ ID NO. 11. A preferred PCV ORF2 polypeptide is provided herein as SEQ ID NO. 5, but it is understood by those of skill in the art that this sequence could vary by as much as 6-10% in sequence homology and still retain the antigenic characteristics that render it useful in immunogenic compositions. The antigenic characteristics of an immunological composition can be, for example, estimated by the challenge experiment as provided by Example 4. Moreover, the antigenic characteristic of an modified antigen is still retained, when the modified antigen confers at least 70%, preferably 80%, more preferably 90% of the protective immunity as compared to the PCV2 ORF 2 protein, encoded by the polynucleotide sequence of SEQ ID NO:3 or SEQ ID NO:4. An “immunogenic composition” as used herein, means a PCV2 ORF2 protein which elicits an “immunological response” in the host of a cellular and/or antibody-mediated immune response to PCV2 ORF2 protein. Preferably, this immunogenic composition is capable to confer protective immunity against PCV2 infection and the clinical signs associated therewith. In some forms, immunogenic portions of PCV2 ORF2 protein are used as the antigenic component in the composition. The term “immunogenic portion” as used herein refers to truncated and/or substituted forms, or fragments of PCV2 ORF2 protein and/or polynucleotide, respectively. Preferably, such truncated and/or substituted forms, or fragments will comprise at least 6 contiguous amino acids from the full-length ORF2 polypeptide. More preferably, the truncated or substituted forms, or fragments will have at least 10, more preferably at least 15, and still more preferably at least 19 contiguous amino acids from the full-length ORF2 polypeptide. Two preferred sequences in this respect are provided herein as SEQ ID NOs. 9 and 10. It is further understood that such sequences may be a part of larger fragments or truncated forms. A further preferred PCV2 ORF2 polypeptide provided herein is encoded by the nucleotide sequences of SEQ ID NO: 3 or SEQ ID NO: 4. But it is understood by those of skill in the art that this sequence could vary by as much as 6-20% in sequence homology and still retain the antigenic characteristics that render it useful in immunogenic compositions. In some forms, a truncated or substituted form, or fragment of ORF2 is used as the antigenic component in the composition. Preferably, such truncated or substituted forms, or fragments will comprise at least 18 contiguous nucleotides from the full-length ORF2 nucleotide sequence, e.g. of SEQ ID NO: 3 or SEQ ID NO: 4. More preferably, the truncated or substituted forms, or fragments will have at least 30, more preferably at least 45, and still more preferably at least 57 contiguous nucleotides the full-length ORF2 nucleotide sequence, e.g. of SEQ ID NO: 3 or SEQ ID NO: 4.
[0052] “Sequence Identity” as it is known in the art refers to a relationship between two or more polypeptide sequences or two or more polynucleotide sequences, namely a reference sequence and a given sequence to be compared with the reference sequence. Sequence identity is determined by comparing the given sequence to the reference sequence after the sequences have been optimally aligned to produce the highest degree of sequence similarity, as determined by the match between strings of such sequences. Upon such alignment, sequence identity is ascertained on a position-by-position basis, e.g., the sequences are “identical” at a particular position if at that position, the nucleotides or amino acid residues are identical. The total number of such position identities is then divided by the total number of nucleotides or residues in the reference sequence to give % sequence identity. Sequence identity can be readily calculated by known methods, including but not limited to, those described in Computational Molecular Biology, Lesk, A. N., ed., Oxford University Press, New York (1988), Biocomputing: Informatics and Genome Projects, Smith, D. W., ed., Academic Press, New York (1993); Computer Analysis of Sequence Data, Part I, Griffin, A. M., and Griffin, H. G., eds., Humana Press, New Jersey (1994); Sequence Analysis in Molecular Biology, von Heinge, G., Academic Press (1987); Sequence Analysis Primer, Gribskov, M. and Devereux, J., eds., M. Stockton Press, New York (1991); and Carillo, H., and Lipman, D., SIAM J. Applied Math., 48: 1073 (1988), the teachings of which are incorporated herein by reference. Preferred methods to determine the sequence identity are designed to give the largest match between the sequences tested. Methods to determine sequence identity are codified in publicly available computer programs which determine sequence identity between given sequences. Examples of such programs include, but are not limited to, the GCG program package (Devereux, J., et al., Nucleic Acids Research, 12(1):387 (1984)), BLASTP, BLASTN and FASTA (Altschul, S. F. et al., J. Molec. Biol., 215:403-410 (1990). The BLASTX program is publicly available from NCBI and other sources (BLAST Manual, Altschul, S. et al., NCVI NLM NIH Bethesda, Md. 20894, Altschul, S. F. et al., J. Molec. Biol., 215:403-410 (1990), the teachings of which are incorporated herein by reference). These programs optimally align sequences using default gap weights in order to produce the highest level of sequence identity between the given and reference sequences. As an illustration, by a polynucleotide having a nucleotide sequence having at least, for example, 85%, preferably 90%, even more preferably 95% “sequence identity” to a reference nucleotide sequence, it is intended that the nucleotide sequence of the given polynucleotide is identical to the reference sequence except that the given polynucleotide sequence may include up to 15, preferably up to 10, even more preferably up to 5 point mutations per each 100 nucleotides of the reference nucleotide sequence. In other words, in a polynucleotide having a nucleotide sequence having at least 85%, preferably 90%, even more preferably 95% identity relative to the reference nucleotide sequence, up to 15%, preferably 10%, even more preferably 5% of the nucleotides in the reference sequence may be deleted or substituted with another nucleotide, or a number of nucleotides up to 15%, preferably 10%, even more preferably 5% of the total nucleotides in the reference sequence may be inserted into the reference sequence. These mutations of the reference sequence may occur at the 5′ or 3′ terminal positions of the reference nucleotide sequence or anywhere between those terminal positions, interspersed either individually among nucleotides in the reference sequence or in one or more contiguous groups within the reference sequence. Analogously, by a polypeptide having a given amino acid sequence having at least, for example, 85%, preferably 90%, even more preferably 95% sequence identity to a reference amino acid sequence, it is intended that the given amino acid sequence of the polypeptide is identical to the reference sequence except that the given polypeptide sequence may include up to 15, preferably up to 10, even more preferably up to 5 amino acid alterations per each 100 amino acids of the reference amino acid sequence. In other words, to obtain a given polypeptide sequence having at least 85%, preferably 90%, even more preferably 95% sequence identity with a reference amino acid sequence, up to 15%, preferably up to 10%, even more preferably up to 5% of the amino acid residues in the reference sequence may be deleted or substituted with another amino acid, or a number of amino acids up to 15%, preferably up to 10%, even more preferably up to 5% of the total number of amino acid residues in the reference sequence may be inserted into the reference sequence. These alterations of the reference sequence may occur at the amino or the carboxy terminal positions of the reference amino acid sequence or anywhere between those terminal positions, interspersed either individually among residues in the reference sequence or in the one or more contiguous groups within the reference sequence. Preferably, residue positions which are not identical differ by conservative amino acid substitutions. However, conservative substitutions are not included as a match when determining sequence identity.
[0053] “Sequence homology”, as used herein, refers to a method of determining the relatedness of two sequences. To determine sequence homology, two or more sequences are optimally aligned, and gaps are introduced if necessary. However, in contrast to “sequence identity”, conservative amino acid substitutions are counted as a match when determining sequence homology. In other words, to obtain a polypeptide or polynucleotide having 95% sequence homology with a reference sequence, 85%, preferably 90%, even more preferably 95% of the amino acid residues or nucleotides in the reference sequence must match or comprise a conservative substitution with another amino acid or nucleotide, or a number of amino acids or nucleotides up to 15%, preferably up to 10%, even more preferably up to 5% of the total amino acid residues or nucleotides, not including conservative substitutions, in the reference sequence may be inserted into the reference sequence. Preferably the homolog sequence comprises at least a stretch of 50, even more preferred of 100, even more preferred of 250, even more preferred of 500 nucleotides.
[0054] A “conservative substitution” refers to the substitution of an amino acid residue or nucleotide with another amino acid residue or nucleotide having similar characteristics or properties including size, hydrophobicity, etc., such that the overall functionality does not change significantly.
[0055] Isolated” means altered “by the hand of man” from its natural state, i.e., if it occurs in nature, it has been changed or removed from its original environment, or both. For example, a polynucleotide or polypeptide naturally present in a living organism is not “isolated,” but the same polynucleotide or polypeptide separated from the coexisting materials of its natural state is “isolated”, as the term is employed herein.
[0056] Thus, a further aspect of the present invention relates to an immunogenic composition effective for lessening the severity of clinical symptoms associated with PCV2 infection comprising PCV2 ORF2 protein. Preferably, the PCV2 ORF2 protein is anyone of those, described above. Preferably, said PCV2 ORF2 protein is
i) a polypeptide comprising the sequence of SEQ ID NO: 5, SEQ ID NO: 6, SEQ ID NO: 9, SEQ ID NO: 10 or SEQ ID NO: 11; ii) any polypeptide that is at least 80% homologous to the polypeptide of i), iii) any immunogenic portion of the polypeptides of i) and/or ii) iv) the immunogenic portion of iii), comprising at least 10 contiguous amino acids included in the sequences of SEQ ID NO: 5, SEQ ID NO: 6, SEQ ID NO: 9, SEQ ID NO: 10 or SEQ ID NO: 11, v) a polypeptide that is encoded by a DNA comprising the sequence of SEQ ID NO: 3 or SEQ ID NO: 4. iv) any polypeptide that is encoded by a polynucleotide that is at least 80% homolog to the polynucleotide of v), vii) any immunogenic portion of the polypeptides encoded by the polynucleotide of v) and/or vi) viii) the immunogenic portion of vii), wherein polynucleotide coding for said immunogenic portion comprises at least 30 contiguous nucleotides included in the sequences of SEQ ID NO: 3, or SEQ ID NO: 4.
[0065] Preferably any of those immunogenic portions having the immunogenic characteristics of PCV2 ORF2 protein that is encoded by the sequence of SEQ ID NO: 3 or SEQ ID NO: 4.
[0066] According to a further aspect, PCV2 ORF2 protein is provided in the immunological composition at an antigen inclusion level effective for inducing the desired immune response, namely reducing the incidence of or lessening the severity of clinical signs resulting from PCV2 infection. Preferably, the PCV2 ORF2 protein inclusion level is at least 0.2 μg antigen/ml of the final immunogenic composition (μg/ml), more preferably from about 0.2 to about 400 μg/ml, still more preferably from about 0.3 to about 200 μg/ml, even more preferably from about 0.35 to about 100 μg/ml, still more preferably from about 0.4 to about 50 μg/ml, still more preferably from about 0.45 to about 30 μg/ml, still more preferably from about 0.6 to about 15 μg/ml, even more preferably from about 0.75 to about 8 μg/ml, even more preferably from about 1.0 to about 6 μg/ml, still more preferably from about 1.3 to about 3.0 μg/ml, even more preferably from about 1.4 to about 2.5 μg/ml, even more preferably from about 1.5 to about 2.0 μg/ml, and most preferably about 1.6 μg/ml.
[0067] According to a further aspect, the ORF2 antigen inclusion level is at least 0.2 μg PCV2 ORF2 protein as described above per dose of the final antigenic composition (μg/dose), more preferably from about 0.2 to about 400 μg/dose, still more preferably from about 0.3 to about 200 μg/dose, even more preferably from about 0.35 to about 100 μg/dose, still more preferably from about 0.4 to about 50 μg/dose, still more preferably from about 0.45 to about 30 μg/dose, still more preferably from about 0.6 to about 15 μg/dose, even more preferably from about 0.75 to about 8 μg/dose, even more preferably from about 1.0 to about 6 μg/dose, still more preferably from about 1.3 to about 3.0 μg/dose, even more preferably from about 1.4 to about 2.5 μg/dose, even more preferably from about 1.5 to about 2.0 μg/dose, and most preferably about 1.6 μg/dose.
[0068] The PCV2 ORF2 polypeptide used in an immunogenic composition in accordance with the present invention can be derived in any fashion including isolation and purification of PCV2 ORF2, standard protein synthesis, and recombinant methodology. Preferred methods for obtaining PCV2 ORF2 polypeptide are described herein above and are also provided in U.S. patent application Ser. No. 11/034,797, the teachings and content of which are hereby incorporated by reference. Briefly, susceptible cells are infected with a recombinant viral vector containing PCV2 ORF2 DNA coding sequences, PCV2 ORF2 polypeptide is expressed by the recombinant virus, and the expressed PCV2 ORF2 polypeptide is recovered from the supernate by filtration and inactivated by any conventional method, preferably using binary ethylenimine, which is then neutralized to stop the inactivation process.
[0069] Thus, according to a further aspect the immunogenic composition comprises i) any of the PCV2 ORF2 protein described above, preferably in concentrations described above, and ii) at least a portion of the viral vector expressing said PCV2 ORF2 protein, preferably of a recombinant baculovirus. Moreover, according to a further aspect, the immunogenic composition comprises i) any of the PCV2 ORF2 protein described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF2 protein, preferably of a recombinant baculovirus, and iii) a portion of the cell culture supernate.
[0070] According to one specific embodiment of the production and recovery process for PCV2 ORF2 protein, the cell culture supernate is filtered through a membrane having a pore size, preferably between about 0.45 to 1 μm. Thus, a further aspect relates to an immunogenic composition that comprises i) any of the PCV2 ORF2 protein described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF2 protein, preferably of a recombinant baculovirus, and iii) a portion of the cell culture; wherein about 90% of the components have a size smaller than 1 μm.
[0071] According to a further aspect, the present invention relates to an immunogenic composition that comprises i) any of the PCV2 ORF2 protein described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF2 protein, iii) a portion of the cell culture, iv) and inactivating agent to inactivate the recombinant viral vector preferably BEI, wherein about 90% of the components i) to iii) have a size smaller than 1 μm. Preferably, BEI is present in concentrations effective to inactivate the baculovirus. Effective concentrations are described above.
[0072] According to a further aspect, the present invention relates to an immunogenic composition that comprises i) any of the PCV2 ORF2 protein described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF2 protein, iii) a portion of the cell culture, iv) an inactivating agent to inactivate the recombinant viral vector preferably BEI, and v) an neutralization agent to stop the inactivation mediated by the inactivating agent, wherein about 90% of the components i) to iii) have a size smaller than 1 μm. Preferably, if the inactivating agent is BEI, said composition comprises sodium thiosulfate in equivalent amounts to BEI.
[0073] The polypeptide is incorporated into a composition that can be administered to an animal susceptible to PCV2 infection. In preferred forms, the composition may also include additional components known to those of skill in the art (see also Remington's Pharmaceutical Sciences. (1990). 18th ed. Mack Publ., Easton). Additionally, the composition may include one or more veterinary-acceptable carriers. As used herein, “a veterinary-acceptable carrier” includes any and all solvents, dispersion media, coatings, adjuvants, stabilizing agents, diluents, preservatives, antibacterial and antifungal agents, isotonic agents, adsorption delaying agents, and the like.
[0074] In a preferred embodiment, the immunogenic composition comprises PCV2 ORF2 protein as provided herewith, preferably in concentrations described above as an antigenic component, which is mixed with an adjuvant, preferably Carbopol, and physiological saline.
[0075] Those of skill in the art will understand that the composition herein may incorporate known injectable, physiologically acceptable sterile solutions. For preparing a ready-to-use solution for parenteral injection or infusion, aqueous isotonic solutions, such as e.g. saline or corresponding plasma protein solutions are readily available. In addition, the immunogenic and vaccine compositions of the present invention can include diluents, isotonic agents, stabilizers, or adjuvants. Diluents can include water, saline, dextrose, ethanol, glycerol, and the like. Isotonic agents can include sodium chloride, dextrose, mannitol, sorbitol, and lactose, among others. Stabilizers include albumin and alkali salts of ethylendiamintetracetic acid, among others. Suitable adjuvants, are those described above. Most preferred is the use of Carbopol, in particular the use of Carbopol 971P, preferably in amounts as described above (e.g. of about 500 μg to about 5 mg per dose, even more preferred in an amount of about 750 μg to about 2.5 mg per dose and most preferred in an amount of about 1 mg per dose).
[0076] Thus, the present invention also relates to an immunogenic composition that comprises i) any of the PCV2 ORF2 proteins described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF2 protein, iii) a portion of the cell culture, iv) an inactivating agent to inactivate the recombinant viral vector preferably BEI, and v) an neutralization agent to stop the inactivation mediated by the inactivating agent, preferably sodium thiosulfate in equivalent amounts to BEI; and vi) a suitable adjuvant, preferably Carbopol 971 in amounts described above; wherein about 90% of the components i) to iii) have a size smaller than 1 μm. According to a further aspect, this immunogenic composition further comprises a pharmaceutical acceptable salt, preferably a phosphate salt in physiologically acceptable concentrations. Preferably, the pH of said immunogenic composition is adjusted to a physiological pH, meaning between about 6.5 and 7.5.
[0077] Thus, the present invention also relates to an immunogenic composition comprises per one ml i) at least 1.6 μg of PCV2 ORF2 protein described above, ii) at least a portion of baculovirus expressing said PCV2 ORF2 protein iii) a portion of the cell culture, iv) about 2 to 8 mM BEI, v) sodium thiosulfate in equivalent amounts to BEI; and vi) about 1 mg Carbopol 971, and vii) phosphate salt in a physiologically acceptable concentration; wherein about 90% of the components i) to iii) have a size smaller than 1 μm and the pH of said immunogenic composition is adjusted to about 6.5 to 7.5.
[0078] The immunogenic compositions can further include one or more other immunomodulatory agents such as, e. g., interleukins, interferons, or other cytokines. The immunogenic compositions can also include Gentamicin and Merthiolate. While the amounts and concentrations of adjuvants and additives useful in the context of the present invention can readily be determined by the skilled artisan, the present invention contemplates compositions comprising from about 50 μg to about 2000 μg of adjuvant and preferably about 250 μg/ml dose of the vaccine composition. In another preferred embodiment, the present invention contemplates vaccine compositions comprising from about 1 ug/ml to about 60 μg/ml of antibiotics, and more preferably less than about 30 μg/ml of antibiotics.
[0079] Thus, the present invention also relates to an immunogenic composition that comprises i) any of the PCV2 ORF2 proteins described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF2 protein, iii) a portion of the cell culture, iv) an inactivating agent to inactivate the recombinant viral vector preferably BEI, and v) an neutralization agent to stop the inactivation mediated by the inactivating agent, preferably sodium thiosulfate in equivalent amounts to BEI; vi) a suitable adjuvant, preferably Carbopol 971 in amounts described above; vii) a pharmaceutical acceptable concentration of a saline buffer, preferably of a phosphate salt, and viii) an anti-microbiological active agent; wherein about 90% of the components i) to iii) have a size smaller than 1 μm.
[0080] It has been surprisingly found, that the immunogenic composition provided herewith comprises was highly stable over a period of 24 months. It has also been found the immunogenic compositions provided herewith, comprising recombinant, baculovirus expressed PCV2 ORF2 protein as provided herewith are very effective in reducing the clinical symptoms associated with PCV2 infections. It has been surprisingly found, that the immunogenic compositions comprising the recombinant baculovirus expressed PCV2 ORF2 protein as provided herewith, are more effective than an immunogenic composition comprising the whole PCV2 virus in an inactivated form, or isolated viral PCV2 ORF2 antigen. In particular, it has been surprisingly found, that the recombinant baculovirus expressed PCV2 ORF2 protein is effective is in very low concentrations, which means in concentrations up to 0.25 μg/dose. This unexpected high immunogenic potential of the PCV2 ORF2 protein could be further increased by the addition of Carbopol.
[0081] A further aspect relates to a container comprises at least one dose of the immunogenic composition of PCV2 ORF2 protein as provided herewith, wherein one dose comprises at least 2 μg PCV2 ORF2 protein, preferably 2 to 16 μg PCV2 ORF2 protein. Said container can comprises 1 to 250 doses of the immunogenic composition, preferably it contains 1, 10, 25, 50, 100, 150, 200, or 250 doses of the immunogenic composition of PCV2 ORF2 protein. Preferably, each of the containers comprising more than one dose of the immunogenic composition of PCV2 ORF2 protein further comprises an anti-microbiological active agent. Those agents are for example antibiotics including Gentamicin and Merthiolate and the like. Thus, one aspect of the present invention relates to a container that comprises 1 to 250 doses of the immunogenic composition of PCV2 ORF2 protein, wherein one dose comprises at least 2 μg PCV2 ORF2 protein, and Gentamicin and/or Merthiolate, preferably from about 1 μg/ml to about 60 μg/ml of antibiotics, and more preferably less than about 30 μg/ml.
[0082] A further aspect relates to a kit, comprising any of the containers, described above, and an instruction manual, including the information for the intramuscular application of at least one dose of the immunogenic composition of PCV2 ORF2 protein into piglets to lessening the severity of clinical symptoms associated with PCV2 infection. Moreover, according to a further aspect, said instruction manual comprises the information of a second or further administration(s) of at least one dose of the immunogenic composition of PCV2 ORF2, wherein the second administration or any further administration is at least 14 days beyond the initial or any former administration. Preferably, said instruction manual also includes the information, to administer an immune stimulant. Preferably, said immune stimulant shall be given at least twice. Preferably, at least 3, more preferably at least 5, even more preferably at least 7 days are between the first and the second or any further administration of the immune stimulant. Preferably, the immune stimulant is given at least 10 days, preferably 15, even more preferably 20, even more preferably at least 22 days beyond the initial administration of the immunogenic composition of PCV2 ORF2 protein. A preferred immune stimulant is for example is keyhole limpet hemocyanin (KLH), still preferably emulsified with incomplete Freund's adjuvant (KLH/ICFA). However, it is herewith understood, that any other immune stimulant known to a person skilled in the art can also be used. “Immune stimulant” as used herein, means any agent or composition that can trigger the immune response, preferably without initiating or increasing a specific immune response, for example the immune response against a specific pathogen. It is further instructed to administer the immune stimulant in a suitable dose. Moreover, the kit may also comprises a container, including at least one dose of the immune stimulant, preferably one dose of KLH, or KLH/ICFA.
[0083] Moreover, it has also been surprisingly found that the immunogenic potential of the immunogenic compositions comprising recombinant baculovirus expressed PCV2 ORF2 protein, preferably in combination with Carbopol, can be further enhanced by the administration of the IngelVac PRRS MLV vaccine (see Example 5). PCV2 clinical signs and disease manifestations are greatly magnified when PRRS infection is present. However, the immunogenic compositions and vaccination strategies as provided herewith lessened this effect greatly, and more than expected. In other words, an unexpected synergistic effect was observed when animals, preferably pigs are treated with any of the PCV2 ORF2 immunogenic composition, as provided herewith, and the Ingelvac PRRS MLV vaccine (Boehringer Ingelheim).
[0084] Thus, a further aspect of the present invention relates to the kit as described above, comprising the immunogenic composition of PCV2 ORF2 as provided herewith and the instruction manual, wherein the instruction manual further include the information to administer the PCV2 ORF2 immunogenic composition together with immunogenic composition that comprises PRRS antigen, preferably adjuvanted PRRS antigen. Preferably, the PRRS antigen is adjuvanted with Carbopol. Preferably, the PRRS antigen is IngelVac® PRRS MLV (Boehringer Ingelheim).
[0085] A further aspect of the present invention also relates to a kit comprising i) a container containing at least one dose of an immunogenic composition of PCV2 ORF2 as provided herewith, and ii) a container containing an immunogenic composition comprising PRRS antigen, preferably adjuvanted PRRS antigen. Preferably, the PRRS antigen is adjuvanted with Carbopol. Preferably the PRRS antigen is IngelVac® PRRS MLV (Boehringer Ingelheim). More preferably, the kit further comprises an instruction manual, including the information to administer both pharmaceutical compositions. Preferably, it contains the information that the PCV2 ORF2 containing composition is administered temporally prior to the PRRS containing composition.
[0086] A further aspect, relates to the use of any of the compositions provided herewith as a medicament, preferably as a veterinary medicament, even more preferred as a vaccine. Moreover, the present invention also relates to the use of any of the compositions described herein, for the preparation of a medicament for lessening the severity of clinical symptoms associated with PCV2 infection. Preferably, the medicament is for the prevention of a PCV2 infection, even more preferably in piglets.
[0087] A further aspect relates to a method for (i) the prevention of an infection, or re-infection with PCV2 or (ii) the reduction or elimination of clinical symptoms caused by PCV2 in a subject, comprising administering any of the immunogenic compositions provided herewith to a subject in need thereof. Preferably, the subject is a pig. Preferably, the immunogenic composition is administered intramuscular. Preferably, one dose or two doses of the immunogenic composition is/are administered, wherein one dose preferably comprises at least about 2 μg PCV2 ORF2 protein, even more preferably about 2 to about 16 μg, and at least about 0.1 to about 5 mg Carbopol, preferably about 1 mg Carbopol. A further aspect relates to the method of treatment as described above, wherein a second application of the immunogenic composition is administered. Preferably, the second administration is done with the same immunogenic composition, preferably having the same amount of PCV2 ORF2 protein. Preferably the second administration is also given intramuscular. Preferably, the second administration is done at least 14 days beyond the initial administration, even more preferably at least 4 weeks beyond the initial administration.
[0088] According to a further aspect, the method of treatment also comprises the administration of an immune stimulant. Preferably, said immune stimulant is administered at least twice. Preferably, at least 3, more preferably at least 5 days, even more preferably at least 7 days are between the first and the second administration of the immune stimulant. Preferably, the immune stimulant is administered at least 10 days, preferably 15, even more preferably 20, even more preferably at least 22 days beyond the initial administration of the PCV2 ORF2 immunogenic composition. A preferred immune stimulant is for example is keyhole limpet hemocyanin (KLH), still preferably emulsified with incomplete Freund's adjuvant (KLH/ICFA). However, it is herewith understood, that any other immune stimulant known to a person skilled in the art can also be used. It is within the general knowledge of a person skilled in the art to administer the immune stimulant in a suitable dose.
[0089] According to a further aspect, the method of treatments described above also comprises the administration of PRRS antigen. Preferably, the PRRS antigen is adjuvanted with Carbopol. Preferably the PRRS antigen is IngelVac® PRRS MLV (Boehringer Ingelheim). Preferably, said PRRS antigen is administered temporally beyond the administration of the immunogenic composition of PCV2 ORF2 protein.
BRIEF DESCRIPTION OF THE DRAWINGS
[0090] FIG. 1 is a schematic flow diagram of a preferred construction of PCV2 ORF2 recombinant baculovirus; and
[0091] FIGS. 2 a and 2 b are a schematic flow diagram of how to produce a composition in accordance with the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0092] The following examples set forth preferred materials and procedures in accordance with the present invention. It is to be understood, however, that these examples are provided by way of illustration only, and nothing therein should be deemed a limitation upon the overall scope of the invention.
Example 1
[0093] This example compares the relative yields of ORF2 using methods of the present invention with methods that are known in the prior art. Four 1000 mL spinner flasks were each seeded with approximately 1.0×10 6 Sf+ cells/ml in 300 mL of insect serum free media, Excell 420 (JRH Biosciences, Inc., Lenexa, Kans.). The master cell culture is identified as SF+( Spodoptera frugiperda ) Master Cell Stock, passage 19, Lot#N112-095W. The cells used to generate the SF+ Master Cell Stock were obtained from Protein Sciences Corporation, Inc., Meriden, Conn. The SF+ cell line for this example was confined between passages 19 and 59. Other passages will work for purposes of the present invention, but in order to scale the process up for large scale production, at least 19 passages will probably be necessary and passages beyond 59 may have an effect on expression, although this was not investigated. In more detail, the initial SF+ cell cultures from liquid nitrogen storage were grown in Excell 420 media in suspension in sterile spinner flasks with constant agitation. The cultures were grown in 100 mL to 250 mL spinner flasks with 25 to 150 mL of Excell 420 serum-free media. When the cells had multiplied to a cell density of 1.0-8.0×10 6 cells/mL, they were split to new vessels with a planting density of 0.5-1.5×10 6 cells/mL. Subsequent expansion cultures were grown in spinner flasks up to 36 liters in size or in stainless steel bioreactors of up to 300 liters for a period of 2-7 days at 25-29° C.
[0094] After seeding, the flasks were incubated at 27° C. for four hours. Subsequently, each flask was seeded with a recombinant baculovirus containing the PCV2 ORF2 gene (SEQ ID NO: 4). The recombinant baculovirus containing the PCV2 ORF2 gene was generated as follows: the PCV2 ORF2 gene from a North American strain of PCV2 was PCR amplified to contain a 5′ Kozak's sequence (SEQ ID NO: 1) and a 3′ EcoR1 site (SEQ ID NO: 2), cloned into the pGEM-T-Easy vector (Promega, Madison, Wis.). Then, it was subsequently excised and subcloned into the transfer vector pVL1392 (BD Biosciences Pharmingen, San Diego, Calif.). The subcloned portion is represented herein as SEQ ID NO: 7. The pVL1392 plasmid containing the PCV2 ORF2 gene was designated N47-064Y and then co-transfected with BaculoGold® (BD Biosciences Pharmingen) baculovirus DNA into Sf+ insect cells (Protein Sciences, Meriden, Conn.) to generate the recombinant baculovirus containing the PCV2 ORF2 gene. The new construct is provided herein as SEQ ID NO: 8. The recombinant baculovirus containing the PCV2 ORF2 gene was plaque-purified and Master Seed Virus (MSV) was propagated on the SF+ cell line, aliquotted, and stored at −70° C. The MSV was positively identified as PCV2 ORF2 baculovirus by PCR-RFLP using baculovirus specific primers. Insect cells infected with PCV2 ORF2 baculovirus to generate MSV or Working Seed Virus express PCV2 ORF2 antigen as detected by polyclonal serum or monoclonal antibodies in an indirect fluorescent antibody assay. Additionally, the identity of the PCV2 ORF2 baculovirus was confirmed by N-terminal amino acid sequencing. The PCV2 ORF2 baculovirus MSV was also tested for purity in accordance with 9 C.F.R. 113.27 (c), 113.28, and 113.55. Each recombinant baculovirus seeded into the spinner flasks had varying multiplicities of infection (MOIs). Flask 1 was seeded with 7.52 mL of 0.088 MOI seed; flask 2 was seeded with 3.01 mL of 0.36 MOI seed; flask 3 was seeded with 1.5 mL of 0.18 MOI seed; and flask 4 was seeded with 0.75 mL of 0.09 MOI seed. A schematic flow diagram illustrating the basic steps used to construct a PCV2 ORF2 recombinant baculovirus is provided herein as FIG. 1 .
[0095] After being seeded with the baculovirus, the flasks were then incubated at 27±2° C. for 7 days and were also agitated at 100 rpm during that time. The flasks used ventilated caps to allow for air flow. Samples from each flask were taken every 24 hours for the next 7 days. After extraction, each sample was centrifuged, and both the pellet and the supernatant were separated and then microfiltered through a 0.45-1.0 μm pore size membrane.
[0096] The resulting samples then had the amount of ORF2 present within them quantified via an ELISA assay. The ELISA assay was conducted with capture antibody Swine anti-PCV2 Pab IgG Prot. G purified (diluted 1:250 in PBS) diluted to 1:6000 in 0.05M Carbonate buffer (pH 9.6). 100 μL of the antibody was then placed in the wells of the mictrotiter plate, sealed, and incubated overnight at 37° C. The plate was then washed three times with a wash solution which comprised 0.5 mL of Tween 20 (Sigma, St. Louis, Mo.), 100 mL of 10× D-PBS (Gibco Invitrogen, Carlsbad, Calif.) and 899.5 mL of distilled water. Subsequently, 250 μL of a blocking solution (5 g Carnation Non-fat dry milk (Nestle, Glendale, Calif.) in 10 mL of D-PBS QS to 100 mL with distilled water) was added to each of the wells. The next step was to wash the test plate and then add pre-diluted antigen. The pre-diluted antigen was produced by adding 200 μL of diluent solution (0.5 mL Tween 20 in 999.5 mL D-PBS) to each of the wells on a dilution plate. The sample was then diluted at a 1:240 ratio and a 1:480 ratio, and 100 μL of each of these diluted samples was then added to one of the top wells on the dilution plate (i.e. one top well received 100 μL of the 1:240 dilution and the other received 100 μL of the 1:480 dilution). Serial dilutions were then done for the remainder of the plate by removing 100 μL form each successive well and transferring it to the next well on the plate. Each well was mixed prior to doing the next transfer. The test plate washing included washing the plate three times with the wash buffer. The plate was then sealed and incubated for an hour at 37° C. before being washed three more times with the wash buffer. The detection antibody used was monoclonal antibody to PCV ORF2. It was diluted to 1:300 in diluent solution, and 100 μL of the diluted detection antibody was then added to the wells. The plate was then sealed and incubated for an hour at 37° C. before being washed three times with the wash buffer. Conjugate diluent was then prepared by adding normal rabbit serum (Jackson Immunoresearch, West Grove, Pa.) to the diluent solution to 1% concentration. Conjugate antibody Goat anti-mouse (H+1)-HRP (Jackson Immunoresearch) was diluted in the conjugate diluent to 1:10,000. 100 μL of the diluted conjugate antibody was then added to each of the wells. The plate was then sealed and incubated for 45 minutes at 37° C. before being washed three times with the wash buffer. 100 μL of substrate (TMB Peroxidase Substrate, Kirkgaard and Perry Laboratories (KPL), Gaithersburg, Md.), mixed with an equal volume of Peroxidase Substrate B (KPL) was added to each of the wells. The plate was incubated at room temperature for 15 minutes. 100 μL of 1N HCL solution was then added to all of the wells to stop the reaction. The plate was then run through an ELISA reader. The results of this assay are provided in Table 1 below:
[0000]
TABLE 1
Day
Flask
ORF2 in pellet (μg)
ORF2 in supernatant (μg)
3
1
47.53
12
3
2
57.46
22
3
3
53.44
14
3
4
58.64
12
4
1
43.01
44
4
2
65.61
62
4
3
70.56
32
4
4
64.97
24
5
1
31.74
100
5
2
34.93
142
5
3
47.84
90
5
4
55.14
86
6
1
14.7
158
6
2
18.13
182
6
3
34.78
140
6
4
36.88
146
7
1
6.54
176
7
2
12.09
190
7
3
15.84
158
7
4
15.19
152
[0097] These results indicate that when the incubation time is extended, expression of ORF2 into the supernatant of the centrifuged cells and media is greater than expression in the pellet of the centrifuged cells and media. Accordingly, allowing the ORF2 expression to proceed for at least 5 days and recovering it in the supernate rather than allowing expression to proceed for less than 5 days and recovering ORF2 from the cells, provides a great increase in ORF2 yields, and a significant improvement over prior methods.
Example 2
[0098] This example provides data as to the efficacy of the invention claimed herein. A 1000 mL spinner flask was seeded with approximately 1.0×10 6 Sf+ cells/ml in 300 mL of Excell 420 media. The flask was then incubated at 27° C. and agitated at 100 rpm. Subsequently, the flask was seeded with 10 mL of PCV2 ORF2/Bac p+6 (the recombinant baculovirus containing the PCV2 ORF2 gene passaged 6 additional times in the Sf9 insect cells) virus seed with a 0.1 MOI after 24 hours of incubation.
[0099] The flask was then incubated at 27° C. for a total of 6 days. After incubation, the flask was then centrifuged and three samples of the resulting supernatant were harvested and inactivated. The supernatant was inactivated by bringing its temperature to 37±2° C. To the first sample, a 0.4M solution of 2-bromoethyleneamine hydrobromide which had been cyclized to 0.2M binary ethlylenimine (BEI) in 0.3N NaOH is added to the supernatant to give a final concentration of BEI of 5 mM. To the second sample, 10 mM BEI was added to the supernatant. To the third sample, no BEI was added to the supernatant. The samples were then stirred continuously for 48 hrs. A 1.0 M sodium thiosulfate solution to give a final minimum concentration of 5 mM was added to neutralize any residual BEI. The quantity of ORF2 in each sample was then quantified using the same ELISA assay procedure as described in Example 1. The results of this may be seen in Table 2 below:
[0000]
TABLE 2
Sample
ORF2 in supernatant (μg)
1
78.71
2
68.75
3
83.33
[0100] This example demonstrates that neutralization with BEI does not remove or degrade significant amounts of the recombinant PCV2 ORF2 protein product. This is evidenced by the fact that there is no large loss of ORF2 in the supernatant from the BEI or elevated temperatures. Those of skill in the art will recognize that the recovered ORF2 is a stable protein product.
Example 3
[0101] This example demonstrates that the present invention is scalable from small scale production of recombinant PCV2 ORF2 to large scale production of recombinant PCV2 ORF2. 5.0×10 5 cells/ml of SF+ cells/ml in 7000 mL of ExCell 420 media was planted in a 20000 mL Applikon Bioreactor. The media and cells were then incubated at 27° C. and agitated at 100 RPM for the next 68 hours. At the 68 th hour, 41.3 mL of PCV2 ORF2 Baculovirus MSV+3 was added to 700 mL of ExCell 420 medium. The resultant mixture was then added to the bioreactor. For the next seven days, the mixture was incubated at 27° C. and agitated at 100 RPM. Samples from the bioreactor were extracted every 24 hours beginning at day 4, post-infection, and each sample was centrifuged. The supernatant of the samples were preserved and the amount of ORF2 was then quantified using SDS-PAGE densitometry. The results of this can be seen in Table 3 below:
[0000]
TABLE 3
Day after infection:
ORF2 in supernatant (μg/mL)
4
29.33
5
41.33
6
31.33
7
60.67
Example 4
[0102] This example tests the efficacy of seven PCV2 candidate vaccines and further defines efficacy parameters following exposure to a virulent strain of PCV2. One hundred and eight (108) cesarean derived colostrum deprived (CDCD) piglets, 9-14 days of age, were randomly divided into 9 groups of equal size. Table 4 sets forth the General Study Design for this Example.
[0000]
TABLE 4
General Study Design
Challenged
KLH/ICFA
with
on Day
Virulent
No. Of
Day of
21 and
PCV2 on
Necropsy
Group
Pigs
Treatment
Treatment
Day 27
Day 24
on Day 49
1
12
PCV2 Vaccine No. 1 -
0
+
+
+
(vORF2 16 μg)
2
12
PCV2 Vaccine No. 2 -
0
+
+
+
(vORF2 8 μg)
3
12
PCV2 Vaccine No. 3 -
0
+
+
+
(vORF2 4 μg)
4
12
PCV2 Vaccine No. 4 -
0
+
+
+
(rORF2 16 μg)
5
12
PCV2 Vaccine No. 5 -
0
+
+
+
(rORF2 8 μg)
6
12
PCV2 Vaccine No. 6 -
0
+
+
+
(rORF2 4 μg)
7
12
PCV2 Vaccine No. 7 -
0
+
+
+
(Killed whole cell
virus)
8
12
None - Challenge
N/A
+
+
+
Controls
9
12
None - Strict
N/A
+
−
+
Negative Control
Group
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
killed whole cell virus = PCV2 virus grown in suitable cell culture
[0103] Seven of the groups (Groups 1-7) received doses of PCV2 ORF2 polypeptide, one of the groups acted as a challenge control and received no PCV2 ORF2, and another group acted as the strict negative control group and also received no PCV2 ORF2. On Day 0, Groups 1 through 7 were treated with assigned vaccines. Piglets in Group 7 were given a booster treatment on Day 14. Piglets were observed for adverse events and injection site reactions following vaccination and on Day 19, piglets were moved to the second study site. At the second study site, Groups 1-8 were group housed in one building while Group 9 was housed in a separate building. All pigs received keyhole limpet hemocyanin (KLH)/incomplete Freund's adjuvant (ICFA) on Days 21 and 27 and on Day 24, Groups 1-8 were challenged with a virulent PCV2.
[0104] Pre- and post-challenge, blood samples were collected for PCV2 serology. Post-challenge, body weight data for determination of average daily weight gain (ADWG), and clinical symptoms, as well as nasal swab samples to determine nasal shedding of PCV2, were collected. On Day 49, all surviving pigs were necropsied, lungs were scored for lesions, and selected tissues were preserved in formalin for Immunohistochemistry (IHC) testing at a later date.
Materials and Methods
[0105] This was a partially blinded vaccination-challenge feasibility study conducted in CDCD pigs, 9 to 14 days of age on Day 0. To be included in the study, PCV2 IFA titers of sows were ≦1:1000. Additionally, the serologic status of sows were from a known PRRS-negative herd. Twenty-eight (28) sows were tested for PCV2 serological status. Fourteen (14) sows had a PCV2 titer of ≦1000 and were transferred to the first study site. One hundred ten (110) piglets were delivered by cesarean section surgeries and were available for this study on Day −4. On Day −3, 108 CDCD pigs at the first study site were weighed, identified with ear tags, blocked by weight and randomly assigned to 1 of 9 groups, as set forth above in table 4. If any test animal meeting the inclusion criteria was enrolled in the study and was later excluded for any reason, the Investigator and Monitor consulted in order to determine the use of data collected from the animal in the final analysis. The date of which enrolled piglets were excluded and the reason for exclusion was documented. Initially, no sows were excluded. A total of 108 of an available 110 pigs were randomly assigned to one of 9 groups on Day −3. The two smallest pigs (No. 17 and 19) were not assigned to a group and were available as extras, if needed. During the course of the study, several animals were removed. Pig 82 (Group 9) on Day −1, Pig No. 56 (Group 6) on Day 3, Pig No. 53 (Group 9) on Day 4, Pig No. 28 (Group 8) on Day 8, Pig No. 69 (Group 8) on Day 7, and Pig No. 93 (Group 4) on Day 9, were each found dead prior to challenge. These six pigs were not included in the final study results. Pig no 17 (one of the extra pigs) was assigned to Group 9. The remaining extra pig, No. 19, was excluded from the study.
[0106] The formulations given to each of the groups were as follows: Group 1 was designed to administer 1 ml of viral ORF2 (vORF2) containing 16 μg ORF2/ml. This was done by mixing 10.24 ml of viral ORF2 (256 μg/25 μg/ml=10.24 ml vORF2) with 3.2 ml of 0.5% Carbopol and 2.56 ml of phosphate buffered saline at a pH of 7.4. This produced 16 ml of formulation for group 1. Group 2 was designed to administer 1 ml of vORF2 containing 8 μg vORF2/ml. This was done by mixing 5.12 ml of vORF2 (128 μg/25 μg/ml=5.12 ml vORF2) with 3.2 ml of 0.5% Carbopol and 7.68 ml of phosphate buffered saline at a pH of 7.4. This produced 16 ml of formulation for group 2. Group 3 was designed to administer 1 ml of vORF2 containing 4 μg vORF2/ml. This was done by mixing 2.56 ml of vORF2 (64 μg/25 μg/ml=2.56 ml vORF2) with 3.2 ml of 0.5% Carbopol and 10.24 ml of phosphate buffered saline at a pH of 7.4. This produced 16 ml of formulation for group 3. Group 4 was designed to administer 1 ml of recombinant ORF2 (rORF2) containing 16 μg rORF2/ml. This was done by mixing 2.23 ml of rORF2 (512 μg/230 μg/ml=2.23 ml rORF2) with 6.4 ml of 0.5% Carbopol and 23.37 ml of phosphate buffered saline at a pH of 7.4. This produced 32 ml of formulation for group 4. Group 5 was designed to administer 1 ml of rORF2 containing 8 μg rORF2/ml. This was done by mixing 1.11 ml of rORF2 (256 μg/230 μg/ml=1.11 ml rORF2) with 6.4 ml of 0.5% Carbopol and 24.49 ml of phosphate buffered saline at a pH of 7.4. This produced 32 ml of formulation for group 5. Group 6 was designed to administer 1 ml of rORF2 containing 8 μg rORF2/ml. This was done by mixing 0.56 ml of rORF2 (128 μg/230 μg/ml=0.56 ml rORF2) with 6.4 ml of 0.5% Carbopol and 25.04 ml of phosphate buffered saline at a pH of 7.4. This produced 32 ml of formulation for group 6. Group 7 was designed to administer 2 ml of PCV2 whole killed cell vaccine (PCV2 KV) containing the MAX PCV2 KV. This was done by mixing 56 ml of PCV2 KV with 14 ml of 0.5% Carbopol. This produced 70 ml of formulation for group 7. Finally group 8 was designed to administer KLH at 0.5 μg/ml or 1.0 μg/ml per 2 ml dose. This was done by mixing 40.71 ml KLH (7.0 μg protein/ml at 0.5 μg/ml=570 ml (7.0 μg/ml)(x)=(0.5)(570 ml)), 244.29 ml phosphate buffered saline at a pH of 7.4, and 285 ml Freunds adjuvant. Table 5 describes the time frames for the key activities of this Example.
[0000]
TABLE 5
Study Activities
Study
Day
Study Activity
−4, 0 to
General observations for overall health and clinical symptoms
49
−3
Weighed; Randomized to groups; Collected blood samples
from all pigs
0
Health examination; Administered IVP Nos. 1-7 to Groups 1-7,
respectively
0-7
Observed pigs for injection site reactions
14
Boostered Group 7 with PCV2 Vaccine No. 7; Blood samples
from all pigs
14-21
Observed Group 7 for injection site reactions
16-19
Treated all pigs with antibiotics (data missing)
19
Pigs transported from the first test site to a second test site
21
Treated Groups 1-9 with KLH/ICFA
24
Collected blood and nasal swab samples from all pigs;
Weighed all pigs; Challenged Groups 1-8 with PCV2 challenge
material
25, 27,
Collected nasal swab samples from all pigs
29, 31,
33, 35,
37, 39,
41, 43,
45, 47
27
Treated Groups 1-9 with KLH/ICFA
31
Collected blood samples from all pigs
49
Collected blood and nasal swab samples from all pigs;
Weighed all pigs; Necropsy all pigs; Gross lesions noted with
emphasis placed on icterus and gastric ulcers; Lungs evaluated
for lesions; Fresh and formalin fixed tissue samples saved; In-
life phase of the study completed
[0107] Following completion of the in-life phase of the study, formalin fixed tissues were examined by Immunohistochemistry (IHC) for detection of PCV2 antigen by a pathologist, blood samples were evaluated for PCV2 serology, nasal swab samples were evaluated for PCV2 shedding, and average daily weight gain (ADWG) was determined from Day 24 to Day 49.
[0108] Animals were housed at the first study site in individual cages in five rooms from birth to approximately 11 days of age (approximately Day 0 of the study). Each room was identical in layout and consisted of stacked individual stainless steel cages with heated and filtered air supplied separately to each isolation unit. Each room had separate heat and ventilation, thereby preventing cross-contamination of air between rooms. Animals were housed in two different buildings at the second study site. Group 9 (The Strict negative control group) was housed separately in a converted finisher building and Groups 1-8 were housed in converted nursery building. Each group was housed in a separate pen (11-12 pigs per pen) and each pen provided approximately 3.0 square feet per pig. Each pen was on an elevated deck with plastic slatted floors. A pit below the pens served as a holding tank for excrement and waste. Each building had its own separate heating and ventilation systems, with little likelihood of cross-contamination of air between buildings.
[0109] At the first study site, piglets were fed a specially formulated milk ration from birth to approximately 3 weeks of age. All piglets were consuming solid, special mixed ration by Day 19 (approximately 4½ weeks of age). At the second study site, all piglets were fed a custom non-medicated commercial mix ration appropriate for their age and weight, ad libitum. Water at both study sites was also available ad libitum.
[0110] All test pigs were treated with Vitamin E on Day −2, with iron injections on Day −1 and with NAXCEL® (1.0 mL, 1M, in alternating hams) on Days 16, 17, 18 and 19. In addition, Pig No. 52 (Group 9) was treated with an iron injection on Day 3, Pig 45 (Group 6) was treated with an iron injection on Day 11, Pig No. 69 (Group 8) was treated with NAXCEL® on Day 6, Pig No. 74 (Group 3) was treated with dexamethazone and penicillin on Day 14, and Pig No. 51 (Group 1) was treated with dexamethazone and penicillin on Day 13 and with NAXCEL® on Day 14 for various health reasons.
[0111] While at both study sites, pigs were under veterinary care. Animal health examinations were conducted on Day 0 and were recorded on the Health Examination Record Form. All animals were in good health and nutritional status before vaccination as determined by observation on Day 0. All test animals were observed to be in good health and nutritional status prior to challenge. Carcasses and tissues were disposed of by rendering. Final disposition of study animals was records on the Animal Disposition Record.
[0112] On Day 0, pigs assigned to Groups 1-6 received 1.0 mL of PCV2 Vaccines 1-6, respectively, IM in the left neck region using a sterile 3.0 mL Luer-lock syringe and a sterile 20 g×½″ needle. Pigs assigned to Group 7 received 2.0 mL of PCV2 Vaccine No. 7 IM in the left neck region using a sterile 3.0 mL Luer-lock syringe and a sterile 20 g×½″ needle. On Day 14, pigs assigned to Group 7 received 2.0 mL of PCV2 Vaccine No. 7 IM in the right neck region using a sterile 3.0 mL Luer-lock syringe and a sterile 20 g×½″ needle.
[0113] On Day 21 all test pigs received 2.0 mL of KLH/ICFA IM in the right ham region using a sterile 3.0 mL Luer-lock syringe and a sterile 20 g×1″ needle. On Day 27 all test pigs received 2.0 mL of KLH/ICFA in the left ham region using a sterile 3.0 mL Luer-lock syringe and a sterile 20 g×1″ needle.
[0114] On Day 24, pigs assigned to Groups 1-8 received 1.0 mL of PCV2 ISUVDL challenge material (5.11 log 10 TCID 50 /mL) IM in the left neck region using a sterile 3.0 mL Luer-lock syringe and a sterile 20 g×1″ needle. An additional 1.0 mL of the same material was administered IN to each pig (0.5 mL per nostril) using a sterile 3.0 mL Luer-lock syringe and nasal canula.
[0115] Test pigs were observed daily for overall health and adverse events on Day −4 and from Day 0 to Day 19. Observations were recorded on the Clinical Observation Record. All test pigs were observed from Day 0 to Day 7, and Group 7 was further observed from Day 14 to 21, for injection site reactions. Average daily weight gain was determined by weighing each pig on a calibrated scale on Days −3, 24 and 49, or on the day that a pig was found dead after challenge. Body weights were recorded on the Body Weight Form. Day −3 body weights were utilized to block pigs prior to randomization. Day 24 and Day 49 weight data was utilized to determine the average daily weight gain (ADWG) for each pig during these time points. For pigs that died after challenge and before Day 49, the ADWG was adjusted to represent the ADWG from Day 24 to the day of death.
[0116] In order to determine PCV2 serology, venous whole blood was collected from each piglet from the orbital venous sinus on Days −3 and 14. For each piglet, blood was collected from the orbital venous sinus by inserting a sterile capillary tube into the medial canthus of one of the eyes and draining approximately 3.0 mL of whole blood into a 4.0 mL Serum Separator Tube (SST). On Days 24, 31, and 49, venous whole blood from each pig was collected from the anterior vena cava using a sterile 18 g×1½″ Vacutainer needle (Becton Dickinson and Company, Franklin Lakes, N.J.), a Vacutainer needle holder and a 13 mL SST. Blood collections at each time point were recorded on the Sample Collection Record. Blood in each SST was allowed to clot, each SST was then spun down and the serum harvested. Harvested serum was transferred to a sterile snap tube and stored at −70±10° C. until tested at a later date. Serum samples were tested for the presence of PCV2 antibodies by BIVI-R&D personnel.
[0117] Pigs were observed once daily from Day 20 to Day 49 for clinical symptoms and clinical observations were recorded on the Clinical Observation Record.
[0118] To test for PCV2 nasal shedding, on Days 24, 25, and then every other odd numbered study day up to and including Day 49, a sterile dacron swab was inserted intra nasally into either the left or right nostril of each pig (one swab per pig) as aseptically as possible, swished around for a few seconds and then removed. Each swab was then placed into a single sterile snap-cap tube containing 1.0 mL of EMEM media with 2% IFBS, 500 units/mL of Penicillin, 500 μg/mL of Streptomycin and 2.5 μg/mL of Fungizone. The swab was broken off in the tube, and the snap tube was sealed and appropriately labeled with animal number, study number, date of collection, study day and “nasal swab.” Sealed snap tubes were stored at −40±10° C. until transported overnight on ice to BIVI-St. Joseph. Nasal swab collections were recorded on the Nasal Swab Sample Collection Form. BIVI-R&D conducted quantitative virus isolation (VI) testing for PCV2 on nasal swab samples. The results were expressed in log 10 values. A value of 1.3 logs or less was considered negative and any value greater than 1.3 logs was considered positive.
[0119] Pigs that died (Nos. 28, 52, 56, 69, 82, and 93) at the first study site were necropsied to the level necessary to determine a diagnosis. Gross lesions were recorded and no tissues were retained from these pigs. At the second study site, pigs that died prior to Day 49 (Nos. 45, 23, 58, 35), pigs found dead on Day 49 prior to euthanasia (Nos. 2, 43) and pigs euthanized on Day 49 were necropsied. Any gross lesions were noted and the percentages of lung lobes with lesions were recorded on the Necropsy Report Form.
[0120] From each of the 103 pigs necropsied at the second study site, a tissue sample of tonsil, lung, heart, liver, mesenteric lymph node, kidney and inguinal lymph node was placed into a single container with buffered 10% formalin; while another tissue sample from the same aforementioned organs was placed into a Whirl-pak (M-Tech Diagnostics Ltd., Thelwall, UK) and each Whirl-pak was placed on ice. Each container was properly labeled. Sample collections were recorded on the Necropsy Report Form. Afterwards, formalin-fixed tissue samples and a Diagnostic Request Form were submitted for IHC testing. IHC testing was conducted in accordance with standard ISU laboratory procedures for receiving samples, sample and slide preparation, and staining techniques. Fresh tissues in Whirl-paks were shipped with ice packs to the Study Monitor for storage (−70°±10° C.) and possible future use. Formalin-fixed tissues were examined by a pathologist for detection of PCV2 by IHC and scored using the following scoring system: 0=None; 1=Scant positive staining, few sites; 2=Moderate positive staining, multiple sites; and 3=Abundant positive staining, diffuse throughout the tissue. Due to the fact that the pathologist could not positively differentiate inguinal LN from mesenteric LN, results for these tissues were simply labeled as Lymph Node and the score given the highest score for each of the two tissues per animal.
Results
[0121] Results for this example are given below. It is noted that one pig from Group 9 died before Day 0, and 5 more pigs died post-vaccination (1 pig from Group 4; 1 pig from Group 6; 2 pigs from Group 8; and 1 pig from Group 9). Post-mortem examination indicated all six died due to underlying infections that were not associated with vaccination or PMWS. Additionally, no adverse events or injection site reactions were noted with any groups.
[0122] Average daily weight gain (ADWG) results are presented below in Table 6. Group 9, the strict negative control group, had the highest ADWG (1.06±0.17 lbs/day), followed by Group 5 (0.94±0.22 lbs/day), which received one dose of 8 μg of rORF2. Group 3, which received one dose of 4 μg of vORF2, had the lowest ADWG (0.49±0.21 lbs/day), followed by Group 7 (0.50±0.15 lbs/day), which received 2 doses of killed vaccine.
[0000]
TABLE 6
Summary of Group Average Daily Weight Gain (ADWG)
ADWG - lbs/day (Day 24 to
Day 49) or adjusted for
Group
Treatment
N
pigs dead before Day 29
1
vORF2 - 16 μg (1 dose)
12
0.87 ± 0.29 lbs/day
2
vORF2 - 8 μg (1 dose)
12
0.70 ± 0.32 lbs/day
3
vORF2 - 4 μg (1 dose)
12
0.49 ± 0.21 lbs/day
4
rORF2 - 16 μg (1 dose)
11
0.84 ± 0.30 lbs/day
5
rORF2 - 8 μg (1 dose)
12
0.94 ± 0.22 lbs/day
6
rORF2 - 4 μg (1 dose)
11
0.72 ± 0.25 lbs/day
7
KV (2 doses)
12
0.50 ± 0.15 lbs/day
8
Challenge Controls
10
0.76 ± 0.19 lbs/day
9
Strict Negative Controls
11
1.06 ± 0.17 lbs/day
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
killed whole cell virus = PCV2 virus grown in suitable cell culture
[0123] PCV2 serology results are presented below in Table 7. All nine groups were seronegative for PCV2 on Day −3. On Day 14, Groups receiving vORF2 vaccines had the highest titers, which ranged from 187.5 to 529.2. Pigs receiving killed viral vaccine had the next highest titers, followed by the groups receiving rORF2 vaccines. Groups 8 and 9 remained seronegative at this time. On Day 24 and Day 31, pigs receiving vORF2 vaccines continued to demonstrate a strong serological response, followed closely by the group that received two doses of a killed viral vaccine. Pigs receiving rORF2 vaccines were slower to respond serologically and Groups 8 and 9 continued to remain seronegative. On Day 49, pigs receiving vORF2 vaccine, 2 doses of the killed viral vaccine and the lowest dose of rORF2 demonstrated the strongest serological responses. Pigs receiving 16 μg and 8 μg of rORF2 vaccines had slightly higher IFA titers than challenge controls. Group 9 on Day 49 demonstrated a strong serological response.
[0000]
TABLE 7
Summary of Group PCV2 IFA Titers
AVERAGE IFA TITER
Group
Treatment
Day −3
Day 14
Day 24
Day 31**
Day 49***
1
vORF2 - 16 μg (1 dose)
50.0
529.2
4400.0
7866.7
11054.5
2
vORF2 - 8 μg (1 dose)
50.0
500.0
3466.7
6800.0
10181.8
3
vORF2 - 4 μg (1 dose)
50.0
187.5
1133.3
5733.3
9333.3
4
rORF2 - 16 μg (1 dose)
50.0
95.5
1550.0
3090.9
8000.0
5
rORF2 - 8 μg (1 dose)
50.0
75.0
887.5
2266.7
7416.7
6
rORF2 - 4 μg (1 dose)
50.0
50.0
550.0
3118.2
10570.0
7
KV (2 doses)
50.0
204.2
3087.5
4620.8
8680.0
8
Challenge Controls
50.0
55.0
50.0
50.0
5433.3
9
Strict Negative Controls
50.0
59.1
59.1
54.5
6136.4
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
killed whole cell virus = PCV2 virus grown in suitable cell culture
*For calculation purposes, a ≦ 100 IFA titer was designated as a titer of “50”; a ≧ 6400 IFA titer was designated as a titer of “12,800”.
**Day of Challenge
***Day of Necropsy
[0124] The results from the post-challenge clinical observations are presented below in Table 8. This summary of results includes observations for Abnormal Behavior, Abnormal Respiration, Cough and Diarrhea. Table 9 includes the results from the Summary of Group Overall Incidence of Clinical Symptoms and Table 10 includes results from the Summary of Group Mortality Rates Post-challenge. The most common clinical symptom noted in this study was abnormal behavior, which was scored as mild to severe lethargy. Pigs receiving the 2 lower doses of vORF2, pigs receiving 16 μg of rORF2 and pigs receiving 2 doses of KV vaccine had incidence rates of ≧27.3%. Pigs receiving 8 μg of rORF2 and the strict negative control group had no abnormal behavior. None of the pigs in this study demonstrated any abnormal respiration. Coughing was noted frequently in all groups (0 to 25%), as was diarrhea (0-20%). None of the clinical symptoms noted were pathognomic for PMWS.
[0125] The overall incidence of clinical symptoms varied between groups. Groups receiving any of the vORF2 vaccines, the group receiving 16 μg of rORF2, the group receiving 2 doses of KV vaccine and the challenge control group had the highest incidence of overall clinical symptoms (≧36.4%). The strict negative control group, the group receiving 8 μg of rORF2 and the group receiving 4 μg of rORF2 had overall incidence rates of clinical symptoms of 0%, 8.3% and 9.1%, respectively.
[0126] Overall mortality rates between groups varied as well. The group receiving 2 doses of KV vaccine had the highest mortality rate (16.7%); while groups that received 4 μg of vORF2, 16 μg of rORF2, or 8 μg of rORF2 and the strict negative control group all had 0% mortality rates.
[0000]
TABLE 8
Summary of Group Observations for Abnormal Behavior, Abnormal
Respiration, Cough, and Diarrhea
Abnormal
Abnormal
Group
Treatment
N
Behavior 1
Behavior 2
Cough 3
Diarrhea 4
1
vORF2 - 16 μg (1 dose)
12
2/12
0/12
3/12
2/12
(16.7%
(0%)
(25%)
(16/7%)
2
vORF2 - 8 μg (1 dose)
12
4/12
0/12
1/12
1/12
(33.3%)
(0%)
(8.3%
(8.3%)
3
vORF2 - 4 μg (1 dose)
12
8/12
0/12
2/12
1/12
(66.7%)
(0%)
(16.7%)
(8.3%)
4
rORF2 - 16 μg (1 dose)
11
3/11
0/11
0/11
2/11
(27.3%)
(0%)
(0%)
(18.2%)
5
rORF2 - 8 μg (1 dose)
12
0/12
0/12
1/12
0/12
(0%)
(0%)
(8.3%)
(0%)
6
rORF2 - 4 μg (1 dose)
11
1/11
0/11
0/11
0/12
(9.1%)
(0%)
(0%)
(0%)
7
KV (2 doses)
12
7/12
0/12
0/12
1/12
(58.3)
(0%)
(0%)
(8.3%)
8
Challenge Controls
10
1/10
0/10
2/10
2/10
(10%)
(0%)
(20%)
(20%)
9
Strict Negative Controls
11
0/11
0/11
0/11
0/11
(0%)
(0%)
(0%)
(0%)
vORF2 = isolated viral ORF2; rORF2 = recombinant baculovirus expressed ORF2; killed whole cell virus = PCV2 virus grown in suitable cell culture
1 Total number of pigs in each group that demonstrated any abnormal behavior for at least one day
2 Total number of pigs in each group that demonstrated any abnormal respiration for at least one day
3 Total number of pigs in each group that demonstrated a cough for at least one day
4 Total number of pigs in each group that demonstrated diarrhea for at least one day
[0000]
TABLE 9
Summary of Group Overall Incidence of Clinical Symptoms
Incidence of
pigs with
Incidence
Group
Treatment
N
Clinical Symptoms 1
Rate
1
vORF2 - 16 μg (1 dose)
12
5
41.7%
2
vORF2 - 8 μg (1 dose)
12
5
41.7%
3
vORF2 - 4 μg (1 dose)
12
8
66.7%
4
rORF2 - 16 μg (1 dose)
11
4
36.4%
5
rORF2 - 8 μg (1 dose)
12
1
8.3%
6
rORF2 - 4 μg (1 dose)
11
1
9.1%
7
KV (2 doses)
12
7
58.3%
8
Challenge Controls
10
4
40%
9
Strict Negative Controls
11
0
0%
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
killed whole cell virus = PCV2 virus grown in suitable cell culture
1 Total number of pigs in each group that demonstrated any clinical symptom for at least one day
[0000]
TABLE 10
Summary of Group Mortality Rates Post-challenge
Dead Post-
Group
Treatment
N
challenge
Mortality Rate
1
vORF2 - 16 μg (1 dose)
12
1
8.3%
2
vORF2 - 8 μg (1 dose)
12
1
8.3%
3
vORF2 - 4 μg (1 dose)
12
0
0%
4
rORF2 - 16 μg (1 dose)
11
0
0%
5
rORF2 - 8 μg (1 dose)
12
0
0%
6
rORF2 - 4 μg (1 dose)
11
1
9.1%
7
KV (2 doses)
12
2
16.7%
8
Challenge Controls
10
1
10%
9
Strict Negative Controls
11
0
0%
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
killed whole cell virus = PCV2 virus grown in suitable cell culture
[0127] PCV2 nasal shedding results are presented below in Table 11. Following challenge on Day 24, 1 pig in Group 7 began shedding PCV2 on Day 27. None of the other groups experienced shedding until Day 33. The bulk of nasal shedding was noted from Day 35 to Day 45. Groups receiving any of the three vORF2 vaccines and groups receiving either 4 or 8 μg of rORF2 had the lowest incidence of nasal shedding of PCV2 (≦9.1%). The challenge control group (Group 8) had the highest shedding rate (80%), followed by the strict negative control group (Group 9), which had an incidence rate of 63.6%.
[0000]
TABLE 11
Summary of Group Incidence of Nasal Shedding of PCV2
No. Of pigs
that shed
Incidence
Group
Treatment
N
for at least one day
Rate
1
vORF2 - 16 μg (1 dose)
12
1
8.3%
2
vORF2 - 8 μg (1 dose)
12
1
8.3%
3
vORF2 - 4 μg (1 dose)
12
1
8.3%
4
rORF2 - 16 μg (1 dose)
11
2
18.2%
5
rORF2 - 8 μg (1 dose)
12
1
8.3%
6
rORF2 - 4 μg (1 dose)
11
1
9.1%
7
KV (2 doses)
12
5
41.7%
8
Challenge Controls
10
8
80%
9
Strict Negative Controls
11
7
63.6%
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
killed whole cell virus = PCV2 virus grown in suitable cell culture
[0128] The Summary of Group Incidence of Icterus, Group Incidence of Gastric Ulcers, Group Mean Lung Lesion Scores, and Group Incidence of Lung Lesions are shown below in Table 12. Six pigs died at the first test site during the post-vaccination phase of the study (Group 4, N=1; Group 6, N=1; Group 8, N=2; Group 9, N=2). Four out of six pigs had fibrinous lesions in one or more body cavities, one pig (Group 6) had lesions consistent with clostridial disease, and one pig (Group 9) had no gross lesions. None of the pigs that died during the post-vaccination phased of the study had lesions consistent with PMWS.
[0129] Pigs that died post-challenge and pigs euthanized on Day 49 were necropsied. At necropsy, icterus and gastric ulcers were not present in any group. With regard to mean % lung lesions, Group 9 had lowest mean % lung lesions (0%), followed by Group 1 with 0.40±0.50% and Group 5 with 0.68±1.15%. Groups 2, 3, 7 and 8 had the highest mean % lung lesions (≧7.27%). Each of these four groups contained one pig with % lung lesions ≧71.5%, which skewed the results higher for these four groups. With the exception of Group 9 with 0% lung lesions noted, the remaining 8 groups had ≦36% lung lesions. Almost all lung lesions noted were described as red/purple and consolidated.
[0000]
TABLE 12
Summary of Group Incidence of Icterus, Group Incidence of Gastric Ulcers,
Group Mean % Lung Lesion Scores, and Group Incidence of Lung Lesions Noted
Incidence of
Gastric
Mean % Lung
Lung Lesions
Group
Treatment
Icterus
Ulcers
Lesions
Noted
1
vORF2 - 16 μg (1
0/12 (0%)
0/12
0.40 ± 0.50%
10/12
dose)
(0%)
(83%)
2
vORF2 - 8 μg (1 dose)
0/12 (0%)
0/12
7.41 ± 20.2%
10/12
(0%)
(83%)
3
vORF2 - 4 μg (1 dose)
0/12 (0%)
0/12
9.20 ± 20.9%
10/12
(0%)
(83%)
4
rORF2 - 16 μg (1
0/11 (0%)
0/11
1.5 ± 4.74%
4/11
dose)
(0%)
(36%)
5
rORF2 - 8 μg (1 dose)
0/12 (0%)
0/12
0.68 ± 1.15%
9/12
(0%)
(75%)
6
rORF2 - 4 μg (1 dose)
0/11 (0%)
0/11
2.95 ± 5.12%
7/11
(0%)
(64%)
7
KV (2 doses)
0/12 (0%)
0/12
7.27 ± 22.9%
9/12
(0%)
(75%)
8
Challenge Controls
0/10 (0%)
0/10
9.88 ± 29.2%
8/10
(0%)
(80%)
9
Strict Negative
0/11 (0%)
0/11
0/11
0/11
Controls
(0%)
(0%)
(0%)
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
KV or killed whole cell virus = PCV2 virus grown in suitable cell culture
[0130] The Summary of Group IHC Positive Incidence Results are shown in Table 13. Group 1 (vORF2—16 μg) and Group 5 (rORF2—8 μg) had the lowest rate of IHC positive results (16.7%). Group 8 (Challenge Controls) and Group 9 (Strict Negative Controls) had the highest rate of IHC positive results, 90% and 90.9%, respectively.
[0000]
TABLE 13
Summary of Group IHC Positive Incidence Rate
No. Of pigs that
had at least one
tissue positive
Incidence
Group
Treatment
N
for PCV2
Rate
1
vORF2 - 16 μg (1 dose)
12
2
16.7%
2
vORF2 - 8 μg (1 dose)
12
3
25.0%
3
vORF2 - 4 μg (1 dose)
12
8
66.7%
4
rORF2 - 16 μg (1 dose)
11
4
36.3%
5
rORF2 - 8 μg (1 dose)
12
2
16.7%
6
rORF2 - 4 μg (1 dose)
11
4
36.4%
7
KV (2 doses)
12
5
41.7%
8
Challenge Controls
10
9
90.0%
9
Strict Negative Controls
11
10
90.9%
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
KV or killed whole cell virus = PCV2 virus grown in suitable cell culture
[0131] Post-challenge, Group 5, which received one dose of 8 μg of rORF2 antigen, outperformed the other 6 vaccine groups. Group 5 had the highest ADWG (0.94±0.22 lbs/day), the lowest incidence of abnormal behavior (0%), the second lowest incidence of cough (8.3%), the lowest incidence of overall clinical symptoms (8.3%), the lowest mortality rate (0%), the lowest rate of nasal shedding of PCV2 (8.3%), the second lowest rate for mean % lung lesions (0.68±1.15%) and the lowest incidence rate for positive tissues (16.7%). Groups receiving various levels of rORF2 antigen overall outperformed groups receiving various levels of vORF2 and the group receiving 2 doses of killed whole cell PCV2 vaccine performed the worst. Tables 14 and 15 contain summaries of group post-challenge data.
[0000]
TABLE 14
Summary of Group Post-Challenge Data - Part 1
Overall
Incidence of
Abnormal
Clinical
Group
N
Treatment
ADWG (lbs/day)
Behavior
Cough
Symptoms
1
12
vORF2 - 16 μg
0.87 ± 0.29
2/12
3/12
41.7%
(1 dose)
(16.7%)
(25%)
2
12
vORF2 - 8 μg
0.70 ± 0.32
4/12
1/12
41.7%
(1 dose)
(33.3%
(8.3%
3
12
vORF2 - 4 μg
0.49 ± 0.21
8/12
2/12
66.7%
(1 dose)
(66.7%)
(16.7%
4
11
rORF2 - 16 μg
0.84 ± 0.30
3/11
0/11
36.4%
(1 dose)
(27.3%)
(0%)
5
12
rORF2 - 8 μg
0.94 ± 0.22
0/12
1/12
8.3%
(1 dose)
(0%)
(8.3%
6
11
rORF2 - 4 μg
0.72 ± 0.25
1/11
0/11
9.1%
(1 dose)
(9.1%
(0%)
7
12
KV
0.50 ± 0.15
7/12
0/12
58.3%
(2 doses)
(58.3)
(0%)
8
10
Challenge
0.76 ± 0.19
1/10
2/10
40%
Controls
(10%)
(20%
9
11
Strict Negative
1.06 ± 0.17
0/11
0/11
0%
Controls
(0%)
(0%)
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
KV or killed whole cell virus = PCV2 virus grown in suitable cell culture
[0000]
TABLE 15
Summary of Group Post-Challenge Data - Part 2
Mean %
Incidence Rate of at
Mortality
Nasal
Lung
least one tissue IHC
Group
N
Treatment
Rate
Shedding
Lesions
positive for PCV2
1
12
vORF2 - 16 μg
8.3%
8.3%
0.40 ± 0.50%
16.7%
(1 dose)
2
12
vORF2 - 8 μg
8.3%
8.3%
7.41 ± 20.2%
25.0%
(1 dose)
3
12
vORF2 - 4 μg
0%
8.3%
9.20 ± 20.9%
66.7%
(1 dose)
4
11
rORF2 - 16 μg
0%
18.2%
1.50 ± 4.74%
36.3%
(1 dose)
5
12
rORF2 - 8 μg
0%
8.3%
0.68 ± 1.15%
16.7%
(1 dose)
6
11
rORF2 - 4 μg
9.1%
9.1%
2.95 ± 5.12%
36.4%
(1 dose)
7
12
KV
16.7%
41.7%
7.27 ± 22.9%
41.7%
(2 doses)
8
10
Challenge
10%
80%
9.88 ± 29.2%
90.0%
Controls
9
11
Strict Negative
0%
63.6%
0/11
90.9%
Controls
(0%)
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
KV or killed whole cell virus = PCV2 virus grown in suitable cell culture
[0132] Results of this study indicate that all further vaccine efforts should focus on a rORF2 vaccine. Overall, nasal shedding of PCV2 was detected post-challenge and vaccination with a PCV2 vaccine resulted in a reduction of shedding. Immunohistochemistry of selected lymphoid tissues also served as a good parameter for vaccine efficacy, whereas large differences in ADWG, clinical symptoms, and gross lesions were not detected between groups. This study was complicated by the fact that extraneous PCV2 was introduced at some point during the study, as evidenced by nasal shedding of PCV2, PCV2 seroconversion and positive IHC tissues in Group 9, the strict negative control group.
Discussion
[0133] Seven PCV2 vaccines were evaluated in this study, which included three different dose levels of vORF2 antigen administered once on Day 0, three different dose levels of rORF2 antigen administered once on Day 0 and one dose level of killed whole cell PCV2 vaccine administered on Day 0 and Day 14. Overall, Group 5, which received 1 dose of vaccine containing 8 μg of rORF2 antigen, had the best results. Group 5 had the highest ADWG, the lowest incidence of abnormal behavior, the lowest incidence of abnormal respiration, the second lowest incidence of cough, the lowest incidence of overall clinical symptoms, the lowest mortality rate, the lowest rate of nasal shedding of PCV2, the second lowest rate for mean % lung lesions and the lowest incidence rate for positive IHC tissues.
[0134] Interestingly, Group 4, which received a higher dose of rORF2 antigen than Group 5, did not perform as well or better than Group 5. Group 4 had a slightly lower ADWG, a higher incidence of abnormal behavior, a higher incidence of overall clinical symptoms, a higher rate of nasal shedding of PCV2, a higher mean % lung lesions, and a higher rate for positive IHC tissues than Group 5. Statistical analysis, which may have indicated that the differences between these two groups were not statistically significant, was not conducted on these data, but there was an observed trend that Group 4 did not perform as well as Group 5.
[0135] Post-vaccination, 6 pigs died at the first study site. Four of the six pigs were from Group 8 or Group 9, which received no vaccine. None of the six pigs demonstrated lesions consistent with PMWS, no adverse events were reported and overall, all seven vaccines appeared to be safe when administered to pigs approximately 11 days of age. During the post-vaccination phase of the study, pigs receiving either of three dose levels of vORF2 vaccine or killed whole cell vaccine had the highest IFAT levels, while Group 5 had the lowest IFAT levels just prior to challenge, of the vaccine groups.
[0136] Although not formally proven, the predominant route of transmission of PCV2 to young swine shortly after weaning is believed to be by oronasal direct contact and an efficacious vaccine that reduces nasal shedding of PCV2 in a production setting would help control the spread of infection. Groups receiving one of three vORF2 antigen levels and the group receiving 8 μg of rORF2 had the lowest incidence rate of nasal shedding of PCV2 (8.3%). Expectedly, the challenge control group had the highest incidence rate of nasal shedding (80%).
[0137] Gross lesions in pigs with PMWS secondary to PCV2 infection typically consist of generalized lymphadenopathy in combination with one or a multiple of the following: (1) interstitial pneumonia with interlobular edema, (2) cutaneous pallor or icterus, (3) mottled atrophic livers, (4) gastric ulcers and (5) nephritis. At necropsy, icterus, hepatitis, nephritis, and gastric ulcers were not noted in any groups and lymphadenopathy was not specifically examined for. The mean % lung lesion scores varied between groups. The group receiving 16 μg of vORF2 antigen had the lowest mean % lung lesion score (0.40±0.50%), followed by the group that received 8 μg of rORF2 (0.68±1.15%). As expected, the challenge control group had the highest mean % lung lesion score (9.88±29.2%). In all four groups, the mean % lung lesion scores were elevated due to one pig in each of these groups that had very high lung lesion scores. Most of the lung lesions were described as red/purple and consolidated. Typically, lung lesions associated with PMWS are described as tan and non-collapsible with interlobular edema. The lung lesions noted in this study were either not associated with PCV2 infection or a second pulmonary infectious agent may have been present. Within the context of this study, the % lung lesion scores probably do not reflect a true measure of the amount of lung infection due to PCV2.
[0138] Other researchers have demonstrated a direct correlation between the presence of PCV2 antigen by IHC and histopathology. Histopathology on select tissues was not conducted with this study. Group 1 (16 μg of vORF2) and Group 5 (8 μg of rORF2) had the lowest incidence rate of pigs positive for PCV2 antigen (8.3%), while Group 9 (the strict negative control group −90.9%) and Group 8 (the challenge control group −90.0%) had the highest incidence rates for pigs positive for PCV2 antigen. Due to the non-subjective nature of this test, IHC results are probably one of the best parameters to judge vaccine efficacy on.
[0139] Thus, in one aspect of the present invention, the Minimum Portective Dosage (MPD) of a 1 ml/1 dose recombinant product with extracted PCV2 ORF2 (rORF2) antigen in the CDCD pig model in the face of a PCV2 challenge was determined. Of the three groups that received varying levels of rORF2 antigen, Group 5 (8 μg of rORF2 antigen) clearly had the highest level of protection. Group 5 either had the best results or was tied for the most favorable results with regard to all of the parameters examined. When Group 5 was compared with the other six vaccine groups post-challenge, Group 5 had the highest ADWG (0.94±0.22 lbs/day), the lowest incidence of abnormal behavior (0%), the second lowest incidence of cough (8.3%), the lowest incidence of overall clinical symptoms (8.3%), the lowest mortality rate (0%), the lowest rate of nasal shedding of PCV2 (8.3%), the second lowest rate for mean % lung lesions (0.68±1.15%) and the lowest incidence rate for positive IHC tissues (16.7%).
[0140] In another aspect of the present invention, the MPD of a 1 ml/1 dose conventional product that is partially purified PCV2 ORF2 (vORF2) antigen in the CDCD pig model in the face of a PCV2 challenge was determined. Of the three groups that received varying levels of vORF2 antigen, Group 1 (16 μg of vORF2) had the highest level of protection. Group 1 outperformed Groups 2 and 3 with respect to ADWG, mean % lung lesions, and IHC. Groups 1 and 2 (8 μg of vORF2 antigen) performed equally with respect to overall incidence of clinical symptoms, Group 3 (4 μg of vORF2 antigen) had the lowest mortality rate, and all three groups performed equally with respect to nasal shedding. Overall, vORF vaccines did not perform as well as rORF vaccines.
[0141] In yet another aspect of the present invention, the efficacy of a maximum dose of a 2 ml/2 dose Conventional Killed PCV2 vaccine in the CDCD pig model in the face of a PCV2 challenge was determined. Of the seven vaccines evaluated in this study, the killed whole cell PCV2 vaccine performed the worst. Piglets receiving two doses of killed whole cell PCV2 vaccine had the lowest ADWG, the second highest rate of abnormal behavior (58.3%), the second highest overall incidence of clinical symptoms (58.3%), the highest mortality rate (16.7%), the second highest incidence of nasal shedding (41.7%), highest mean % lung lesions (9.88±29.2%), a high incidence of lung lesions noted (75%) and a moderate IHC incidence rate in tissues (41.7%). However, it was still effective at invoking an immune response.
[0142] In still another aspect of the present invention, nasal shedding of PCV2 was assessed as an efficacy parameter and the previous PCV2 efficacy parameters from previous studies were reconfirmed. Results from this study indicate that nasal shedding of PCV2 occurs following intra nasal challenge and that PCV2 vaccines reduce nasal shedding of PCV2 post-challenge. Furthermore, results from this study and reports in the literature indicate that IHC should continue to be evaluated in future PCV2 vaccine trials as well.
[0143] Some additional conclusions arising from this study are that lymphadenopathy is one of the hallmarks of PMWS. Another one of the hallmarks of PMWS is lymphoid depletion and multinucleated/giant histiocytes. Additionally, no adverse events or injection site reactions were noted for any of the 7 PCV2 vaccines and all 7 PCV2 vaccines appeared to be safe when administered to young pigs.
Example 5
[0144] This example tests the efficacy of eight PCV2 candidate vaccines and reconfirms PCV2 challenge parameters from earlier challenge studies following exposure to a virulent strain of PCV2. One hundred and fifty (150) cesarean derived colostrum deprived (CDCD) piglets, 6-16 days of age, were blocked by weight and randomly divided into 10 groups of equal size. Table 16 sets forth the General Study Design for this Example.
[0000]
TABLE 16
General Study Design
Challenge
with
KLH/ICFA
Virulent
PRRSV
Necropsy
No. Of
Day of
on Day 22
PCV2 on
MLV on
on Day
Group
Pigs
Treatment
Treatment
and Day 28
Day 25
Day 46
50
1
15
PVC2 Vaccine 1
0 & 14
+
+
+
+
16 μg
rORF2 - IMS 1314
2
15
PVC2 Vaccine 2
0 & 14
+
+
+
+
16 μg
vORF2 - Carbopol
3
15
PCV2 Vaccine 3
0 & 14
+
+
+
+
16 μg
rORF2 - Carbopol
4
15
PCV2 Vaccine 2
0
+
+
+
+
16 μg
vORF2 - Carbopol
5
15
PVC2 Vaccine 3
0 & 14
+
+
+
+
4 μg
rORF2 - Carbopol
6
15
PVC2 Vaccine 3
0 & 14
+
+
+
+
1 μg
rORF2 - Carbopol
7
15
PVC2 Vaccine 3
0 & 14
+
+
+
+
0.25 μg
rORF2 - Carbopol
8
15
PVC2 Vaccine 4 >
0 & 14
+
+
+
+
8.0 log
KV - Carbopol
9
15
Challenge
N/A
+
+
+
+
Controls
10
15
None - Strict
N/A
+
−
+
+
Negative Control
Group
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
KV or killed whole cell virus = PCV2 virus grown in suitable cell culture
[0145] The vaccine formulation given to each group were as follows. PCV2 Vaccine No. 1, administered at 1×2 ml dose to Group 1, was a high dose (16 ug/2 ml dose) of inactivated recombinant ORF2 antigen adjuvanted with IMS 1314 (16 ug rORF2-IMS 1314). PCV2 Vaccine No. 2, administered at 1×2 ml dose to Group 2, was a high dose (16 ug/2 ml dose) of a partially purified VIDO R-1 generated PCV2 ORF2 antigen adjuvanted with Carbopol (16 ug vORF2—Carbopol). PCV2 Vaccine No. 3, administered at 1×2 ml dose to Group 3, was a high dose (16 ug/2 ml dose) of inactivated recombinant ORF2 antigen adjuvanted with Carbopol (16 ug rORF2—Carbopol). PCV2 Vaccine No. 4, administered at 1×1 ml dose to Group 4, was a high dose (16 ug/1 ml dose) of a partially purified VIDO R-1 generated PCV2 ORF2 antigen adjuvanted with Carbopol (16 ug vORF2—Carbopol). Vaccine No. 5, administered at 1×2 ml dose to Group 5, was a 4 ug/2 ml dose of an inactivated recombinant ORF2 antigen adjuvanted with Carbopol (4 ug rORF2—Carbopol). PCV2 Vaccine No. 6, administered at 1×2 ml dose to Group 6, was a 1 ug/2 ml dose of an inactivated recombinant ORF2 antigen adjuvanted with Carbopol (1 ug rORF2—Carbopol). PCV2 Vaccine No. 7, administered at 1×2 ml dose to Group 7, was a low dose (0.25 ug/2 ml dose) of inactivated recombinant ORF2 antigen adjuvanted with Carbopol (0.25 ug rORF2—Carbopol). PCV2 Vaccine No. 8, administered at 1×2 ml dose to Group 8, was a high dose (pre-inactivation titer>8.0 log/2 ml dose) Inactivated Conventional Killed VIDO R-1 generated PCV2 Struve antigen adjuvanted with Carbopol (>8.0 log KV—Carbopol). On Day 0, Groups 1-8 were treated with their assigned vaccines. Groups 1-3 and 5-8 received boosters of their respective vaccines again on Day 14. The effectiveness of a single dose of 16 μg of vORF2—Carbopol was tested on Group 4 which did not receive a booster on Day 14. Piglets were observed for adverse events and injection site reactions following both vaccinations. On Day 21 the piglets were moved to a second study site where Groups 1-9 were group housed in one building and Group 10 was housed in a separate building. All pigs received keyhole limpet hemocyanin emulsified with incomplete Freund's adjuvant (KLH/ICFA) on Days 22 and 28. On Day 25, Groups 1-9 were challenged with approximately 4 logs of virulent PCV2 virus. By Day 46, very few deaths had occurred in the challenge control group. In an attempt to immunostimulate the pigs and increase the virulence of the PCV2 challenge material, all Groups were treated with INGELVAC® PRRSV MLV (Porcine Reproductive and Respiratory Vaccine, Modified Live Virus) on Day 46.
[0146] Pre- and post-challenge blood samples were collected for PCV2 serology. Post-challenge, body weight data for determination of average daily weight gain (ADWG) and observations of clinical signs were collected. On Day 50, all surviving pigs were necropsied, gross lesions were recorded, lungs were scored for pathology, and selected tissues were preserved in formalin for examination by Immunohistochemistry (IHC) for detection of PCV2 antigen at a later date.
Materials and Methods
[0147] This was a partially-blind vaccination-challenge feasibility study conducted in CDCD pigs, 6 to 16 days of age on Day 0. To be included in the study, PCV2 IFA titers of sows were ≦1:1000. Additionally, the serologic status of sows were from a known PRRS-negative herd. Sixteen (16) sows were tested for PCV2 serological status and all sixteen (16) had a PCV2 titer of ≦1000 and were transferred to the first study site. One hundred fifty (150) piglets were delivered by cesarean section surgeries and were available for this study on Day −3. On Day −3, 150 CDCD pigs at the first study site were weighed, identified with ear tags, blocked by weight and randomly assigned to 1 of 10 groups, as set forth above in table 16. Blood samples were collected from all pigs. If any test animal meeting the inclusion criteria was enrolled in the study and was later excluded for any reason, the Investigator and Monitor consulted in order to determine the use of data collected from the animal in the final analysis. The date of which enrolled piglets were excluded and the reason for exclusion was documented. No sows meeting the inclusion criteria, selected for the study and transported to the first study site were excluded. No piglets were excluded from the study, and no test animals were removed from the study prior to termination. Table 17 describes the time frames for the key activities of this Example.
[0000]
TABLE 17
Study Activities
Study Day
Actual Dates
Study Activity
−3
Apr. 04, 2003
Weighed pigs; health exam; randomized to groups; collected
blood samples
−3,
Apr. 04, 2003
Observed for overall health and for adverse events post-
0-21
Apr. 07, 2003 to
vaccination
May 27, 2003
0
Apr. 07, 2003
Administered respective IVPs to Groups 1-8
0-7
Apr. 07, 2003 to
Observed pigs for injection site reactions
Apr. 14, 2003
14
Apr. 21, 2003
Boostered Groups 1-3, 5-8 with respective IVPs; blood
sampled all pigs
14-21
Apr. 21, 2003 to
Observed pigs for injection reactions
Apr. 28, 2003
19-21
Apr. 26, 2003 to
Treated all pigs with antibiotics
Apr. 28, 2003
21
Apr. 28, 2003
Pigs transported from Struve Labs, Inc. to Veterinary
Resources, Inc.(VRI)
22-50
Apr. 28, 2003 to
Observed pigs for clinical signs post-challenge
May 27, 2003
22
Apr. 29, 2003
Treated Groups 1-10 with KLH/ICFA
25
May 02, 2003
Collected blood samples from all pigs; weighed all pigs;
challenged Groups 1-9 with PCV2 challenge material
28
May 05, 2003
Treated Groups 1-10 with KLH/ICFA
32
May 09, 2003
Collected blood samples from all pigs
46
May 23, 2003
Administered INGELVAC ® PRRS MLV to all groups
50
May 27, 2003
Collected blood samples, weighed and necropsied all pigs;
gross lesions were recorded; lungs were evaluated for
lesions; fresh and formalin fixed tissue samples were saved;
In-life phase of the study was completed
[0148] Following completion of the in-life phase of the study, formalin fixed tissues were examined by Immunohistochemistry (IHC) for detection of PCV2 antigen by a pathologist, blood samples were evaluated for PCV2 serology, and average daily weight gain (ADWG) was determined from Day 25 to Day 50.
[0149] Animals were housed at the first study site in individual cages in seven rooms from birth to approximately 11 days of age (approximately Day 0 of the study). Each room was identical in layout and consisted of stacked individual stainless steel cages with heated and filtered air supplied separately to each isolation unit. Each room had separate heat and ventilation, thereby preventing cross-contamination of air between rooms. Animals were housed in two different buildings at the second study site. Group 10 (The Strict negative control group) was housed separately in a converted nursery building and Groups 1-9 were housed in a converted farrowing building. Each group was housed in a separate pen (14-15 pigs per pen) and each pen provided approximately 2.3 square feet per pig. Groups 2, 4 and 8 were penned in three adjacent pens on one side of the alleyway and Groups 1, 3, 5, 6, 7, and 9 were penned in six adjacent pens on the other side of the alleyway. The Group separation was due to concern by the Study Monitor that vaccines administered to Groups 2, 4, and 8 had not been fully inactivated. Each pen was on an elevated deck with plastic slatted floors. A pit below the pens served as a holding tank for excrement and waste. Each building had its own separate heating and ventilation systems, with little likelihood of cross-contamination of air between buildings.
[0150] At the first study site, piglets were fed a specially formulated milk ration from birth to approximately 3 weeks of age. All piglets were consuming solid, special mixed ration by Day 21 (approximately 4½ weeks of age). At the second study site, all piglets were fed a custom non-medicated commercial mix ration appropriate for their age and weight, ad libitum. Water at both study sites was also available ad libitum.
[0151] All test pigs were treated with 1.0 mL of NAXCEL®, IM, in alternating hams on Days 19, 20, and 21. In addition, Pig No. 11 (Group 1) was treated with 0.5 mL of NAXCEL® IM on Day 10, Pig No. 13 (Group 10) was treated with 1 mL of Penicillin and 1 mL of PREDEF® 2× on Day 10, Pig No. 4 (Group 9) was treated with 1.0 mL of NAXCEL® IM on Day 11, and Pigs 1 (Group 1), 4 and 11 were each treated with 1.0 mL of NAXCEL® on Day 14 for various health reasons.
[0152] While at both study sites, pigs were under veterinary care. Animal health examinations were conducted on Day −3 and were recorded on the Health Examination Record Form. All animals were in good health and nutritional status before vaccination as determined by observation on Day 0. All test animals were observed to be in good health and nutritional status prior to challenge. Carcasses and tissues were disposed of by rendering. Final disposition of study animals was recorded on the Animal Disposition Record.
[0153] On Days 0 and 14, pigs assigned to Groups 1-3 and 5-8 received 2.0 mL of assigned PCV2 Vaccines 1-4, respectively, IM in the right and left neck region, respectively, using a sterile 3.0 mL Luer-lock syringe and a sterile 20 g×½″ needle. Pigs assigned to Group 4 received 1.0 mL of PCV2 Vaccine No. 2, IM in the right neck region using a sterile 3.0 mL Luer-lock syringe and a sterile 20 g×½″ needle on Day 0 only.
[0154] On Day 22 all test pigs received 2.0 mL of KLH/ICFA IM in the left neck region using a sterile 3.0 mL Luer-lock syringe and a sterile 20 g×1″ needle. On Day 28 all test pigs received 2.0 mL of KLH/ICFA in the right ham region using a sterile 3.0 mL Luer-lock syringe and a sterile 20 g×1″ needle.
[0155] On Day 25, pigs assigned to Groups 1-9 received 1.0 mL of PCV2 ISUVDL challenge material (3.98 log 10 TCID 50 /mL) IM in the right neck region using a sterile 3.0 mL Luer-lock syringe and a sterile 20 g×1″ needle. An additional 1.0 mL of the same material was administered IN to each pig (0.5 mL per nostril) using a sterile 3.0 mL Luer-lock syringe and nasal canula.
[0156] On Day 46, all test pigs received 2.0 mL INGELVAC® PRRS MLV, IM, in the right neck region using a sterile 3.0 mL Luer0lock syringe and a sterile 20 g×1″ needle. The PRRSV MLV was administered in an attempt to increase virulence of the PCV2 challenge material.
[0157] Test pigs were observed daily for overall health and adverse events on Day −3 and from Day 0 to Day 21. Each of the pigs were scored for normal or abnormal behavior, respiration or cough. Observations were recorded on the Clinical Observation Record. All test pigs were observed from Day 0 to Day 7, and Group 7 was further observed from Day 14 to 21, for injection site reactions. Average daily weight gain was determined by weighing each pig on a calibrated scale on Days −3, 25 and 50, or on the day that a pig was found dead after challenge. Body weights were recorded on the Body Weight Form. Day −3 body weights were utilized to block pigs prior to randomization. Day 25 and Day 50 weight data was utilized to determine the average daily weight gain (ADWG) for each pig during these time points. For pigs that died after challenge and before Day 50, the ADWG was adjusted to represent the ADWG from Day 25 to the day of death.
[0158] In order to determine PCV2 serology, venous whole blood was collected from each piglet from the orbital venous sinus on Days −3 and 14. For each piglet, blood was collected from the orbital venous sinus by inserting a sterile capillary tube into the medial canthus of one of the eyes and draining approximately 3.0 mL of whole blood into a 4.0 mL Serum Separator Tube (SST). On Days 25, 32, and 50, venous whole blood from each pig was collected from the anterior vena cava using a sterile 20 g×1½″ Vacutainer® needle (Becton Dickinson and Company, Franklin Lakes, N.J.), a Vaccutainer® needle holder and a 13 mL SST. Blood collections at each time point were recorded on the Sample Collection Record. Blood in each SST was allowed to clot, each SST was then spun down and the serum harvested. Harvested serum was transferred to a sterile snap tube and stored at −70±10° C. until tested at a later date. Serum samples were tested for the presence of PCV2 antibodies by BIVI-R&D personnel.
[0159] Pigs were observed once daily from Day 22 to Day 50 for clinical symptoms and scored for normal or abnormal behavior, respiration or cough. Clinical observations were recorded on the Clinical Observation Record.
[0160] Pigs Nos. 46 (Group 1) and 98 (Groups 9) died at the first study site. Both of these deaths were categorized as bleeding deaths and necropsies were not conducted on these two pigs. At the second study site, pigs that died after challenge and prior to Day 50, and pigs euthanized on Day 50, were necropsied. Any gross lesions were noted and the percentages of lung lobes with lesions were recorded on the Necropsy Report Form.
[0161] From each of the pigs necropsied at the second study site, a tissue sample of tonsil, lung, heart, and mesenteric lymph node was placed into a single container with buffered 10% formalin; while another tissue sample from the same aforementioned organs was placed into a Whirl-pak® (M-Tech Diagnostics Ltd., Thelwall, UK) and each Whirl-pak® was placed on ice. Each container was properly labeled. Sample collections were recorded on the Necropsy Report Form. Afterwards, formalin-fixed tissue samples and a Diagnostic Request Form were submitted for IHC testing. IHC testing was conducted in accordance with standard laboratory procedures for receiving samples, sample and slide preparation, and staining techniques. Fresh tissues in Whirl-paks® were shipped with ice packs to the Study Monitor for storage (−70°±10° C.) and possible future use.
[0162] Formalin-fixed tissues were examined by a pathologist for detection of PCV2 by IHC and scored using the following scoring system: 0=None; 1=Scant positive staining, few sites; 2=Moderate positive staining, multiple sites; and 3=Abundant positive staining, diffuse throughout the tissue. For analytical purposes, a score of 0 was considered “negative,” and a score of greater than 0 was considered “positive.”
Results
[0163] Results for this example are given below. It is noted that Pigs No. 46 and 98 died on days 14 and 25 respectively. These deaths were categorized as bleeding deaths. Pig No. 11 (Group 1) was panting with rapid respiration on Day 15. Otherwise, all pigs were normal for behavior, respiration and cough during this observation period and no systemic adverse events were noted with any groups. No injection site reactions were noted following vaccination on Day 0. Following vaccination on Day 14, seven (7) out of fourteen (14) Group 1 pigs (50.0%) had swelling with a score of “2” on Day 15. Four (4) out of fourteen (14) Group 1 (28.6%) still had a swelling of “2” on Day 16. None of the other groups experienced injection site reactions following either vaccination.
[0164] Average daily weight gain (ADWG) results are presented below in Table 18. Pigs No. 46 and 98 that died from bleeding were excluded from group results. Group 4, which received one dose of 16 ug vORF2-Carbopol, had the highest ADWG (1.16±0.26 lbs/day), followed by Groups 1, 2, 3, 5, 6, and 10 which had ADWGs that ranged from 1.07±0.23 lbs/day to 1.11±0.26 lbs/day. Group 9 had the lowest ADWG (0.88±0.29 lbs/day), followed by Groups 8 and 7, which had ADWGs of 0.93±0.33 lbs/day and 0.99±0.44 lbs/day, respectively.
[0000]
TABLE 18
Summary of Group Average Daily Weight Gains (ADWG)
ADWG - lbs/day
(Day 25 to Day 50) or adjusted for pigs
Group
Treatment
N
dead before Day 50
1
rORF2 - 16 μg - IMS 1314 2 doses
14
1.08 ± 0.30 lbs/day
2
vORF2 - 16 μg - Carbopol 2 doses
15
1.11 ± 0.16 lbs/day
3
rORF2 - 16 μg - Carbopol 2 doses
15
1.07 ± 0.21 lbs/day
4
vORF2 - 16 μg - Carbopol 1 dose
15
1.16 ± 0.26 lbs/day
5
rORF2 - 4 μg - Carbopol 1 dose
15
1.07 ± 0.26 lbs/day
6
rORF2 - 1 μg - Carbopol 2 doses
15
1.11 ± 0.26 lbs/day
7
rORF2 - 0.25 μg - Carbopol 2 doses
15
0.99 ± 0.44 lbs/day
8
KV > 8.0 log - Carbopol 2 doses
15
0.93 ± 0.33 lbs/day
9
Challenge Controls
14
0.88 ± 0.29 lbs/day
10
Strict Negative Controls
15
1.07 ± 0.23 lbs/day
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
KV or killed whole cell virus = PCV2 virus grown in suitable cell culture
[0165] PVC2 serology results are presented below in Table 19. All ten (10) groups were seronegative for PCV2 on Day −3. On Day 14, PCV2 titers remained low for all ten (10) groups (range of 50-113). On Day 25, Group 8, which received the whole cell killed virus vaccine, had the highest PCV2 titer (4617), followed by Group 2, which received 16 ug vORF2—Carbopol, Group 4, which received as single dose of 16 ug vORF2—Carbopol, and Group 3, which received 16 ug rORF2-Carbopol, which had titers of 2507, 1920 and 1503 respectively. On Day 32 (one week post challenge), titers for Groups 1-6 and Group 8 ranged from 2360 to 7619; while Groups 7 (0.25 ug rORF2—Carbopol), 9 (Challenge Control), and 10 (Strict negative control) had titers of 382, 129 and 78 respectively. On Day 50 (day of necropsy), all ten (10) groups demonstrated high PCV2 titers (≧1257).
[0166] On Days 25, 32, and 50, Group 3, which received two doses of 16 ug rORF2—Carbopol had higher antibody titers than Group 1, which received two doses of 16 ug rORF2—IMS 1314. On Days 25, 32 and 50, Group 2, which received two doses of 16 ug vORF2 had higher titers than Group 4, which received only one does of the same vaccine. Groups 3, 5, 6, 7, which received decreasing levels of rORF2—Carbopol, of 16, 4, 1, and 0.25 ug respectively, demonstrated correspondingly decreasing antibody titers on Days 25 and 32.
[0000]
TABLE 19
Summary of Group PCV2 IFA Titers
Day
Group
Treatment
Day −3
Day 14**
Day 25***
Day 32
50****
1
rORF2 - 16 μg -
50
64
646
3326
4314
IMS 1314 2 doses
2
vORF2 - 16 μg -
50
110
2507
5627
4005
Carbopol 2 doses
3
rORF2 - 16 μg -
50
80
1503
5120
6720
Carbopol 2 doses
4
vORF2 - 16 μg -
50
113
1920
3720
1257
Carbopol 1 dose
5
rORF2 - 4 μg -
50
61
1867
3933
4533
Carbopol 1 dose
6
rORF2 - 1 μg -
50
70
490
2360
5740
Carbopol 2 doses
7
rORF2 - 0.25 μg -
50
73
63
382
5819
Carbopol 2 doses
8
KV > 8.0 log - Carbopol
50
97
4617
7619
10817
2 doses
9
Challenge Controls
50
53
50
129
4288
10
Strict Negative Controls
50
50
50
78
11205
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
KV or killed whole cell virus = PCV2 virus grown in suitable cell culture
*For calculation purposes, a ≦ 100 IFA titer was designated as a titer of “50”; a ≧ 6400 IFA titer was designated as a titer of “12,800”.
**Day of Challenge
***Day of Necropsy
[0167] The results from the post-challenge clinical observations are presented below. Table 20 includes observations for Abnormal Behavior, Abnormal Respiration, Cough and Diarrhea. Table 21 includes the results from the Summary of Group Overall Incidence of Clinical Symptoms and Table 22 includes results from the Summary of Group Mortality Rates Post-challenge. The incidence of abnormal behavior, respiration and cough post-challenge were low in pigs receiving 16 ug rORF2-IMS 1314 (Group 1), 16 ug rORF2-Carbopol (Group 3), 1 ug rORF2-Carbopol (Group 6), 0.25 ug rORF2-Carbopol (Group 7), and in pigs in the Challenge Control Group (Group 9). The incidence of abnormal behavior respiration and cough post-challenge was zero in pigs receiving 16 ug vORF2-Carbopol (Group 2), a single dose of 16 ug vORF2-Carbopol (Group 4), 4 ug rORF2-Carbopol (Group 5), >8 log KV-Carbopol (Group 8), and in pigs in the strict negative control group (Group 10).
[0168] The overall incidence of clinical symptoms varied between groups. Pigs receiving 16 ug vORF2-Carbopol (Group 2), a single dose of 16 ug vORF2-Carbopol (Group 4), and pigs in the Strict negative control group (Group 10) had incidence rates of 0%; pigs receiving 16 ug rORF2-Carbopol (Group 3), and 1 ug rORF2-Carbopol (Group 6) had incidence rates of 6.7%; pigs receiving 16 ug rORF2-IMS 1314 (Group 1) had an overall incidence rate of 7.1%; pigs receiving 4 ug rORF2-Carbopol (Group 5), 0.25 ug rORF2-Carbopol (Group 7), and >8 log KV vaccine had incidence rates of 13.3%; and pigs in the Challenge Control Group (Group 9) had an incidence rate of 14.3%.
[0169] Overall mortality rates between groups varied as well. Group 8, which received 2 doses of KV vaccine had the highest mortality rate of 20.0%; followed by Group 9, the challenge control group, and Group 7, which received 0.25 ug rORF2-Carbopol and had mortality rates of 14.3% and 13.3% respectively. Group 4, which received one dose of 16 ug vORF2-Carbopol had a 6.7% mortality rate. All of the other Groups, 1, 2, 3, 5, 6, and 10 had a 0% mortality rate.
[0000]
TABLE 20
Summary of Group Observations for Abnormal Behavior, Abnormal
Respiration, and Cough Post-Challenge
Abnormal
Abnormal
Group
Treatment
N
Behavior 1
Behavior 2
Cough 3
1
rORF2 - 16 μg -
14
0/14
0/14
1/14
IMS 1314 2 doses
(0%)
(0%)
(7.1%)
2
vORF2 - 16 μg -
15
0/15
0/15
0/15
Carbopol 2 doses
(0%)
(0%)
(0%)
3
rORF2 - 16 μg -
15
0/15
0/15
1/15
Carbopol 2 doses
(0%)
(0%)
(6.7%)
4
vORF2 - 16 μg -
15
0/15
0/15
0/15
Carbopol 1 dose
(0%)
(0%)
(0%)
5
rORF2 - 4 μg -
15
1/15
1/15
0/15
Carbopol 1 dose
(6.7%)
(6.7%)
(0%)
6
rORF2 - 1 μg -
15
0/15
0/15
1/15
Carbopol 2 doses
(0%)
(0%)
(6.7%)
7
rORF2 - 0.25 μg -
15
0/15
1/15
1/15
Carbopol 2 doses
(0%)
(6.7%)
(06.7%)
8
KV > 8.0 log -
15
1/15
1/15
0/15
Carbopol 2 doses
(6.7%)
(6.7%)
(0%)
9
Challenge Controls
14
1/14
1/14
2/14
(7.1%)
(7.1%)
(14/3%)
10
Strict Negative Controls
15
0/15
0/15
0/15
(0%)
(0%)
(0%)
1 Total number of pigs in each group that demonstrated any abnormal behavior for at least one day
2 Total number of pigs in each group that demonstrated any abnormal respiration for at least one day
3 Total number of pigs in each group that demonstrated a cough for at least one day
[0000]
TABLE 21
Summary of Group Overall Incidence of Clinical Symptoms Post-
Challenge
Incidence of
pigs with
Clinical
Incidence
Group
Treatment
N
Symptoms 1
Rate
1
rORF2 - 16 μg -
14
1
7.1%
IMS 1314 2 doses
2
vORF2 - 16 μg - Carbopol 2
15
0
0.0%
doses
3
rORF2 - 16 μg - Carbopol 2
15
1
6.7%
doses
4
vORF2 - 16 μg - Carbopol 1
15
0
0.0%
dose
5
rORF2 - 4 μg -
15
2
13.3%
Carbopol 1 dose
6
rORF2 - 1 μg -
15
1
6.7%
Carbopol 2 doses
7
rORF2 - 0.25 μg - Carbopol
15
2
13.3%
2 doses
8
KV > 8.0 log - Carbopol 2
15
2
13.3%
doses
9
Challenge Controls
14
2
14.3%
10
Strict Negative Controls
15
0
0.0%
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
KV or killed whole cell virus = PCV2 virus grown in suitable cell culture
1 Total number of pigs in each group that demonstrated any clinical symptom for at least one day
[0000]
TABLE 22
Summary of Group Mortality Rates Post-Challenge
Dead Post-
Mortality
Group
Treatment
N
challenge
Rate
1
rORF2 - 16 μg -
14
0
0.0%
IMS 1314 2 doses
2
vORF2 - 16 μg - Carbopol 2
15
0
0.0%
doses
3
rORF2 - 16 μg - Carbopol 2
15
0
0.0%
doses
4
vORF2 - 16 μg - Carbopol 1
15
1
6.7%
dose
5
rORF2 - 4 μg -
15
0
0.0%
Carbopol 1 dose
6
rORF2 - 1 μg -
15
0
0.0%
Carbopol 2 doses
7
rORF2 - 0.25 μg - Carbopol 2
15
2
13.3%
doses
8
KV > 8.0 log - Carbopol 2
15
3
20.0%
doses
9
Challenge Controls
14
2
14.3%
10
Strict Negative Controls
15
0
0.0%
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
KV or killed whole cell virus = PCV2 virus grown in suitable cell culture
[0170] The Summary of Group Mean Percentage Lung Lesions and Tentative Diagnosis is given below in Table 23. Group 9, the challenge control group, had the highest percentage lung lesions with a mean of 10.81±23.27%, followed by Group 7, which received 0.25 ug rORF2-Carbopol and had a mean of 6.57±24.74%, Group 5, which received 4 ug rORF2-Carbopol and had a mean of 2.88±8.88%, and Group 8, which received the KV vaccine and had a mean of 2.01±4.98%. The remaining six (6) groups had lower mean percentage lung lesions that ranged from 0.11±0.38% to 0.90±0.15%.
[0171] Tentative diagnosis of pneumonia varied among the groups. Group 3, which received two doses of 16 ug rORF2-Carbopol, had the lowest tentative diagnosis of pneumonia, with 13.3%. Group 9, the challenge control group, had 50% of the group tentatively diagnosed with pneumonia, followed by Group 10, the strict negative control group and Group 2, which received two doses of 16 ug vORF2-Carbopol, with 46.7% of 40% respectively, tentatively diagnosed with pneumonia.
[0172] Groups 1, 2, 3, 5, 9, and 10 had 0% of the group tentatively diagnosed as PCV2 infected; while Group 8, which received two doses if KV vaccine, had the highest group rate of tentative diagnosis of PCV2 infection, which 20%. Group 7, which received two doses of 0.25 ug rORF2-Carbopol, and Group 4, which received one dose of 16 ug vORF2-Carbopol had tentative group diagnoses of PCV2 infection in 13.3% and 6.7% of each group, respectively.
[0173] Gastric ulcers were only diagnosed in one pig in Group 7 (6.7%); while the other 9 groups remained free of gastric ulcers.
[0000]
TABLE 23
Summary of Group Mean % Lung Lesion and Tentative Diagnosis
No. Of pigs that
shed for at
Incidence
Group
Treatment
N
least one day
Rate
1
rORF2 - 16 μg -
15
0
0%
IMS 1314 2 doses
2
vORF2 - 16 μg -
15
1
6.7%
Carbopol 2 doses
3
rORF2 - 16 μg -
15
3
20.0%
Carbopol 2 doses
4
vORF2 - 16 μg -
15
2
13.3%
Carbopol 1 dose
5
rORF2 - 4 μg -
15
3
20.0%
Carbopol 1 dose
6
rORF2 - 1 μg -
15
6
40.0%
Carbopol 2 doses
7
rORF2 - 0.25 μg -
15
7
46.7%
Carbopol 2 doses
8
KV > 8.0 log - Carbopol
15
12
80%
2 doses
9
Challenge Controls
14
14
100.0%
10
Strict Negative Controls
15
14
93.3%
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
KV or killed whole cell virus = PCV2 virus grown in suitable cell culture
[0174] The Summary of Group IHC Positive Incidence Results are shown below in Table 24. Group 1 (16 ug rORF2—IMS 1314) had the lowest group rate of IHC positive results with 0% of the pigs positive for PCV2, followed by Group 2 (16 ug vORF2—Carbopol) and Group 4 (single dose 16 ug vORF2—Carbopol), which had group IHC rates of 6.7% and 13.3% respectively. Group 9, the challenge control group, had the highest IHC positive incidence rate with 100% of the pigs positive for PCV2, followed by Group 10, the strict negative control group, and Group 8 (KV vaccine), with 93.3% and 80% of the pigs positive for PCV2, respectively.
[0000]
TABLE 24
Summary of Group IHC Positive Incidence Rate
No. Of pigs
that shed for
Incidence
Group
Treatment
N
at least one day
Rate
1
rORF2 - 16 μg -
15
0
0%
IMS 1314 2 doses
2
vORF2 - 16 μg -
15
1
6.7%
Carbopol 2 doses
3
rORF2 - 16 μg -
15
3
20.0%
Carbopol 2 doses
4
vORF2 - 16 μg -
15
2
13.3%
Carbopol 1 dose
5
rORF2 - 4 μg -
15
3
20.0%
Carbopol 1 dose
6
rORF2 - 1 μg -
15
6
40.0%
Carbopol 2 doses
7
rORF2 - 0.25 μg -
15
7
46.7%
Carbopol 2 doses
8
KV > 8.0 log - Carbopol
15
12
80%
2 doses
9
Challenge Controls
14
14
100.0%
10
Strict Negative Controls
15
14
93.3%
vORF2 = isolated viral ORF2;
rORF2 = recombinant baculovirus expressed ORF2;
KV or killed whole cell virus = PCV2 virus grown in suitable cell culture
Discussion
[0175] Seven PCV2 vaccines were evaluated in this example, which included a high dose (16 μg) of rORF2 antigen adjuvanted with IMS 1314 administered twice, a high dose (16 μg) of vORF2 antigen adjuvanted with Carbopol administered once to one group of pigs and twice to a second group of pigs, a high dose (16 μg) of rORF2 antigen adjuvanted with Carbopol administered twice, a 4 μg dose of rORF2 antigen adjuvanted with Carbopol administered twice, a 1 μg dose of rORF2 antigen adjuvanted with Carbopol administered twice, a low dose (0.25 μg) of rORF2 antigen adjuvanted with Carbopol administered twice, and a high dose (>8 log) of killed whole cell PCV2 vaccine adjuvanted with Carbopol. Overall, Group 1, which received two doses of 16 μg rORF2—IMS 1314, performed slightly better than Groups 2 through 7, which received vaccines containing various levels of either vORF2 or rORF2 antigen adjuvanted with Carbopol and much better than Group 8, which received two doses of killed whole cell PCV2 vaccine. Group 1 had the third highest ADWG (1.80±0.30 lbs/day), the lowest incidence of abnormal behavior (0%), the lowest incidence of abnormal respiration (0%), a low incidence of cough (7.1%), a low incidence of overall clinical symptoms (7.1%), was tied with three other groups for the lowest mortality rate (0%), the second lowest rate for mean % lung lesions (0.15±0.34%), the second lowest rate for pneumonia (21.4%) and the lowest incidence rate for positive IHC tissues (0%). Group 1 was, however, the only group in which injection site reactions were noted, which included 50% of the vaccinates 1 day after the second vaccination. The other vaccines administered to Groups 2 through 7 performed better than the killed vaccine and nearly as well as the vaccine administered to Group 1.
[0176] Group 8, which received two doses of killed PCV2 vaccine adjuvanted with Carbopol, had the worst set of results for any vaccine group. Group 8 had the lowest ADWG (0.93±0.33 lbs/day), the second highest rate of abnormal behavior (6.7%), the highest rate of abnormal respiration (6.7%), was tied with three other groups for the highest overall incidence rate of clinical symptoms (13.3%), had the highest mortality rate of all groups (20%), and had the highest positive IHC rate (80%) of any vaccine group. There was concern that the killed whole cell PCV2 vaccine may not have been fully inactivated prior to administration to Group 8, which may explain this group's poor results. Unfortunately, definitive data was not available to confirm this concern. Overall, in the context of this example, a Conventional Killed PCV2 vaccine did not aid in the reduction of PCV2 associated disease.
[0177] As previously mentioned, no adverse events were associated with the test vaccines with exception of the vaccine adjuvanted with IMS 1314. Injection site reactions were noted in 50.0% of the pigs 1 day after the second vaccination with the vaccine formulated with IMS 1314 and in 28.6% of the pigs 2 days after the second vaccination. No reactions were noted in any pigs receiving Carbopol adjuvanted vaccines. Any further studies that include pigs vaccinated with IMS 1314 adjuvanted vaccines should continue to closely monitor pigs for injection site reactions.
[0178] All pigs were sero-negative for PCV2 on Day −3 and only Group 2 had a titer above 100 on Day 14. On Day 25 (day of challenge), Group 8 had the highest PCV2 antibody titer (4619), followed by Group 2 (2507). With the exception of Groups 7, 9 and 10, all groups demonstrated a strong antibody response by Day 32. By Day 50, all groups including Groups 7, 9 and 10 demonstrated a strong antibody response.
[0179] One of the hallmarks of late stage PCV2 infection and subsequent PMWS development is growth retardation in weaned pigs, and in severe cases, weight loss is noted. Average daily weight gain of groups is a quantitative method of demonstrating growth retardation or weight loss. In this example, there was not a large difference in ADWG between groups. Group 8 had the lowest ADWG of 0.88±0.29 lbs/day, while Group 4 had the highest ADWG of 1.16±0.26 lb/day. Within the context of this study there was not a sufficient difference between groups to base future vaccine efficacy on ADWG.
[0180] In addition to weight loss—dyspnea, lethargy, pallor of the skin and sometimes icterus are clinical symptoms associated with PMWS. In this example, abnormal behavior and abnormal respiration and cough were noted infrequently for each group. As evidenced in this study, this challenge model and challenge strain do not result in overwhelming clinical symptoms and this is not a strong parameter on which to base vaccine efficacy.
[0181] Overall, mortality rates were not high in this example and the lack of a high mortality rate in the challenge control group limits this parameter on which to base vaccine efficacy. Prior to Day 46, Groups 4 and 7 each had one out of fifteen pigs die, Group 9 had two out of fourteen pigs die and Group 8 had three out of fifteen pigs die. Due to the fact that Group 9, the challenge control group was not demonstrating PCV2 clinical symptoms and only two deaths had occurred in this group by Day 46, Porcine Respiratory and Reproductive Syndrome Virus (PRRSV) MLV vaccine was administered to all pigs on Day 46. Earlier studies had utilized INGELVAC® PRRS MLV as an immunostimulant to exasperate PCV2-associated PMWS disease and mortality rates were higher in these earlier studies. Two deaths occurred shortly after administering the PRRS vaccine on Day 46—Group 4 had one death on Day 46 and Group 7 had one death on Day 47—which were probably not associated with the administration of the PRRS vaccine. By Day 50, Group 8, which received two doses of killed vaccine, had the highest mortality rate (20%), followed by Group 9 (challenge control) and Group 7 (0.25 ug rORF2—Carbopol), with mortality rates of 14.3% and 13.3% respectively. Overall, administration of the PRRS vaccine to the challenge model late in the post-challenge observation phase of this example did not significantly increase mortality rates.
[0182] Gross lesions in pigs with PMWS secondary to PCV2 infection typically consist of generalized lymphadenopathy in combination with one or more of the following: (1) interstitial pneumonia with interlobular edema, (2) cutaneous pallor or icterus, (3) mottled atrophic livers, (4) gastric ulcers and (5) nephritis. At necropsy (Day 50), icterus, hepatitis, and nephritis were not noted in any groups. A gastric ulcer was noted in one Group 7 pig, but lymphadenopathy was not specifically examined for. Based on the presence of lesions that were consistent with PCV2 infection, three groups had at least one pig tentatively diagnosed with PCV2 (PMWS). Group 8, which received two doses of killed vaccine, had 20% tentatively diagnosed with PCV2, while Group 7 and Group 4 had 13.3% and 6.7%, respectively, tentatively diagnosed with PCV2. The mean % lung lesion scores varied between groups at necropsy. Groups 1, 2, 3, 4, 6 and 10 had low % lung lesion scores that ranged from 0.11±0.38% to 0.90±0.15%. As expected, Group 9, the challenge control group, had the highest mean % lung lesion score (10.81±23.27%). In four groups, the mean % lung lesion scores were elevated due to one to three pigs in each of these groups having very high lung lesion scores. The lung lesions were red/purple and consolidated. Typically, lung lesions associated with PMWS are described as tan, non-collapsible with interlobular edema. The lung lesions noted in this study were either not associated with PCV2 infection or a second pulmonary infectious agent may have been present. Within the context of this study, the % lung lesion scores probably do no reflect a true measure of the amount of lung infection due to PCV2. Likewise, tentative diagnosis of pneumonia may have been over-utilized as well. Any pigs with lung lesions, some as small as 0.10% were listed with a tentative diagnosis of pneumonia. In this example, there was no sufficient difference between groups with respect to gross lesions and % lung lesions on which to base vaccine efficacy.
[0183] IHC results showed the largest differences between groups. Group 1 (16 μg rORF2—IMS 1314) had the lowest positive IHC results for PCV2 antigen (0%); while Groups 9 and 10 had the highest positive IHC results with incidence rates of 100% and 93.3% respectively. Groups 3, 5, 6 and 7, which received 16, 4, 1 or 0.25 μg of rORF2 antigen, respectively, adjuvanted with Carbopol, had IHC positive rates of 20%, 20%, 40% and 46.7%, respectively. Group 2, which received two doses of 16 μg vORF2 adjuvanted with Carbopol had an IHC positive rate of 6.7%, while Group 4 which received only one dose of the same vaccine, had an IHC positive rate of 13.3%. Due to the objective nature of this test and the fact that IHC results correlated with expected results, IHC testing is probably one of the best parameters on which to base vaccine efficacy.
[0184] Thus in one aspect of the present invention, the Minimum Protective Dosage (MPD) of PCV2 rORF2 antigen adjuvanted with Carbopol in the CDCD pig model in the face of a PCV2 challenge is determined. Groups 3, 5, 6 and 7 each received two doses of rORF2 antigen adjuvanted with Carbopol, but the level of rORF2 antigen varied for each group. Groups 3, 5, 6 and 7 each received 16, 4, 1 or 0.25 μg of rORF2 antigen respectively. In general, decreasing the level of rORF2 antigen decreased PCV2 antibody titers, and increased the mortality rate, mean % lung lesions and the incidence of IHC positive tissues. Of the four groups receiving varying levels of rORF2-Carbopol, Groups 3 and 5, which received two doses of 16 or 4 μg of rORF2 antigen, respectively, each had an IHC positive rate of only 20%, and each had similar antibody titers. Overall, based on IHC positive results, the minimum protective dosage of rORF2 antigen administered twice is approximately 4 μg.
[0185] In another aspect of the present invention, the antigenicity of recombinant (rORF2) and VIDO R-1 (vORF2) PCV2 antigens were assessed. Group 2 received two doses of 16 μg vORF2 and Group 3 received two doses of 16 μg rORF2. Both vaccines were adjuvanted with Carbopol. Both vaccines were found to be safe and both had 0% mortality rate. Group 2 had a PCV2 antibody titer of 2507 on Day 25, while Group 3 had a PCV2 antibody titer of 1503. Group 3 had a lower mean % lung lesion score than Group 2 (0.11±0.38% vs. 0.90±0.15%), but Group 2 had a lower IHC positive incidence rate that Group 3 (6.7% vs. 20%). Overall, both vaccines had similar antigenicity, but vORF2 was associated with slightly better IHC results.
[0186] In yet another aspect of the present invention, the suitability of two different adjuvants (Carbopol and IMS 1314) was determined. Groups 1 and 3 both received two doses of vaccine containing 16 ug of rORF2 antigen, but Group 1 received the antigen adjuvanted with IMS 1314 while Group 3 received the antigen adjuvanted with Carbopol. Both groups had essentially the same ADWG, essentially the same incidence of clinical signs post-challenge, the same mortality rate, and essentially the same mean % lung lesions; but Group 1 had an IHC positive rate of 0% while Group 3 had an IHC positive rate of 20%. However, Group 3, which received the vaccine adjuvanted with Carbopol had higher IFAT PCV2 titers on Days 25, 32 and 50 than Group 1, which received the vaccine adjuvanted with IMS 1314. Overall, although the PCV2 vaccine adjuvanted with IMS 1314 did provide better IHC results, it did not provide overwhelmingly better protection from PCV2 infection and did induce injection site reaction. Whereas the PCV2 vaccine adjuvanted with Carbopol performed nearly as well as the IMS 1314 adjuvanted vaccine, but was not associated with any adverse events.
[0187] In still another aspect of the present invention, the feasibility of PCV2 ORF2 as a 1 ml, 1 dose product was determined. Groups 2 and 4 both received 16 μg of vORF2 vaccine adjuvanted with Carbopol on Day 0, but Group 2 received a second dose on Day 14. Group 4 had a slightly higher ADWG and a lower mean % lung lesions than Group 2, but Group 2 had higher IFAT PCV2 titers on Day 25, 32 and 50, and a slightly lower incidence rate of IHC positive tissues. All other results for these two groups were similar. Overall, one dose of vORF2 adjuvanted with Carbopol performed similar to two doses of the same vaccine. | An improved method for recovering the protein expressed by open reading frame 2 from porcine circovirus type 2 is provided. The method generally involves the steps of transfecting recombinant virus containing open reading frame 2 coding sequences into cells contained in growth media, causing the virus to express open reading frame 2, and recovering the expressed protein in the supernate. This recovery should take place beginning approximately 5 days after infection of the cells in order to permit sufficient quantities of recombinant protein to be expressed and secreted from the cell into the growth media. Such methods avoid costly and time-consuming extraction procedures required to separate and recover the recombinant protein from within the cells. | 0 |
CROSS REFERENCE
This application is a continuation-in-part of Ser. No. 08/648,857 filed May 16, 1996 which is a divisional application of Ser. No. 08/318, 042, filed Oct. 4, 1994, now U.S. Pat. No. 5,554,601; which is a continuation in part of 08/149,175 filed Nov. 5, 1993 now abandoned. This application is furthermore a continuation-in-part of Ser. No. 08/685,574 filed Nov. 14, 1997. These applications and patents are herein incorporated by reference.
TECHNICAL FIELD
The present invention relates to the protection of cells that would otherwise die as a result of an ischemic event.
BACKGROUND ART
Ischemia is an acute condition associated with an inadequate flow of oxygenated blood to a part of the body, caused by the constriction or blockage of the blood vessels supplying it. Ischemia occurs any time that blood flow to a tissue is reduced below a critical level. This reduction in blood flow can result from: (i) the blockage of a vessel by an embolus (blood clot); (ii) the blockage of a vessel due to atherosclerosis; (iii) the breakage of a blood vessel (a bleeding stroke); (iv) the blockage of a blood vessel due to vasoconstriction such as occurs during vasospasms and possibly, during transient ischemic attacks (TIA) and following subarachnoid hemorrhage. Conditions in which ischemia occurs, further include (i) during myocardial infarction (when the heart stops, the flow of blood to organs is reduced and ischemia results); (ii) trauma; and (iii) during cardiac and neurosurgery (blood flow needs to be reduced or stopped to achieve the aims of surgery).
When an ischemic event occurs, there is a gradation of injury that arises from the ischemic site. The cells at the site of blood flow restriction, undergo necrosis and form the core of a lesion. A penumbra is formed around the core where the injury is not as immediately fatal but slowly progresses to cell death. This progression to cell death may be reversed upon reestablishment of blood flow within a short time of the ischemic event.
Focal ischemia encompasses cerebrovascular disease (stroke), subarachnoid hemorrhage (SAH), and trauma. Stroke is the third leading cause of morbidity in the U.S., with over 500,000 cases per year, including 150,000 deaths annually. Post-stroke sequelae are mortality and debilitating chornic neurological complications which result from neuronal damage for which prevention or treatment are not currently available.
Following a stroke, the core area shows signs of cell death, but cells in the penumbra are still alive although malfunctioning and will, in several days, resemble the necrotic core. The neurons in the penumbra seem to malfunction in a graded manner with respect to regional blood flow. As the blood flow is depleted, neurons fall electrically silent, their ionic gradients decay, the cells depolarize, and then they die. Endothelial cells of the brain capillaries undergo swelling and the luminal diameter of the capillaries decrease. Associated with these events, the blood brain barrier appears to be disrupted, and an inflammatory response follows which further interrupts blood flow and the access of cells to oxygen.
The effects of a stroke on neurons result from the depletion of energy sources associated with oxygen deprivation which in turn disrupts the critically important ion pumps responsible for electrical signaling and neurotransmitter release. The failure of the ATP-dependant ion specific pumps to maintain ion gradients through active transport of sodium, chlorine, hydrogen, and calcium ions out of the cell and potassium ions into the cell results in a series of adverse biochemical events. For example, increase in intracellular calcium ion levels results in: (i) the production of free radicals that extensively damage lipids and proteins; (ii) the disruption of calcium sensitive receptors such as the N-methyl D-aspartate (NMDA) and the α-amino-3-hydroxy-5-methyl-4-isoxazoleproprionic acid (AMPA) synaptic glutamate receptors; (iii) the swelling of cells with water as a result of abnormal accumulation of ions; and (iv) the decrease in intracellular pH. The alteration in metabolism within the cell further results in the accumulation of ions in the cells as energy sources are depleted. For example, anaerobic glycolysis that forms lactic acid, replaces the normal aerobic glycolysis pathways in the mitochondria. This results in acidosis that results in further accumulation of calcium ions in the cell.
Despite the frequency of occurrence of ischemia (including stroke) and despite the serious nature of the outcome for the patient, treatments for these conditions have proven to be elusive. There are two basic approaches that have been undertaken to rescue degenerating cells in the penumbra. The first and most effective approach to date has been the identification of blood clot dissolvers that bring about rapid removal of the vascular blockage that restricts blood flow to the cells. Recombinant tissue plasminogen activator (TPA) has been approved by the Federal Drug Administration for use in dissolving clots that cause ischemia in thrombotic stroke. Nevertheless, adverse side effects are associated with the use of TPA. For example, a consequence of the breakdown of blood clots by TPA treatment is cerebral hemorrhaging that results from blood vessel damage caused by the ischemia. A second basic approach to treating degenerating cells deprived of oxygen is to protect the cells from damage that accumulates from the associated energy deficit. To this end, glutamate antagonists and calcium channel antagonists have been most thoroughly investigated. None of these have proven to be substantially efficacious but they are still in early clinical development. No treatment other than TPA is currently approved for stroke. The pathophysiology and treatment of focal cerebral ischemia has been reviewed by B. K. Seisjo 1992, J. Neurosurgery 77 169-184 and 337-354.
In addition to the targets of drug development described by Seisjo (1992), epidemiological studies have shown that women undergoing hormone replacement therapy with estrogen and progesterone experienced a reduction in the incidence and severity of heart disease. This correlation was further investigated for stroke with mixed results. A 10-year epidemiological study on 48,000 women reported by Stampfer et al. (New England Journal of Medicine 325, p. 756) concluded that there was a correlation between use of estrogen and decrease in incidence of coronary heart disease, but no decrease in the incidence of stroke was observed. In contrast, a report by Wren (The Medical Journal of Australia, 1992, vol. 157, p. 204) who reviewed 100 articles directed to the question as to whether estrogens reduce the risk of atherosclerosis and myocardial infarction, concluded that estrogens in hormone replacement therapies do significantly reduce the incidence of myocardial infarction and stroke and may accomplish this at the site of the blood vessel wall. This conclusion was further supported by Falkeborn et al. Arch Intern. Med. vol. 153, 1201 (1993). The above correlation between estrogen replacement therapy and reduced incidence of stroke relies on epidemiological data only. No biochemical data was analyzed to interpret or support these conclusions. Furthermore, these studies were restricted to the patients receiving long-term hormone replacement treatment. No studies were performed on patients who might be administered estrogen shortly before, during, or after a stroke for the first time. Furthermore, the studies were limited to estrogens utilized in estrogen replacement therapy. No studies were performed on any non-sex related estrogens that might be used in treating males.
Studies have been conducted on the neuroprotective effects of steroids in which glucocorticosteroid for example was found to have a positive effect in reducing spinal chord injury but had a negative effect on hippocampal neurodegeneration. For example, Hall (J. Neurosurg vol. 76, 13-22 (1992) noted that the glucocorticoid steroid, methylprednisolone, believed to involve the inhibition of oxygen free radical-induced lipid peroxidation, could improve the 6-month recovery of patients with spinal cord injury when administered in an intensive 24-hour intravenous regimen beginning within 8 hours after injury. However, when the steroid was examined for selective protection of neuronal necrosis of hippocampal neurons, it was found that the hippocampal neuronal loss was significantly worsened by glucocorticoid steroid dosing suggesting that this hormone is unsuitable for treating acute cerebral ischemia. Hall reported that substitution of a complex amine on the non-glucocorticoid steroid in place of the 21 hydroxyl functionality results in an enhancement of lipid anti-oxidant activity. No data was provided concerning the behavior of this molecule in treating ischemic events or in neuroprotection of neurons in the brain. Additionally, free radical scavenging activity has been reported for a lazaroid, another non-glucocorticoid steroid having a substituted 21 hydroxyl functionality, but there is until now no evidence that this compound is significantly efficacious for treating stroke or other forms of ischemia.
There is a need for effective treatments for stroke and other forms of ischemia that may safely be administered preventatively to men and women who are susceptible to such conditions, and may further be used after the ischemia has occurred so as to protect cells from progressive degeneration that is initiated by the ischemic event.
SUMMARY OF THE INVENTION
The invention satisfies the above need. Novel methods are provided for prevention and treatment of ischemic damage using estrogen compounds.
A preferred embodiment of the invention provides a method for conferring protection on a population of cells associated with an ischemic focus, in a subject following an ischemic event that includes the steps of providing an estrogen compound; and administering an effective cumulative amount of the compound over a course that includes at least one dose, within a time that is effectively proximate to the ischemic event, so as to confer protection on the population of cells. Further embodiments include selecting a proximate time for administering the effective dose of estrogen that is prior to the ischemic event. Alternatively, estrogen may be administered within an effective proximate time after the ischemic event. The method of the invention may be applied to any of a cerebrovascular disease, subarachnoid hemorrhage, myocardial infarct, surgery, and trauma. In particular, when the ischemic event is a stroke, the protected cells include at least one of neurons and endothelial cells.
The method includes administering the estrogen by means of oral, buccal, rectal, intramuscular, transdermal, intravenous, or subcutaneous delivery routes and further may include a sustained controlled release vehicle exemplified by an estrogen-chemical delivery system or a silastic pellet.
The method utilizes an estrogen compound which includes alpha isomers and beta isomers of estrogen compounds. Examples of different isomers are provided wherein the estrogen compound is selected from the group consisting of 17α-estradiol and 17β-estradiol.
In a preferred embodiment of the invention, a method is provided for protecting cells in a subject from degeneration during or after an ischemic event. The steps of the method include identifying a susceptible subject, providing an effective dose of a non-sex related estrogen compound prior to the ischemic event, and protecting cells from degeneration otherwise occurring in the absence of the estrogen compound.
In a further embodiment of the invention, a method is provided for treating stroke in a subject, including the steps of providing an effective dose of an estrogen compound in a pharmaceutical and administering the formulation to the subject so as to reduce the adverse effects of the stroke.
LIST OF FIGURES
These and other features, aspects, and advantages of the present invention will be better understood with reference to the following description, appended claims, and accompanying drawings, where:
FIG. 1. shows the effects of pretreatment of ovariectomized rats, with 17β-estradiol, initiated 24 hours prior to ischemia induced by middle cerebral artery occlusion (MCAO); where the 17β-estradiol is administered as a subcutaneous 5 mm silastic implant (E2) or an Estradiol-Chemical Delivery System (E2-CDS) (1 mg/kg body weight) and a control is provided (a sham pellet). Values are given as the mean±SEM for the percent area ischemic area in 3 brain slices. *=p<0.05 vs. sham group. The total number of survivors of each treatment over 24 hours and 7 days were summed. Number of samples for sham=6, for 17β-estradiol=8, and for E2-CDS groups=10.
FIG. 2. shows the effects of treatment of ovariectomized (OVX) rats with 17β-estradiol, at 2 hours prior to ischemia induced by MCAO, where the 17β-estradiol (100 μg/kg E 2 ) is injected subcutaneously in an oil vehicle. A control is included which consists of the oil vehicle without estrogen. Rats were decapitated 24 hours after the MCAO. Rat brains were dissected coronally as region A-E, 24 hours after MCAO. Values were given as the mean±SEM where n=8 for OVX+E 2 group and n=6 for OVX group(control). * p<0.05 vs. corresponding vehicle control groups.
FIG. 3 shows the effects of pretreatment of ovariectomized rats with 17α-estradiol, initiated 24 hours prior to ischemia induced by MCAO, where the 17α-estradiol is administered in a 5 mm silastic tube, and the negative control is a 5 mm silastic tube without estrogen (sham). Rats were decapitated 24 hours after the MCAO. Values are given as the mean±SEM for the percent ischemic area in 5 brain slices. A to E designate the distance caudal to the olfactory bulb A=5 mm, B=7 mm, C=9 mm, D=11 mm, and E=13 mm. *=p<0.05 vs. sham group for the equivalent brain slice; for sham n=10 and for 17α-estradiol groups, n=13.
FIG. 4 shows the effects of posttreatrnent of ovariectomized rats with 17β-estradiol or a control (HPCD) at 40 minutes (a) and 90 minutes (b) post onset of MCAO. The 17β-estradiol was formulated in an estradiol-chemical delivery system at a concentration 1 mg/kg body weight (E2-CDS) and injected intravenously. Rats were decapitated 24 hours after the MCAO. Values are given as the mean±SEM for the percent ischemic area in 5 brain slices. A to E designate the distance caudal to the olfactory bulb A=5 mm, B=7 mm, C=9 mm, D =11 mm and E =13 mm. Where *=p<0.05 vs HPCD group for the same brain slice, N=9 for vehicle, and 13 for E2-CDS groups.
FIG. 5 shows the effects of 17β-estradiol (2 nM) on brain capillary endothelial cell (BCEC) mortality following 24 hours of hypoglycemia. The control consists of the ethanol vehicle only. The glucose concentrations in the cell media were adjusted from 20 mg % to 200 mg % by adding appropriate amount of D-(+)-glucose to the glucose-free media. BCEC were incubated for 24 hours (a) and 48 hours (b). Trypan blue staining was used to distinguish live cells from dead cells. Two cell countings at two different hemacytometer squares were averaged. Mean±SEM are depicted (n=8-12). *p<0.05 vs. corresponding vehicle control.
FIG. 6 shows the effects of 17β-estradiol (2 nm) on BCEC mortality following anoxia. The control consists of the ethanol vehicle without estrogen. Cell media contained 200 mg % glucose. Culture dishes containing BCEC were placed in nitrogen filled chamber for 4 hours. Trypan blue staining was used to distinguish live cells from dead cells. Two cell countings at two different hemacytometer squares were averaged. Mean±SEM are depicted (n=8-12). *p<0.05 vs. corresponding vehicle control.
FIG. 7 shows the effects of 17β-estradiol (2 nm) on BCEC mortality compared with a control (ethanol vehicle) following combination of anoxia and hypoglycemia. Cell media contained 100 mg % or 200 mg % glucose. Culture dishes containing BCEC were placed in either incubator or nitrogen filled chamber for two hours. Trypan blue staining was used to distinguish live cells from dead cells. Two cell countings at two different hemacytometer squares were averaged. Mean±SEM are depicted (n=8.12). *<0.05 vs. corresponding vehicle control.
DETAILED DESCRIPTION OF THE INVENTION
The invention provides an effective treatment for stroke and other forms of ischemia that may safely be administered to men and women so as to protect cells from progressive degeneration that is initiated by the ischemic event.
Estrogen compounds are defined here and in the claims as any of the structures described in the 11th edition of "Steroids" from Steraloid Inc., Wilton, N. H., here incorporated by reference. Included in this definition are non-steroidal estrogens described in the aforementioned reference. Other estrogens included in this definition are estrogen derivatives, isomers, estrogen metabolites, estrogen precursors, and modifications of the foregoing as well as molecules capable of binding cell associated estrogen receptor as well as other molecules where the result of binding triggers a characteristic estrogen effect. Also included are mixtures of more then one estrogen.
β-estrogen and α-estrogen are isomers of estrogen. The term "estradiol" refers to either 17α- or 17β-estradiol unless specifically identified.
The term "E2" is synonymous with β-estradiol ,17β-estradiol, E 2 , and β-E 2 .
An "animal subject" is defined here and in the claims as a higher organism including humans.
The term "non-sex hormone" is defined here and in the claims as a hormone having substantially no sex-related effect on the subject.
Estrogen compounds are here shown to protect cells from degeneration in the penumbra of the ischemic lesion. (Examples 1 and 2) Estrogen compounds are further shown to be protective of a plurality of cell types, including neuronal cells and endothelial cells (Examples 1-3). According to the invention, estrogen compounds may be used to protect cells from the effects of oxygen deprivation and glucose deprivation and consequently from energy deprivation associated with ischemia.
In an embodiment of the invention, a method of treatment is provided that is suitable for human male and female subjects and involves administering an effective dose of estrogen either before or after a stroke has occurred.
In certain circumstances according to the invention, it is desirable to administer estrogen prior to a predicted ischemic event. Such circumstances arise when, for example, a subject has already experienced a stroke. In this case, the subject will have an increased probability of experiencing a second stroke. Subjects who are susceptible to transient ischemic attacks also have an increased risk of a stroke. Subjects who suffer a subarachnoid hemorrhage may experience further ischemic events induced by vasospasms that constrict the blood vessels. Subjects who experience trauma to organs such as the brain are also susceptible to an ischemic event. The above situations exemplify circumstances when a subject would benefit from pretreatment with an estrogen compound. Such pretreatment may be beneficial in reducing the adverse effects of a future ischemic event when administered in the short term, such as within 24 hours before the event, (Example 1) or in the long term, where administration begins immediately after an event such as a stroke and continues prophylactically for an extended period of time. An example of time of administration for prophylactic use may extend from days to months depending of the particular susceptibility profile of the individual. In these circumstances, a course of at least one dose of estrogen may be administered over time so that an effective dose is maintained in the subject. For short term treatments, parenteral administration may be used as an alternative to the delivery of a dose by any of the routes specified below. The effective dose of estrogen compound for prophylactic use should provide a plasma concentration of 10-1000 pg/ml of estrogen compound. More particularly, the plasma concentration of the administered estrogen compound may be 50-500 pg/ml. In these circumstances, the use of non-sex estrogen compounds such as the α-isomers are of particular utility in men and women because the sex-related functions of the hormone are avoided.
According to embodiments of the invention, estrogen compounds are effective in reducing the adverse effects of an ischemic event such as cerebrovascular disease, subarachnoid hemorrhage, or trauma. Accordingly, the compound is administered as soon as possible after initiation of the event and preferably within 10 hours, more particularly, within 5 hours following the event. It is desirable that an increased concentration of estrogen compound be maintained in the plasma for at least several hours to several days following the ischemic event. The increased concentration of estrogen compound should be in the range of 10-1000 pg/ml of estrogen compound in the plasma. More particularly, the plasma concentration of the administered estrogen compound may be 50-500 pg/ml.
The present invention demonstrates for the first time that pretreatment with estrogens or early posttreatment of an estrogen compound can significantly reduce the size of the necrotic area following an ischemic event. This effect of estrogen pretreatment is independent of the isomeric form and the route of administration of the estrogen compound. α-isomers of estrogen have been shown to be as effective as β-isomers of estrogen in protecting cells from the effects of ischemia. The method as exemplified in Example 1 and FIGS. 1 and 2 confirm that the protective activity of estrogen compounds is not dependant on the sex-related activity of the hormone (estrogenicity). Alpha isomers of estrogen compounds appear to have substantially no sex-related activity, yet these compounds are as effective at protecting the brain against ischemic damage as the β isomers. Furthermore, Example 1 further demonstrates that the observed reduction in mortality of ovariectomized rats when treated with 17β-estradiol is not dependant on the route of administration, since the protective effect was similar when the same estrogen compound was administered as a subcutaneous implant or as an intravenous injection of E2-CDS. Regardless of the route of administration or the formulation of the estrogen compound, the estrogen has a remarkable effect on the ability of animals to survive an ischemic event.
The demonstration that estrogen is efficacious in protection of cells in an ischemic area is demonstrated in the examples below using rat animal models in which the middle cerebral artery (MCA) is experimentally occluded. This animal model is well known in the art to recapitulate an in vivo ischemic event such as may occur in a human subject. The experimental occlusion of the MCA causes a unilateral large ischemic area that typically involves the basal ganglion and frontal, parietal, and temporal cortical areas (Menzies et al. Neurosurgery 31, 100-106 (1992)). The ischemic lesion begins with a smaller core at the site perfused by the MCA and grows with time. This penumbral area around the core infarct is believed to result from a propagation of the lesion from the core outward to tissue that remains perfused by collateral circulation during the occlusion. The effect of a therapeutic agent on the penumbra surrounding the core of the ischemic event may be examined when brain slices are obtained from the animal. The MCA supplies blood to the cortical surfaces of frontal, parietal, and temporal lobes as well as basal ganglia and internal capsule. Slices of the brain are taken around the region where the greatest ischemic effect occurs. These regions have been identified as region B, C, and D in Examples 1 and 2. These regions are not as readily compensated by alternative sources of blood flow as are regions A and E. This is because MCA is the terminal artery on which the lace of collateral arteries supplying the MCA-distributed area relies, thereby making the MCA-occlusion induced ischemia uncompensatible. On the other hand, anastomoses between MCA and the anterior carotid artery (ACA) in region A and between MCA and the posterior carotid artery (PCA) in region E (Examples 1 and 2), may compensate for the MCA occlusion-induced ischemia as observed in the present study.
In order to study the effect of estrogen on the propagation of the lesion following an ischemic event, rats were ovariectomized (OVX) and two weeks later were exposed to various estrogen preparations prior to or following MCA occlusion. (Examples 1 and 2) Pretreatment with a brain-targeted E2-CDS or 17β-estradiol (E2) itself decreased mortality from 65% in OVX rats to 22% in E2 treated and 16% in E2-CDS-treated rats. This marked reduction in mortality was accompanied by a reduction in the ischemic area of the brain from 25.6±5.7% in the OVX rates to 9.8±4.0 and 9.1±4.2% in the E2 implanted and the E2-CDS-treated rats, respectively. Similarly, pretreatment with the presumed inactive estrogen (17α-estradiol) reduced ischemic area by 55 to 81% (Examples 1). When administered 40 or 90 minutes after MCA occlusion, E2-CDS reduced ischemic area by 45-90% or 31%, respectively (Example 2). These results demonstrate the neuroprotective effect of estrogen in the brain following an ischemic event.
Reduction in available oxygen and glucose for energy metabolism is a feature of an ischemic event. This has a negative impact on the blood vessels that may be required to supply nutrients once the occlusion is reversed. The negative effect on blood vessels following ischemia, further increases the long-term damage associated with the event. This effect can be reproduced in vitro as described in Example 3. In these circumstances, it has been shown here, that estrogen compounds are capable of protecting brain capillary endothelial cells from cell death that would otherwise occur during hypoglycemia and anoxia during an ischemic event (FIGS. 5-7). As a consequence of this protection, the integrity of the vascular supply and the blood brain barrier is preserved by estrogen compounds such that following reperfusion of the brain after the ischemic event, blood flow and transport functions can once again occur.
Estrogen compounds have been shown here to have equivalent activity using different methods of delivery (Examples 1 and 2). Examples of sustained delivery described here include subcutaneous delivery by means of a silastic pellet and intravenous delivery by a chemical delivery system. Estrogen delivered by subcutaneous injection was also found to be effective (Example 1). Consequently, the method of delivery of estrogen should not be limited according to efficacy at the ischemic site, but instead should be selected according to factors affecting overall convenience. Such factors may include the rate of uptake of estrogen compounds into the blood and the central nervous system. Routes of administration of estrogen compounds for protecting cells against the effects of ischemia include any of subcutaneous, transdermal, oral, rectal, buccal, intramuscular, or intravenous methods or any alternative methods commonly used in the art to deliver estrogens. Furthermore, delivery may occur by means of a controlled delivery device sustained or by injection.
EXAMPLES
Example 1
Measurement of the effect on ischemia of pretreatment with estrogen compounds.
Rats were used as experimental models to test the effects of estrogen in protecting against ischemia. To remove the naturally occurring source of estrogen, an ovariectomy was performed prior to induction of ischemia.
Subsequent to the ovariectomy, rats were treated with an estrogen compound either by subcutaneous delivery 24 hours prior to the MCA occlusion or by intravenous delivery as follows:
Subcutaneous sustained delivery: 17β- or 17α-estradiol was packed into 5 mm long Silastic® tubes (Dow-Corning, Midland, Mich.) according to the method of Mohammed et al. Ann. Neurol 18, 705-711, 1985. Sham (empty) pellets were similarly prepared as estrogen negative controls. The pellets were implanted subcutaneously (sc) into ovariectomized rats 24 hours prior to MCA occlusion. 5 mm of silastic tubing containing estrogen results in plasma levels of 100-200 pg/ml.
Intravenous (iv) delivery: 17β-estradiol was prepared for intravenous delivery using an estrogen-chemical delivery system (E2-CDS) as described in Brewster et al., Reviews in the Neurosciences 2, 241-285 (1990) and Estes et al., Life Sciences 40:1327-1334 (1987). E2-CDS was complexed with hydroxypropyl-β-cyclodextrin (HPCD) (Brewster et al. J. Parenteral Science and Technology 43: 231-240, (1989)). The complexation achieved was 32 mg of E2-CDS per gram HPCD. In the first study, a single iv injection of E2-CDS (1 mg/kg body weight) was administered at 24 hours prior to MCA occlusion. The control was HPCD only. The chemical delivery system is formulated so that the estrogen is slowly released from the carrier. This delivery system has been shown to effectively deliver estrogen in a sustained manner to the brain. Indeed, the dose of E2-CDS used in Examples 1 and 2 (1000 mg/kg) is sufficient to provide 1000 pg/gm brain tissue at 24 hours post administration.
At 7 to 8 days after ovariectomy, a method for occluding the middle carotid artery was applied to the rat using the methods of Longa et al. (1989) Stroke, vol. 20, 84-91; and Nagasawa et al. (1989) Stroke, vol. 20, 1037-1043 with the following modifications.
Animals were anesthetized with ketamine (60 mg/kg, ip) and xylazine (10 mg/kg, intraperitoneal). Rectal temperature was monitored and maintained between 36.5° and 37.0° C. with a heat lamp throughout the entire procedure. The left carotid artery was exposed through a midline cervical incision. The left sternohyloid, sternomastoid, digastric (posterior belly) and the omohyloid muscles were divided and retracted. Part of the greater horn of the hyloid bone was cut to facilitate exposure of the distal external carotid artery (ECA). The common carotid artery (CCA), ECA, and internal carotid artery (ICA) were dissected away from adjacent nerves. The distal ECA and its branches, the CCA, and the pterygopalatine arteries were coagulated completely. A microvascular clip was placed on the ICA near skull base. A 2.5 cm length of 3-0 monofilament nylon suture was heated to create a globule for easy movement and blocking of the lumen of the vessel. This was introduced into the ECA lumen through the puncture. The suture was gently advanced to the distal ICA until it reached the clipped position. The microvascular clip was then removed and the suture was inserted until resistance was felt. The distance between the CCA bifurcation and the resistive point was about 1.8 cm. This operative procedure was completed within 10 min without bleeding. After the prescribed occlusion time (40 min), the suture was withdrawn from the ICA and the distal ICA was immediately cauterized.
Animals that survived until the scheduled sacrifice time were killed by decapitation. Scheduled post-ischemic sacrifices occurred at 6 hours, 24 hours and 1 week post MCAO (Table 1). For the 6-hour sample, animals were monitored continuously. For the 24-hour sample, animals were observed for about 4 hours and were then returned to their cage. Similarly, animals scheduled for the 1 week post-ischemic sacrifice were monitored for the first 4 hours after surgery and then daily thereafter.
The brains were isolated from the decapitated heads, sliced into 3 or 5 coronal tissue slices as described below for (a) and (b) and then stained with hematoxylin and eosin to determine the extent of the ischemic area. Stained slices were photographed and subsequently imaged using a Macintosh Cadre 800 computer, equipped with an Image 1.47 software program for the assessment of the cross-sectional area of the ischemic lesion. These images and the calculated area of ischemic damage were stored in the program for later retrieval and data reduction. The significance of differences in mortality among the different treatment groups (sham, E2 pellet and E2-CDS) was determined using Chi-Square analysis.
The results obtained using different routes of administration and different isomeric forms of estrogen compounds are provided below.
(a) The administration of estrogen (17β-estradiol) by sustained subcutaneous delivery or by controlled intravenous delivery, at 24 hours prior to the ischemic event, causes brain lesion size and mortality to be reduced
Three coronal slices were made at 1, 5, and 7 mm posterior to the olfactory bulb. Only 35% of the control (sham treated) animals survived until the scheduled post-ischemic sacrifice time (Table 1). In contrast, 78% and 84% of animals, treated 24 hours prior to MCA occlusion with either 17β-estradiol in a sc implant (5 mm silastic tube) or with E2-CDS (1 mg/kg) by an iv injection survived until the scheduled post-ischemic sacrifice time at 6 hours, 1 day, and 1 week. Elevated estrogen levels were detected in all samples at the time of sacrifice. The reduction in mortality in the estrogen pretreatment group was most notable at 1 day and 1 week after MCA occlusion. (Table 1). Furthermore, the reduced mortality in the estrogen-treated rats was correlated with the reduction of ischemic area in animals that survived to the scheduled 1 day or 1 week post-ischemia sacrifice time (FIG. 1). Control (sham treated) rats had ischemic lesions that occupied 25.6±5.7% of the cross-sectional area of brain sections evaluated (FIG. 1). By contrast, rats treated with 17β-estradiol or E2-CDS had ischemic lesions that occupied only 9.8±4.0 and 9.1±4.2%, respectively, of the brain area evaluated. The significance of differences among groups was determined by analysis of variance (ANOVA) and the Fischer's test was used for the post hoc comparison. Area under the curve determinations were not done here as only three brain slices were taken.
(b) Effect on brain lesion size of a subcutaneous injection of 17β-estradiol (100 μg/ml) two hours prior to an ischemic event.
Rats were ovariectomized, treated with a single dose of 17β-estradiol (100 μg/kg ) by a sc injection, 14 days after the ovariectomy and two hours prior to the ischemic event (MCA) as described above. This injection was sufficient to achieve a plasma concentration of 250 pg/ml at the time of occlusion. The animals were sacrificed at 24 hours and the brains extracted. The results shown in FIG. 2 illustrate the significant protective effect of E2 in tissue slices A-D. E2 replacement in OVX rats reduced by 46.3% and 44.1% (p<0.05) ischemic lesion size of the whole coronal section at region C and D, respectively (FIG. 2). These regions correspond to sections taken at 9 and 11 mm caudal to the olfactory bulb.
(c) Effect on brain lesion size and mortality, of a sustained subcutaneous delivery of 17α-estradiol initiated 24 hours prior to the ischemic event
Ovariectomized rats were treated with 5 mm silastic pellets containing 17α-estradiol at 24 hours prior to MCAO. At 24 hours after the MCAO, the animals were sacrificed and the brains extracted. Five, 2 mm thick coronal sections were made at 5, 7, 9, 11, and 13 mm posterior of the olfactory bulb. The slices were then incubated for 30 minutes in a 2% solution of 2,3,5-triphenyltetrazolium (TTC) (Sigma Chemical Corp., St. Louis, Mo.) in physiological saline at 37° C. Sham-treated rats showed the expected ischemic lesion, with the maximum ischemic area (24.1±2.4%) occurring in slice C (9 mm posterior to the olfactory bulb) and smaller lesion occurring in more rostral and caudal slices (FIG. 3). Animals pretreated with 17α-estradiol exhibited smaller ischemic areas compared with the sham treated animals in all slices evaluated (FIG. 3, A-E). Specifically, slices C, D and E (sections taken at 7, 9, and 11 mm posterior to the olfactory bulb), ischemic area was reduced significantly by 55%, 66%, and 81%, respectively (FIG. 3). The area under the ischemic lesion curve for the sham-treated, and the 17α-E2 groups was 8.1±0.8 and 3.7±1.3, respectively (Table 2) using student t tests. The significance of differences between sham and steroid-treated groups, were thus determined and data from two groups were compared for each experiment. To determine the area under the lesion curve for a given treatment, the trapezoidal method was used. Areas calculated for each animal were grouped and the differences between groups were determined by the student t test.
Example 2
Measurement of the effect of estrogen compounds administered after the ischemic event.
To test the extent to which estrogen treatment was effective after the onset of the occlusion, ovariectomized rats were treated iv with a sustained release of either E2-CDS or with a control (HPCD vehicle), the positive sample causing a brain tissue concentration of estrogen of 1000 pg/gm estrogen, 24 hours after administration. The estrogen compound was administered at 40 minutes and 90 minutes after the onset of the MCA occlusion (FIG. 4a and b, Table 2) and the animals sacrificed at 24 hours after the MCA occlusion. Five 2 mm thick coronal sections were made at 5, 7, 9, 11, and 13 mm posterior of the olfactory bulb as described in Example 1.
Post treatment at 40 minutes: As shown in FIG. 4a, the control (HPCD treated) rats had large ischemic areas in all slices sampled, with the maximum ischemic area of 25.6±2.7% observed in slice C. E2-CDS treatment reduced ischemic area in all slices sampled (FIG. 4). The extent of reduction in ischemic area ranged from 90% in slice A (5 mm posterior of the olfactory bulb) to 45% in slice C (9 m posterior to the olfactory bulb) (FIG. 4a). The integrated area under the ischemic lesion curve was 10.1±1.6 for the vehicle (HPCD-treated) rats and 4.5±0.9 for the E2-CDS animals (Table 2).
Post treatment at 90 minutes: Rats were treated with E2-CDS or HPCD vehicle at 90 minutes after the onset of the occlusion (FIG. 4b and Table 2). Again, HPCD treated animals showed a large lesion in all slices sampled, with the maximum ischemic area seen in Slice C (20.5±3.1% of the slice area). Treatment with E2-CDS reduced the mean ischemic area in all slices examined, however, the differences were not statistically significant. An evaluation of the area under the ischemia curve for the two groups revealed that treatment with E2-CDS reduced the ischemic area by 37.1%, from 8.2±1.7 (HPCD treated animals ) to 5.2±1.7 (E2-CDS treated animals).
These data show that the effect of treatment of an ischemic event with estrogen compounds is diminished as the time of treatment after the event increases.
Example 3
Estrogen compounds protect brain capillary endothelial cells under conditions associated with focal ischemia.
Primary rat brain capillary endothelial cells (BCEC) cultures were prepared following the method of Goldstein, J. Neurochemistry vol. 25, 715-717, 1975, incorporated herein by reference.
Hypoglycemia experiments were undertaken. 17β-estradiol (2 nm) or control (ethanol vehicle) were added to BCEC cultures. The glucose concentration of the culture media was then adjusted from 20 mg % to 200 mg % by adding appropriate amount of D-(+)-glucose to the glucose-free media and monitored by Glucose and L-Lactate Analyzer (YSI model 2300 STAT plus, YSI, Inc., Yellow Springs, Ohio). The hypoglycemic cultures were maintained for 24 hours or 48 hours prior to staining with Trypan blue.
Anoxia environment was created by placing culture dishes containing BCEC with or without 2 mn 17β-estradiol in the Modular Incubator Chamber (Billups-Rothenberg, Inc., Delmar, Calif.). Nitrogen gas was influxed to replaced the oxygen inside the chamber. The chamber was sealed and placed in the incubator four hours for nonhypoglycemic cultures and 2 hours for hypoglycemic cultures.
Cell mortality was counted using Trypan blue staining method. Cell death percentage was calculated as dead cell/alive cell×100%.
Statistics
The two-way analysis of variance was applied to determine the significance of the difference among the experimental groups. Kruskal-Wallis nanparametric analysis was used for data presented as percentage. The Mann-Whitney U tests were used when Kruskal-Wallis showed significance among groups. P<0.05 was considered significant.
The results are shown in FIG. 5a, 5b for cells deprived of glucose. The normal glucose concentration in the media is 200 mg % and there is little difference in % cell death between cultures with and without estrogen supplement. However, reduction in media glucose to 100 mg %, 40 mg %, and 20 mg % caused cell death, and 17β-estradiol saved cell loss by 35.9%, 28.4% and 23% (p<0.05), respectively, compared with corresponding control groups. It was further noted that there were floating cells, which meant more dead cells, in the control groups than in the E2-treated groups. Since these cells were excluded when counting cell mortality, the protective effects of E 2 may be underestimated. A similar beneficial effect was observed over a 24 hours and 48 hours hypoglycemic treatment (FIG. 5a and b).
Anoxia had a more dramatic effect in cell viability as shown in FIG. 6 for cells in media containing 200 mg % glucose. Anoxia induced cell death as much as 48.8% and 39.8% in the control and E2 reduced cell death by 28.4% (p<0.05) at 1-hour and 18.4% (p<0.05) at 4-hour anoxic insults.
When cells were exposed to both hypoglycemia (100 mg % hypoglycemia) and anoxia conditions (2 hours), 17β-estradiol was effective in protecting cultured BCEC from the cumulative effect of both conditions (FIG. 7).
The in vitro assay is representative of events that follow ischemia such as induced by occlusion of the MCA where oxygen and glucose supplies to the BBB endothelial cells are reduced.
TABLE 1______________________________________Effects of Pretreatment with 17 β-Estradiol or an Estradiol-ChemicalDelivery System (E2-CDS) on Mortality following MiddleCerebral Artery Occlusion. Time of Number of Number of Number of Planned Animals Animals Animals %Treatment Sacrifice Tested Alive Dead Survival______________________________________Sham 6 hrs 12 5 7 42 1 Day 18 6 12 33 1 Week 5 1 4 20 Total 35 12 23 35E2 Implant 6 hrs 6 3 3 50 1 Day 8 8 0 100* 1 Week 4 3 1 75* Total 18 14 4 78*E2CDS 6 hrs 7 5 2 71 1 Day 8 7 1 88* 1 Week 4 4 0 100 Total 19 16 3 84*______________________________________ *p < 0.05 versus sham control group at the same time by Chi Squares analysis.
TABLE 2______________________________________Effects of Estrogens on the Area Under the Ischemic LesionCurve in Ovariectomized Rats.Steroid Treatment Area Under Curve______________________________________Sham 24 hour pretreatment 8.1 ± 0.817α-estradiol 24 hour pretreatment 3.7 ± 1.3*HPCD Vehicle 40 min posttreatment 10.1 ± 1.6E2-CDS 40 min posttreatment 4.5 ± 0.9*HPCD Vehicle 90 min posttreatment 8.2 ± 1.7E2-CDS 90 min posttreatment 5.21 ± 1.7______________________________________ * p < 0.02 versus sham control by Students t test | The present invention is directed to a method of conferring protection on a population of cells associated with an ischemic focus, in subject, comprising:
(a) providing an estrogen compound having insubstantial sex-related activity; and
(b) administering an effective cumulative amount of the compound over a course that includes at least one dose within a time that is effectively proximate to the ischemic event, so as to confer protection on the population of cells. Also directed is a method of treating a myocardial infarct in a subject and an ischemic event with the above combination. | 0 |
BACKGROUND OF THE INVENTION
This invention relates generally to the sensing of temperatures in occupied spaces and deals more particularly with an electronic temperature sensor which is constructed and arranged to be mounted on a wall substantially flush with the wall surface.
In office buildings and other occupied spaces which are serviced by heating, ventilating and air conditioning (HVAC) systems, the HVAC equipment is normally controlled by a temperature sensor or thermostat in order to maintain the temperature in the occupied space at the desired level. Typically, the temperature sensor is contained in an enclosure which protrudes into the room from one of its walls. It is also common for the sensor to be mounted in a return air opening or duct where there is a positive flow of air from the conditioned space around the temperature sensing element. In either case, accuracy in the sensing of the temperature requires that the air in the room have good thermal contact with the temperature sensing element. Also, the element itself should have the minimum possible thermal capacity compared to its thermal conductivity to the room air so that it can respond quickly to temperature changes.
In the case of wall mounted sensors or thermostats, the active component is normally hidden behind a cosmetic cover which is provided with openings so that room air can migrate behind the cover and come into contact with the sensing element. Accuracy requires that the element have maximum thermal contact with the air in the conditioned space and minimum thermal contact with the wall which may have a temperature considerably different from that of the room air. Therefore, it is standard practice to mount the thermostat unit directly on the wall surface rather than recessing it or mounting it flush with the wall. Even though units which protrude into the room are recognized as being architecturally and aesthetically undesirable, they have largely been viewed as a necessary evil which must be tolerated in order to achieve both good thermal contact with the air and minimal thermal contact with the wall.
In mechanical or electrical sensing devices, the room air is allowed to directly contact a bimetal strip which provides the switching action for the HVAC equipment. The bimetal strip is thermally isolated from the remainder of the structure to the extent possible in order to prevent the wall temperature from effecting the temperature measurement. In electronic temperature sensors, the room air contacts a low power temperature sensitive element such as a thermocouple or a temperature sensitive resistor. The voltage or resistance of the element is measured from a remote location where more sophisticated active circuitry is provided.
The need to physically separate the active electronic circuitry from the sensing element creates calibration problems when the sensing element is initially installed or replaced. The element and wiring must be matched to the active circuitry which measures the output signal from the element. Although precalibrated sensing elements are available, they are relatively expensive and must be field calibrated in order to take into account the unknown resistance in the wiring which leads from the sensing element to the active circuitry. Field calibration adds significantly to the time and labor necessary to install the device and increases the cost accordingly. Another problem is that possible electromagnetic noise in the environment creates an additional uncertainty, particularly when the signal level is relatively low.
In recent years, small integrated circuits have been developed for use as low power, temperature sensitive current sources, as exemplified by the device shown in U.S. Pat. No. 4,123,698. The patented device is precalibrated on an absolute temperature scale (1 micro amp/°K., for example). Because the device acts as a current source, its output can be measured at a remote location without being distorted by the resistance of the wiring which transmits the signal to the remote location. However, the signal level is so low that electromagnetic interference is a significant problem that can adversely effect the accuracy of the temperature measurement. Also, circuits of this type have a wide span in their intrinsic temperature range, and this makes their accuracy unacceptable in the relatively narrow temperature range of human comfort (22°-26° C.).
These problems have been recognized, and circuits have been proposed for converting the low power level and wide temperature range to a higher power (such as 4-20 milliamps) and a narrower temperature range (such as 17°-30° C.). Although these circuits have rather high power requirements in comparison to the low power sensing devices, they can be used successfully in applications where there is good thermal contact with the medium which is being sensed, such as when the sensor is embedded in solid machinery or is immersed in liquid.
Similar circuits have been proposed for use in the sensing of air temperatures in occupied spaces, but the results have not been entirely satisfactory. When the sensor can be conveniently mounted in a moving air stream such as in a return air duct, the heat generating components are not particularly objectionable because the air stream acts to dissipate the heat. However, attempts to mount the temperature sensor and the heat generating active components in a wall mounted enclosure have not met with success. In order to obtain the necessary cooling from the convection of room air, it is necessary for the enclosure to protrude out well into the room, and this is undesirable from an architectural and aesthetic standpoint. Even then, satisfactory operation requires minimum convection which is not always present and ma fluctuate in any event. Due to the presence of the heat generating components, there is a noticeable offset (typically on the order of 1° C.), between the actual room temperature and the measured temperature. In order to account for this offset, the device is usually calibrated low intentionally. However, if the actual convection is different from the convection that is expected when the device is calibrated, the temperature signal is inaccurate.
At times, convection of air in the vicinity of the temperature sensor can be completely or nearly completely stopped. Then, the temperature can build up in the dead air space in the device, and the cosmetic cover prevents the heat from being dissipated by radiation. In this situation, errors as large as several degrees centigrade can result, and temperature errors of this magnitude are unacceptable. In the HVAC industry, electronic temperature sensors are expected to perform more accurately than conventional sensors rather than being lower than average in accuracy as occurs with the electronic sensors that are currently available.
Two different approaches have been followed in attempting to improve the accuracy of electronic temperature sensors. First, convection has been promoted by enlarging the package which contains the sensor and mounting it such that it protrudes out well into the room. The aesthetic disadvantages of this type of arrangement make it unacceptable in most applications even if the accuracy is within acceptable limits. The other approach that has been used involves removing the active heat generating components from the vicinity of the temperature sensing element. This approach has its own disadvantages, most notably in the inconvenience, high cost and accuracy degradation associated with the need for field calibration to compensate for the resistance in the wiring.
Using the wall as a heat sink to receive the heat generated by the electronic components has been rejected because the wall temperature often differs appreciably from the air temperature which dominates human perception. If the device is embedded in the wall to remove the heat that is generated, the wall temperature significantly affects the sensing element and results in significant steady state temperature errors caused by the difference between the wall temperature and the air temperature in the occupied space. Even more importantly, thermal delays arise and the HVAC control system can be completely destabilized in its temperature response capabilities.
SUMMARY OF THE INVENTION
Because of the foregoing thermal problems, temperature sensors used in HVAC control systems have not been mounted flush on the wall in any form (pneumatic, electric or electronic), despite the recognized architectural desirability of flush mounted sensors. Therefore, it is evident that a need exists for a temperature sensor which can be flush mounted on a wall without being subject to inaccuracy or other problems resulting from thermal effects. It is the primary goal of the present invention to meet that need. More specifically, it is among the important objects of the invention to provide a flush mounted electronic temperature sensor for HVAC application which operates accurately and is subject to only minimal self heating from the active circuit components so that it can be calibrated in the factory and interchanged in the field without being significantly affected by the resistance of the field wiring or reasonable levels of electromagnetic noise.
In accordance with the invention, a low power electronic temperature sensor which acts as a current source is packaged together with but thermally isolated from active heat generating circuit components which enhance the output signal from the sensor and make it useful in an HVAC control system. The unique electronic circuit includes an operational amplifier to provide a stable reference voltage. The temperature sensor is connected with the positive input of another operational amplifier, and the reference voltage is adjusted for calibration purposes by a potentiometer and applied to the negative input of the second operational amplifier. The amplifier output connects with its positive input through a current divider formed by three series resistors. The output from the circuit is obtained at the junction between two of the series resistors and has a gain established by the ratio of the resistances. The current gain is selected to convert the one microamp/°C. calibration of the low power sensor to about 33 microamps/°F. at the output terminal. The output zero point is also shifted from absolute zero to zero°F. which is more meaningful in connection with human comfort levels.
The current gain makes the circuit relatively insensitive to noise because it provides at the remote panel a relatively high voltage (typically, 0.75 volt). At the same time, a nearly optimal terminal resistance of 300 ohms can be used to obtain a temperature measurement which is 100 times the voltage that appears across the terminal resistance. The sensing device acts as a current source so that the resistance of the wiring has no effect on the signal. Consequently, calibration can be carried out at the factory, and the device is easier and less expensive to install and replace than devices which require calibration in the field.
The temperature sensor is thermally isolated from the heat generating electronic components and from the wall of the building by a unique physical arrangement of the parts. A flat mounting plate which can be mounted flush on a wall has a recess in its outer surface which receives a flat aluminum sensor plate. The sensor plate is exposed to the air in the room and is mounted to a styrofoam insulating block which keeps the sensor plate thermally isolated from the mounting plate and wall. Except for the temperature sensor, all of the circuit components are mounted on the back side of a printed circuit board which is recessed within a pocket on the back side of the mounting plate. The temperature sensor is glued to the back side of the aluminum plate in order to accurately sense the air temperature in the room, and the lead wires of the sensor connect with the rest of the circuitry on the back side of the circuit board.
This arrangement maintains the aluminum plate and temperature sensor in thermal isolation from the mounting plate and wall and from the heat generating components of the circuitry. At the same time, the sensor plate is exposed to the room air and the sensor is in infinite thermal contact with the sensor plate for accurate sensing of the air temperature. The contact of the mounting plate with the wall assists in conducting heat from the circuit board to the wall. The heat is also dissipated into the wall cavity by radiation and convection. The circuit board and the walls of its mounting cavity effectively shield the sensor and sensor plate from the active components on the back side of the circuit board to prevent the heat which is generated by the active components of the circuit from having a significant thermal effect on the sensor operation.
DESCRIPTION OF THE DRAWINGS
In the accompanying drawinqs which form a part of the specification and are to be read in conjunction therewith and in which like reference numerals are used to indicate like parts in the various views:
FIG. 1 is an exploded perspective view taken from the back of a temperature sensor constructed according to a preferred embodiment of the present invention;
FIG. 2 is an exploded perspective view taken from the front of the temperature sensor;
FIG. 3 is a front elevational view of the temperature sensor on an enlarged scale, with a portion of the sensor plate broken away for purposes of illustration;
FIG. 4 is a fragmentary sectional view taken generally along line 4--4 of FIG. 3 in the direction of the arrows; and
FIG. 5 is a schematic diagram of the circuitry included in the temperature sensor.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawings in more detail, a temperature sensor constructed in accordance with the present invention is generally designated by numeral 10. The temperature sensor 10 includes a generally flat mounting plate 12 which is constructed to be mounted flush on the surface of a wall such as the wall 14 shown in broken lines in FIG. 4. Plate 12 may conveniently formed from rigid plastic, although metals and other materials may also be used. The outer surface of plate 12 faces into an occupied space such as an office or other room located within a building and heated and cooled by an air conditioning system. The air conditioning equipment operates under the control of the temperature sensor 10. The outer surface of the plate 12 is beveled at l2a on its periphery. The back surface of plate 12 is located adjacent to the wall 14 and is provided on its periphery with a flat lip l2b which directly contacts the surface of wall 14. A pair of wall fasteners 16 (see FIG. 4) are extended through holes 18 formed in plate 12 and are threaded into or otherwise fastened to the wall 14 in order to mount plate 12 substantially flush with the exposed surface of the wall.
A rectangular cavity 20 is formed in the outer surface of plate 12. The cavity 20 is approximately 1.1 inches wide, 1.6 inches long, and 1/4 inch deep in one embodiment of the invention. The bottom of cavity 20 is formed by a flat base panel 22 which is integral with plate 12.
Mounted in cavity 20 are a styrofoam block 24 and an aluminum sensor plate 26. The block 24 serves as a thermal insulator for the sensor plate 26 and may be approximately 0.9 inch wide, 1.4 inches long and 3/16 inches thick. Both of the flat surfaces of block 24 are provided with a suitable adhesive, and the back side of the block is adhesively secured to the base panel 22. Block 24 is somewhat smaller than cavity 20 so that an air space is provided between the edges of the block and the walls of the cavity 20, as best shown in FIG. 4. A passage 24a is formed through the center of block 24 and registers with a larger opening 22a which is formed through the base panel 22. By way of example, passage 24a can have a diameter of 1/4 inch, while the diameter of opening 22a may be 3/8 inch.
The length and width dimensions of the aluminum sensor plate 26 are slightly less than those of the cavity 20 and slightly greater than those of block 24. For example, plate 26 may have a width of one inch, a length of 1.5 inches and a thickness of approximately 0.03 inch. The front or exposed face of plate 26 is roughened or provided with a backed enamel coating and is coplanar with the exposed surface of plate 12. The back face of plate 26 is bare aluminum and is adhesively secured to the insulating block 24. Because of the difference between the dimensions of cavity 20 and plate 26, a small gap of approximately 0.05 inch is provided between each edge of plate 26 and the corresponding wall of the cavity 20. The manner in which the sensor plate 26 is mounted maintains it thermally isolated from the mounting plate 12.
A rectangular pocket 28 is formed on the back surface of plate 12. The pocket 28 includes opposite side walls 28a, a top wall 28b and a bottom wall 28c, all of which are integral with plate 12. The pocket 28 is considerably larger and deeper than the cavity 28 on the front side of plate 12. The base panel 22 forms the bottom of the pocket 28. Extending along the base panel 22 adjacent to the opposite side walls 28a of the pocket are a pair of ribs 30 (one of which is shown in FIG. 1). The ribs 30 cooperate with upper and lower tabs 32 to form a mounting surface for receiving the edges of a rectangular printed circuit board 34. The front side of the circuit board 34 engages ribs 30 and tabs 32 and faces toward and is spaced from the base panel 22. Screws 36 are extended through the circuit board and threaded into the tabs 32 in order to hold the circuit board in place within the pocket 28. The circuit board has substantially the same width and length as pocket 28 in order to fit closely therein, as best shown in FIG. 4.
The active circuit components of the temperature sensor are mounted on the back side of circuit board 34 or the side which faces into the wall cavity. The pocket 28 is located within the wall cavity when plate 12 is mounted on the wall.
An electronic temperature transducer is formed by an integrated circuit 38 which provides an output current proportional to the temperature sensed by the transducer. The temperature sensing circuit 38 may be of the type commercially available under the trade designation AD590, and its components and manner of operation are described in U.S. Pat. No. 4,123,698 which is herein incorporated by reference.
The temperature sensing circuit 38 is enclosed within a metal housing which is secured to the back face of plate 26 by a drop of heat conductive adhesive 40 (see FIG. 4). The housing for the integrated circuit 38 is thus in thermal contact with plate 26 and is located within the passage 24a in the styrofoam insulated block 24. Circuit 38 includes a pair of electrical leads 42 which extend through passage 24a and opening 22a to the circuit board 34. The leads 42 are connected with the remainder of the circuit by soldering them to pads 42a located on the back side of the circuit board 34.
A cover plate 44 may be attached by screws 46 to the back edge of the pocket 28 if it is desired to enclose the circuitry within the pocket. However, in most cases, it is more desirable to leave the back of the pocket open so that the heat generated by the active circuit components on the back side of the circuit board can be dissipated into the wall cavity by radiation and convection. Consequently, the cover plate 44 is normally used only during handling and shipping and is removed when the unit is installed.
Referring now to FIG. 5, the electronic circuitry associated with the temperature sensing circuit 38 includes a diode 48 having its anode connected with a terminal 50 to which an unregulated positive DC voltage in the range of +6 to +9 volts DC is applied. The diode 48 protects the remainder of the circuit from damage in the event that the wiring is improperly connected. Also, an ammeter 52 can be connected across the diode 48 to provide a current measurement. The measured current in milliamps multiplied by 30 yields a measurement of the temperature in °F. Thus, the diode provides a convenient local means for measuring the temperature.
A filtering capacitor 53 is connected between the cathode of diode 48 and an internal common ground line of the circuit. The capacitor 53 filters out high frequency noise. The cathode of the diode 48 is also connected with an operational amplifier 54 and with one side of the temperature sensing circuit 38. The temperature sensing circuit is precalibrated to provide an output current of one microamp per degree centigrade, and the output side of circuit 38 is connected with the positive input to the operational amplifier 54.
Another operational amplifier 56 is included with amplifier 54 in a single integrated circuit package 58 (see FIGS. 1 and 4) mounted on the back side of the printed circuit board 34. The two amplifiers 54 and 56 are powered by the DC voltage that is available at the cathode of diode 48. The operational amplifiers have excellent temperature and voltage stability (50-100 ppm) over the temperature and voltage range to which they are normally subjected.
Amplifier 56 serves as a reference voltage source. The internal regulated voltage of 200 millivolts is applied to the positive input of amplifier 56. The output of amplifier 56 connects to its negative input through resistor 60 and filtering capacitor 62 in parallel. Resistor 64 connects the negative input to amplifier 56 with the common internal ground line of the circuit.
The reference voltage which is thereby obtained from amplifier 56 (approximately 499 millivolts) is more stable than that which could be obtained from a Zener diode of comparable cost. The current and power consumption are also low in comparison to those of a more conventional integrated circuit acting as a separate voltage reference source.
The stable reference voltage on the output of amplifier 56 is applied to a pair of series resistors 66 and 68, and to a calibration potentiometer 70 connected between the resistors 66 and 68. Resistor 68 is connected with the common ground line for the circuit. The center tap 72 of the potentiometer 70 connects with the negative input of operational amplifier 54. Potentiometer 70 preferably has an adjustment range of approximately 20° F. By properly adjusting the potentiometer, a calibrated reference voltage is applied to the negative input of amplifier 54. A filtering capacitor 74 is connected between the output and the negative input of operational amplifier 54 to filter high frequency noise.
The variable output of amplifier 54 connects through resistor 76 with the common ground line of the circuit. The output then combines with other substantially constant currents and flows from the system common line through resistor 78 to the negative terminal 80 of the circuit. The negative terminal 80 connects with the positive input of amplifier 54 through resistor 82 and filtering capacitor 84 which are in parallel with one another and in series with resistor.
A remotely located panel 86 connects with the negative terminal 80 through suitable wiring 88 which leads to one end of a 300 ohm, 1% precision resistor 90. The other end of resistor 90 connects with actual ground. A read out display 92 on panel 86 is connected across the resistor 90 and measures the voltage across the resistor. The voltage measurement in volts can be multiplied by 100 to provide an indication of the actual room temperature in °F. The temperature may be displayed on the read out device 92, and it may also be used as a thermostat signal to control air conditioning equipment and other machinery if desired.
The temperature sensor 10 is assembled by first securing the styrofoam insulating block 24 to the base panel 22 and then securing the aluminum sensor plate 26 to the insulating block 24. For good thermal isolation of the sensor plate 26, it is necessary that the edges of the plate remain out of contact with the mounting plate 12. The integrated circuit 40 normally has three leads 42, one of which is normally used to facilitate mounting of the device. This third leg is preferably trimmed off to prevent it from conducting heat to the circuit 38. The other two leads 42 are extended through the circuit board 34 to its back side and are hand soldered to the pads 42a while the housing for the integrated circuit 38 is held by a jig (not shown) a preselected distance away from the front surface of the circuit board 34. This properly locates the circuit 38 relative to the circuit board. The circuit 38 should be spaced at least 1/4 inch away from the circuit board 34.
At this point, all of the circuit components have been soldered or otherwise installed on the back side of the circuit board 34. A drop of heat conducting glue 40 is applied to the back face of plate 26 through opening 22a and passage 24a, and the circuit board 34 is then applied to the ribs 30 and mounting tabs 32 with the integrated circuit 38 disposed against the back face of plate 26 and against the glue 40. The screws 36 can then be applied to secure the circuit board 34 in place within the pocket 28. The back cover 44 can be applied to protect the circuit components from damage during shipping and handling. As previously indicated, the cover 44 is removed before the device is installed. The potentiometer 70 is adjusted in the factory in order to properly calibrate the device.
Installation on the wall 14 is quickly and easily carried out by first cutting a rectangular hole 14a in the wall at the proper location and the same size as or slightly larger than the pocket 28. Plate 12 can be applied flush to the surface of wall 14 and mounted on the wall by applying the screws 16. The remote panel 86 can be situated at any desired location and connected to terminal 80 the wiring 88. The installed unit has an aesthetically pleasing and architecturally desirable appearance with only the outer surface of the mounting plate 12 and the sensor plate 26 visible. The flush mounting of the unit is an architecturally desirable feature, and the sensor is no more objectionable than an ordinary flush mounted wall switch or outlet cover plate.
In operation of the sensor, naturally occurring convection carries the air within the occupied space into direct thermal contact with the exposed face of the sensor plate 26. The sensor plate 26 is thereby maintained at the same temperature as the air within the occupied space, and this temperature is transmitted by conduction to the temperature sensing circuit 38. Circuit 38 acts as a current source which provides a current that is directly proportional to the sensed temperature. If the current through the sensing circuit 38 increases, the current through resistor 82 also increases, and the voltage on the positive input to the operational amplifier 54 increases as a result. Because of the high gain of the operational amplifier 54, this increase in the positive input increases the output voltage and thus increases the current through resistors 76 and 78, making the output terminal 80 more negative. The negative incremental voltage at terminal 80, working back through resistor 82, drains off the incremental current from circuit 38 and pulls the voltage on the positive input to the operational amplifier back down to where it is approximately equal to the reference voltage applied to the negative input of amplifier 54. In this manner, the output voltage of the operational amplifier changes as necessary to effect substantial equality in the inputs to amplifier 54.
The current gain is established by the current divider network comprising resistors 82 and 78. With resistor 82 having a resistance of 1.8 kohms and resistor 78 having a resistance of 30.1 ohms, the current gain is given by 1+1800/30.1=60. The current gain thus converts the one microamp/°C. output from the low power temperature sensing circuit 38 to 33 microamps/°F. appearing at terminal 80. The current gain makes the device less sensitive to noise by making it possible to provide at the remote panel 86 a relatively large voltage (typically 0.75 volts compared to the 0.025 ambient thermal voltage). Also, the terminal resistor 90 has a nearly optimal terminal resistance (300 ohms compared to the 377 ohm characteristic resistance of free space). The zero output point is shifted from absolute zero to 0° F., thereby reducing the typical offset and improving the overall accuracy by reducing the problem of resolving a small difference in a large number. It also permits factory calibration at the temperature of greatest interest (approximately 34° or 75° F.). The voltage across the terminal resistor 90, when multiplied by 100, provides a measurement of the air temperature in the occupied space.
The improved electrical capabilities of the circuit are obtained at the cost of a substantial increase in the heat generated during operation of the device. The heat should be minimized by keeping the applied voltage as low as possible, and the applied voltage should thus be maintained at a maximum of 8 volts DC. Self heating can also be minimized by minimizing the current. However, due to the nature of the circuit and the active components, it is not practical to reduce the current below the values indicated previously without reducing the current to the low power temperature sensing circuit 38, which would result in a loss in the advantages of noise immunity, offset compensation, and factory calibration for improved accuracy and field interchangeability.
Because of the current gain, the temperature sensing circuit 38 generates only 1/60 of the power of the rest of the circuitry, and the considerable heat which is generated by the remainder of the circuitry is transmitted by conduction to the wall 14. The key generating components are all located on the back side of the circuit board 34, and the heat is conducted from the components to the fiberglass circuit board 34 and then from the circuit board to the mounting plate 12 and the wall 14. At the same time, the temperature sensor 38 and sensor plate 26 are thermally isolated from the wall due to their physical separation from the wall and the insulation provided by the styrofoam block 24. The air gap which is provided between the housing for circuit 38 and the circuit board 34 provides effective thermal insulation, with only a small amount of heat being transmitted through the electrical leads 42. The heat generated by the active circuit components on the back side of circuit board 34 is also dissipated by radiation and convection through the back of the pocket 28 and into the wall cavity.
It is preferred that the sensor plate 26 be constructed of aluminum because of its good thermal properties. Also, the ratio of the area of the sensor plate to its thickness should be approximately as indicated above for thermal reasons as well as structural and economic reasons. Plate 26 should not only conduct heat but it should do so with a minimum possible time delay in order to avoid delays in the response time. By increasing the thickness of the plate to improve its thermal conductivity, the thermal performance is actually degraded because of the added thermal capacity which slows down the response time and thereby tends to destabilize the HVAC control system.
The exposed parts of the temperature sensor 10 can be painted or otherwise attractively finished in order to match the color and decor of the room in which it is installed. Most paints improve the thermal contact with the air in the occupied space by improving the thermal emissivity to thereby improve the radiative transfer to the sensor plate from all of the surfaces and bodies in the room. If the paint is relatively thin (less than 0.003 inch thick), the radiative transfer improves faster than the thermal conductivity is degraded or the thermal capacity is increased. However, it is important to assure that the paint does not for a conductive bridge between the edge of the aluminum sensor plate 26 and the walls of the cavity 20. For this reason, the dimensions of the styrofoam block 24 are preferably somewhat less than those of the sensor plate 26 so that a large gap is provided behind the plate between the styrofoam block and the cavity walls. It is difficult for paint and other finishing materials to fill such a broad gap.
From the foregoing, it will be seen that this invention is on well adapted to attain all the ends and objects hereinabove set forth together with other advantages which are obvious and which are inherent to the structure.
It will be understood that certain features and subcombinations are of utility and may be employed without reference to other features and subcombinations. This is contemplated by and is within the scope of the claims.
Since many possible embodiments may be made of the invention without departing from the scope thereof, it is to be understood that all matter herein set forth or shown in the accompanying drawings is to be interpreted as illustrative and not in a limiting sense. | A temperature sensor which is flush mounted on a wall of a room in which the temperature is sensed. A mounting plate secured to the wall has a cavity in its face which receives an aluminum sensor plate and an insulating block which thermally insulates the sensor plate from the mounting plate. A temperature sensing integrated circuit contacts the back side of the sensor plate and has electrical leads which extend to the back side of a printed circuit board mounted in a pocket on the back side of the mounting plate. The integrated circuit acts as a current source having its output signal enhanced by active solid state circuit components mounted on the back side of the circuit board where their heat is dissipated by conduction through the mounting plate and wall and by convection and radiation into the wall cavity to avoid affecting the sensor plate. The circuitry allows active factory calibration and eliminates adverse effects on the signal caused by background environmental noise. | 8 |
This application is a continuation-in-part of Ser. No. 86,627 filed Oct. 19, 1979 now abandoned.
BACKGROUND OF THE INVENTION
Trauma to the brain or spinal chord caused by physical forces acting on the skull or spinal column, by ischemic stroke or by hydrocephalus results in edema and swelling of the affected tissues. This is followed by ischemia, temporary or permanent brain and/or spinal chord injury and may result in death. The tissues mainly affected are classified as grey matter, more specifically astroglial cells.
The specific therapy currently used for the treatment of the medical problems described is limited to steroids, such as, the sodium salt of 6-α-methylprednisolone succinate. Although these agents are effective in situations involving white matter edema, they comprise relative ineffective therapy for grey matter edema. Thus, the compounds of this invention comprise a novel and specific treatment for a medical problem where no specific therapy is available.
The compounds of the invention have the added advantage of being devoid of the toxic side effects of the steroids and of having little or no renal effects.
DESCRIPTION OF THE INVENTION
The compounds of the instant invention are best characterized by reference to the following structural formula: ##STR1## wherein R is H, lower alkyl, branched or unbranched, such as methyl, ethyl, propyl, isopropyl, butyl, sec. butyl, isobutyl and the like; lower alkenyl, such as vinyl and allyl; lower alkynyl, such as propargyl; aryl, such as phenyl; aryl lower alkyl, such as benzyl; lower cycloalkyl, such as cyclopropyl and cyclobutyl, lower cycloalkyl lower alkyl, such as cyclopropylmethyl and the like;
R 1 is H, lower alkyl, such as methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl and the like; lower alkenyl, such as, allyl, 2-butenyl, and the like; lower alkynyl, such as, propargyl, butynyl and the like; lower cycloalkyl, such as cyclobutyl, cyclopentyl and the like; substituted lower alkyl, where the substituent is carboxy, lower alkoxycarbonyl, oxo, hydroxy, lower alkoxy, halo, lower acyloxy, lower dialkylamino, sulfamoyl, pyridyl, furyl, tetrahydrofuryl, aryl, 1-methylpiperidyl, morpholinyl, pyrrolidinyl, 1-methylpiperazinyl, thienyl, and the like; substituted cycloalkyl, such as carboxycycloalkyl; and the like; heterocyclic, such as, imidazolyl, pyridyl, thiazolyl, pyrazinyl, furyl, and the like; aryl, such as phenyl, carboxyphenyl, hydroxymethylphenyl and the like;
Y 1 and Y 2 are Cl and CH 3
A is (CH 2 ) 2 or ##STR2## where R 2 is H, methyl or ethyl, R 3 is H, F or methyl and R 2 and R 3 may be joined together to form a ring which can be represented by >C(CH 2 ) n where n=2, 3, or 4.
Since the 9a carbon atom in the molecule is asymmetric, the compounds of the invention are racemic; however, these compounds can be resolved, so that the invention includes the pure enantiomers. In addition, in some instances, the group represented by A and by R 1 includes an asymmetric carbon atom. Thus, these molecules may contain two or three asymmetric carbon atoms and now can consist of two or four diastereomers, each of which consists of two enantiomers. The invention includes each diastereomer and their enantiomers whenever they exist.
Although the invention involves novel [(5,6,9a-substituted-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-alkanoic and cycloalkanoic acids, it also includes the obvious analogs, the corresponding esters, salts and their derivatives such as anhydrides, amides, hydrazides, guanidides and the like.
PREFERRED EMBODIMENTS OF THE INVENTION
The preferred embodiments of the instant invention are realized in structural formula IA wherein:
R is lower alkyl, alkenyl, alkynyl, cyclopropyl, cyclopropylmethyl, or aralkyl ##STR3## R 2 is hydrogen, lower alkyl, substituted alkyl, such as carboxyalkyl, hydroxyalkyl, dihydroxyalkyl, trihydroxyalkyl, oxoalkyl, dilower alkylaminoalkyl, and heterocyclic-alkyl.
Y 1 and Y 2 are chloro
Also included are the enantiomers of each racemic compound.
A preferred compound is [(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid.
Another preferred compound is [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid and its enantiomers.
Another preferred compound is [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid and its enantiomers.
Another preferred compound is [(5,6-dichloro-3-oxo-9a-isopropyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetic acid.
Another preferred compound is [(9a-butyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid and its enantiomers.
Another preferred compound is [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid.
Another preferred compound is [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetic acid and its enantiomers.
Another preferred compound is [(5,6-dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetic acid and its enantiomers.
Another preferred compound is [(5,6-dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid and its enantiomers.
Another preferred compound is [(5,6-dichloro-9a-cyclopropylmethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid and its enantiomers.
Another preferred compound is [(9a-benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetic acid and its enantiomers.
Another preferred compound is 1-carboxy-1-methylethyl [(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is 1-carboxy-1-methylethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
Another preferred compound is 1-carboxy-1-methylethyl [(5,6-dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
Another preferred compound is 1-carboxy-1-methylethyl [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is 1-carboxy-1-methylethyl [(9a-butyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is 1-carboxy-1-methylethyl [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetra-hydro-3H-fluoren-7-yl)oxy]acetate.
Another preferred compound is 1-carboxy-1-methylethyl [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is 1-carboxy-1-methylethyl [(5,6-dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is 1-carboxy-1-methylethyl [(5,6-dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is 1-carboxy-1-methylethyl [(5,6-dichloro-9a-cyclopropylmethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is 1-carboxy-1-methylethyl [(9a-benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is ethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is 3-pyridylmethyl-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is 2-oxopropyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is 2-(dimethylamino)-ethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is 3-carboxypropyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and its enantiomers.
Another preferred compound is carboxymethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
Another preferred compound is 3-hydroxypropyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
Another preferred compound is [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid hydrazide.
Especially preferred are the (+)R enantiomers of the racemic modification of each compound; thus, the most preferred compounds are the (+)R enantiomers of the compounds tested supra.
Included within the scope of this invention are the analogs and derivatives of the parent carboxylic acids, their salts, their esters and their amides and other derivatives which may be prepared by conventional methods well known to those skilled in the art.
Thus, the acid addition salts can be prepared by the reaction of the carboxylic acids of the invention with an appropriate amine, guanidine, ammonium hydroxide, alkali metal hydroxide, alkali metal bicarbonate or alkali metal carbonate and the like. The salts are selected from among the non-toxic, pharmaceutically acceptable bases.
The synthesis of the carboxylic acid compounds of Formula II is generally carried out by the hydrolysis of the corresponding ester (III): ##STR4##
The process can be effected by heating the ester in a solution of acetic and aqueous inorganic acid, such as hydrochloric acid, sulfuric acid and the like. The hydrolysis also can be effected in aqueous alcoholic base such as sodium hydroxide or potassium hydroxide in aqueous methanol or ethanol. The product is recovered by acidification with an acid, such as, hydrochloric acid. The reaction can be carried out at temperatures of 30° C. to 100° C. for periods of about 20 minutes to 6 hours, depending on the specific ester used and the other reaction conditions. In the instances, such as where A is --CHF--, it is advantageous to carry out the hydrolysis using a weak base, such as aqueous sodium bicarbonate. A solvent, such as aqueous ethanol, methanol or isopropyl alcohol is used and the mixture heated at 45° C. to 100° C. for periods of 15 minutes to 4 hours. Acidification of the reaction mixture with strong aqueous acids, such as hydrochloric acid, hydrobromic acid or sulfuric acid produces the desired compound of Formula II.
A second method for the preparation of compounds of the type illustrated by Formula II involve the reaction of a haloalkanoic or halocycloalkanoic acid (X-A-COOH) with the appropriate phenol (IV). ##STR5## Using a haloalkanoic or halocycloalkanoic acid X-A-COOH, where X=iodo, bromo or chloro and A is as defined above, for example, iodoacetic acid or bromofluoroacetic acid, as the etherification agent, the reaction is conducted in the presence of a base. The base is selected from among the alkaline earth or alkali metal bases such as sodium or potassium carbonate, calcium hydroxide and the like. The reaction is carried out in a liquid reaction milieu, the choice being based on the nature of the reactants; however, solvents which are reasonably inert to the reactants and are fairly good solvents for the compounds of Formula IV and the X-A-COOH reagent, can be used. Highly preferable are dimethylformamide, ethanol, acetone, and N-methylpyrrolidine-2-one, and the like.
A third method for preparing compounds of Formula II involves the pyrolysis of the corresponding tert.-butyl ester (IB): ##STR6##
This method involves heating a tert.-butyl ester of the type illustrated by formula IB at from about 80° C. to 120° C. in a suitable nonaqueous solvent in the presence of catalytic amount of a strong acid. The solvents are generally selected from among the type benzene, toluene, xylene, etc. and the acid catalyst may be a strong organic or inorganic acid, such as p-toluenesulfonic acid, benzenesulfonic acid, methane-sulfonic acid, sulfuric etc. The acid, being a catalyst, is generally used in relatively small quantities as compared to the tert.-butyl ester (IB). It is to be noted that this reaction is a pyrolysis and not a hydrolysis, since water is excluded from the reaction and the products are a carboxylic acid (Formula II) and isobutylene and no alcohol is produced.
Another method of converting compounds of Type IB to those of Type II is by heating compounds of type IB with trifluoroacetic acid in a solvent like dichloromethane.
A fourth method is limited to the instances wherein compounds of Formula IIA are produced, i.e., where A is ethylene: ##STR7##
This synthesis involves the reaction of the appropriate phenol (IV) with propiolactone in the presence of a base and a solvent, preferably while heating and stirring the reaction mixture. Solvents, such as a mixture of water and an alcohol, such as methanol, ethanol or propanol are used. The base is selected from among the alkali metal hydroxides or carbonates, such as sodium hydroxide, potassium hydroxide, potassium carbonate and the like. The temperature is generally at the boiling point of the solvent mixtures but it may be at 50° C.-110° C. depending on the reactants involved. The product is isolated by acidification of the reaction mixture with a strong acid such as hydrochloric or sulfuric acid.
Special methods are used to synthesize compounds of Formula II where R is vinyl (Formula IIB) or cyclopropyl (Formula IIC). ##STR8##
An alkyl [(2-ethylidene-1-oxo-2,3-dihydro-1H-indene-5-yl)oxy]alkanoate is treated with methyl vinyl ketone (MVK) in the presence of a base, such as, potassium tert.-butoxide, in 1,2-dimethoxyethane at 0° C. or lithium dimethylamide at -70° C. in tetrahydrofuran. The reaction is conducted in an atmosphere of dry nitrogen.
The alkyl [[1-oxo-2-(3-oxobutyl)-2-vinyl-2,3-dihydro-1H-inden-5-yl]oxy]alkanoate produced is cyclized to an alkyl [(3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]alkanoate by heating in the presence of a reagent like pyrrolidine acetate and the like in benzene or toluene. Heating with a base, such as, potassium tert.-butoxide in tert.-butyl alcohol is also effective.
Finally, the compound of Formula IIB is produced by saponification of the alkyl[(3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]alkanoate by heating with a base, such as, sodium or potassium hydroxide in a solvent, such as water or a mixture of methanol or ethanol and water. The product is generated upon acidification with an acid, such as, hydrochloric or sulfuric acid.
Alternatively, compounds of Formula IIB can be generated directly from an alkyl [[1-oxo-2-(3-oxobutyl)-2-vinyl-2,3-dihydro-1H-inden-5-yl]oxy]alkanoate by dissolving in a mixture of an alcohol, such as, methanol or ethanol and aqueous sodium hydroxide or potassium hydroxide. After standing at ambient temperature for 24 to 48 hours, the product is isolated by acidification with an acid, such as, hydrochloric or sulfuric acid.
The preparation of compounds of Formula IIC is carried out by treating an alkyl [(3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]alkanoate with a zinc-copper couple and methylene iodide in a solvent, such as, ethyl ether, tetrahydrofuran or 1,2-dimethoxyethane at ambient temperature for an hour according to the conditions of the Simmons-Smith reaction. The alkyl [(3-oxo-9a-cyclopropyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate is then hydrolyzed to a compound of Formula IIC by heating with an aqueous-alcoholic solution of a base, such as, potassium hydroxide or sodium hydroxide followed by acidification with an acid, such as, hydrochloric or sulfuric acid.
Alternatively, a compound of Formula IIC can be produced by treating an alkyl [[1-oxo-2-(3-oxobutyl)-2-vinyl-2,3-dihydro-1H-inden-5-yl]oxy]alkanoate with zinc-copper couple and methylene iodide in tetrahydrofuran to give an alkyl [[1-oxo-2-(3-oxobutyl)-2-cyclopropyl-2,3-dihydro-1H-inden-5-yl]oxy]alkanoate which is then cyclized and finally hydrolyzed by the methods just described. Likewise, the alkyl [[1-oxo-2-(3-oxobutyl)-2-cyclopropyl-2,3-dihydro-1H-inden-5-yl]oxy]alkanoate may be converted directly to IIC by treatment with aqueous methanolic sodium hydroxide followed by acidification with hydrochloric acid.
The preparation of compound IV can be carried out by one or the other of two methods. The first method involves the following three-step process: ##STR9##
Compounds of the type represented by Formula V which are used to produce the compounds of this invention have generally been described in the scientific and/or patent literature. For those that have not been previously disclosed or must be prepared by new methods, a description of their synthesis will be described later.
The first step (Step A) in the synthesis involves the reaction of a compound of Formula V with methyl vinyl ketone to produce a compound of Formula VI. The reaction is catalyzed by a base, such as triton B (benzyltrimethylammonium hydroxide) in methanol but other bases such as tetramethylammonium hydroxide, tetraethylammonium hydroxide or sodium methoxide are effective catalysts. Solvents which are inert to the reaction and are effective in dissolving the reactants and product are normally used. Tetrahydrofuran is an especially preferred solvent but others, like p-dioxane or 1,2-dimethoxyethane can be used. The reaction is generally conducted at ambient temperatures but temperatures in the range of 10° C. to 45° C. or somewhat above or below these values can be used.
The second step (Step B) in the synthesis is the cyclization of a compound of Formula VI to give a compound of Formula VII. The reaction is generally conducted in the presence of a solvent such as benzene, toluene, xylene, anisole and the like but many other solvents which are inert to the reactants and to the catalyst are useful. A catalyst is necessary for increasing the rate of reaction. Salts of weak organic acids and weak inorganic or organic bases are preferred; for example, pyrrolidine acetate, piperidine acetate, pyrrolidine propionate and the like. The reaction is preferably conducted at the temperature of the boiling solvent but temperature of 30° C.-120° C. can be used. It is advantageous to carry out the reaction under conditions in which the water produced in the reaction is constantly removed. This is effected by various means, such as using a Dean-Stark constant water separator or co-distilling the solvent and the water. Another device for removing the water is to add molecular sieves designed for removing water, for example, Davison Molecular Sieves of 3 A size M-564 (Cation: potassium, base:alumina-silicate).
In some instances, bases, such as potassium tert.-butoxide in tert.-butyl alcohol or potassium hydroxide or sodium hydroxide in aqueous methanol or ethanol may be used to effect cyclization.
The last step (Step C) involves the ether cleavage of a compound of Formula VII to produce a compound of Formula IV. This can be accomplished by many of the agents known to cleave ethers, especially useful are hydrohalide salts of weak bases, such as pyridine hydrochloride or pyridine hydrobromide, but other agents, such as aqueous hydrobromic acid or aluminum bromide can be used. When pyridine hydrohalides are used, the temperatures above that which these substances melt are generally employed. This usually involves temperatures in the range of 150° C. to 215° C., but temperatures somewhat lower or higher can be used. The period of heating varies depending on the specific compound but periods of from 15 minutes to 2 hours may be used.
The second method for preparing compounds of Formula IV is shown by the five-step reaction illustrated below. It should be mentioned that this is not simply a cyclical method whereby a compound of the invention (Formula II) is converted to one of its precursors (Formula IV) simply to be reconverted to the product again (Formula II).
In this instance, a readily accessible compound of Formula VIII, for example, where the A moiety is CH 2 , is converted to a compound of Formula II which, in turn, is converted to a compound of Formula IV which now can be used to synthesize a compound of Formula II which is difficultly accessible, i.e., wherein A is --CHF--, >C(CH 3 ) 2 , or >C(CH 2 ) 3 . ##STR10##
The first step (Step A) involves the esterification of compound of Formula VIII to produce the ester of Formula IX. The starting material, Formula VIII, is generally known; however, the synthesis of those which are not known or are accessible only by new methods will be discussed later. The esterification can be effected by many of the known methods. Especially useful is the procedure whereby compound of Formula VIII is reacted with an alkyl halide, such as methyl iodide, in the presence of an alkaline earth or alkali metal carbonate, such as potassium carbonate or sodium carbonate in the presence of a solvent such as dimethylformamide, 1-methylpyrrolidin-2-one, and the like to produce a compound of Formula IX. The reaction is generally conducted at a temperature of 30° C.-60° C. for from 3 to 20 hours. Alternatively, the esterification may be effected by the reaction of a compound of Formula VIII with an alkanol, such as methanol, ethanol or isopropyl alcohol in the presence of an acid catalyst. The acid catalyst may be a strong organic or inorganic acid, such as sulfuric acid, hydrochloric acid, p-toluenesulfonic acid and the like.
The second step (Step B) involves the reaction of a compound of Formula IX with methyl vinyl ketone to form a compound of Formula X. The conditions for this reaction are similar to those described above for the conversion of a compound of Formula V to one of Formula VI.
The third step (Step C) is the cyclization of compounds of Formula X to form those of Formula IC. The conditions for this reaction are similar to those described for the conversion of compounds of Formula VI to those of Formula VII.
The fourth step (Step D) is the hydrolysis of compounds of Formula IC to those of Formula II. The conditions of this reaction have been described earlier.
The final step (Step E) is the ether cleavage of a compound of Formula II to produce a compound of Formula IV. The conditions for this reaction are similar to those described for the conversion of a compound of Formula VII to those of Formula IV.
As indicated earlier, those compounds of Formula V and Formula VIII which are not known or are accessible only by new synthetic routes, may be prepared by methods disclosed in this invention which are illustrated below. ##STR11##
The first step is the etherification of a compound of Formula XI to produce a compound of Formula XII. This is accomplished by a reaction involving a compound of Formula XI in any one of a number of chemical processes; especially useful is dimethyl sulfate in the presence of potassium carbonate using a solvent, such as dimethylformamide.
The second step (Step B) is the conversion of a compound of Formula XII to one of Formula XIII. This can be accomplished by one or another of many methods; especially useful is the reaction of a compound of Formula XII with malonic acid in the presence of a solvent such as pyridine and a weak organic base, such as piperidine or pyrrolidine. The reaction is effected by heating for 1 to 6 hours at a temperature of 75° C. to 120° C., preferably at about 95° C. to 100° C. Quenching the reaction mixture in ice and acidification with a strong acid, such as hydrochloric acid yields the desired compound of Formula XIII.
The third step (Step C) involves the catalytic hydrogenation of a compound of Formula XIII to produce a compound of Formula XIV. The reduction is conducted in an atmosphere of hydrogen at an initial pressure of 10 to 100 psi and at temperatures of from 15° C. to 45° C. A solvent in which the starting material and product are reasonably soluble and which is inert to the reactants, product and catalyst is employed. Solvents such as tetrahydrofuran, dioxane, and the like are especially useful. The catalyst is usually a finely divided noble metal (which may be on an inert support) i.e., palladium on characoal or it may be a noble metal derivative which upon exposure to hydrogen is reduced to the free metal, i.e., platinum oxide. The fourth step (Step D) consists of the cyclization of a compound of Formula XIV to produce a compound of Formula XV. This is accomplished by first converting a compound of Formula XIV to the corresponding acid chloride using a reagent like thionyl chloride or phosphorus oxychloride. A solvent, such as benzene is advantageous. The acid chloride is subjected to the conditions of the Friedel-Crafts reaction which results in the cyclization of the acid chloride to form a compound of Formula XV. A reagent such as aluminum chloride, stannic chloride and the like are used to effect the cyclization. The reaction is conducted in a typical Friedel-Crafts solvent, such as methylene chloride or carbon disulfide. The reaction time is generally 1 to 6 hours.
The fifth step (Step E) involves the reduction of a compound of Formula XV to one of Formula XVI. This reaction is accomplished by using zinc amalgam and hydrochloric acid. The reaction is generally conducted in a solvent such as a mixture of water and an alkanol, such as ethanol or 1-propanol. The reaction time is generally between 3 and 10 hours and is generally conducted at temperatures of 60° C. to 110° C. The time and temperature are interdependent so that when the temperature is lower, the time is longer.
The sixth step (Step F) involves the oxidation of a compound of formula XVI to produce one of Formula XVII. The oxidation is best accomplished using a reagent such as chromium trioxide in a mixture of acetic acid and water. The reaction is advantageously conducted at ambient temperatures but temperatures somewhat higher or lower may be used.
The seventh step (Step G) consists of the alkylation of a compound of Formula XVII to produce one of Formula V. This first involves formation of the anion of a compound of Formula XVII by treatment with a base, such as an alkali metal alkoxide, for example, potassium tert.-butoxide in tert.-butyl alcohol. An alkali metal hydride, such as sodium hydride and the like, or an alkali metal amide, such as sodium amide, lithium amide and the like, also may be used. The anion is then treated with an alkylating agent, Alkyl-X. Solvents which are inert to the reactants may be employed. Suitable solvents are 1,2-dimethoxyethane, tert.-butyl alcohol, dimethylformamide, benzene and the like. The reaction is conducted at a temperature in the range from about 25° C. to about 150° C.
The eighth step (Step H) consists of the ether cleavage of a compound of Formula V to produce one of Formula XVIII. This reaction is carried out under conditions similar to those described earlier for the conversion of compounds of Formula VII to those of Formula IV.
The ninth step (Step I) consists of the etherification of a compound of Formula XVIII to one of Formula IX. This reaction is carried out under conditions described for the conversion of compounds of Formula IV to those of Formula IC.
Compound VIII may be prepared by one of two methods. The first method (Step J) involves the hydrolysis or pyrolysis of a compound of Formula IX to produce one of Formula VIII. This reaction is carried out by the methods described for the conversion of compounds of Formula IC or ID to those of Formula II.
The second method for the preparation of compounds of Formula VIII is the etherification of compounds of Formula XVIII. This reaction is carried out by the methods described for the conversion of compounds of Formula IV to those of Formula II.
As mentioned earlier, the compounds of this invention possess one and sometimes two or three asymmetric carbon atoms. In the instances where they possess two or three asymmetric carbon atoms, the reaction whereby these chiral centers are established can produce two or four diastereomers. These may be separated to obtain each pure diastereomer by methods well known to those skilled in the art, such as by fractional crystallization, column chromatography, high pressure liquid chromatography and the like.
Those compounds possessing only one asymmetric carbon atom, as well as each pure diastereomer from compounds possessing two or three asymmetric carbon atoms, consist of a racemate composed of two enantiomers. The resolution of the two enantiomers may be accomplished by forming a salt of the racemic mixture with an optically active base such as (+) or (-) amphetamine, (-) cinchonidine, dehydroabietylamine, (+) or (-)-α-methylbenzylamine, (+) or (-)-α-(1-naphthyl)ethylamine, (+) cinchonine, brucine, or strychnine and the like in a suitable solvent such as methanol, ethanol, 2-propanol, benzene, acetonitrile, nitromethane, acetone and the like. There is formed in the solution two diastereomeric salts one of which is usually less soluble in the solvent than the other. Repetitive recrystallization of the crystalline salt generally affords a pure diasteriomeric salt from which is obtained the desired pure enantiomer. The optically pure enantiomer of the [(5,6,9a-substituted-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]alkanoic cycloalkanoic acid is obtained by acidification of the salt with a mineral acid, isolation by filtration and recrystallization of the optically pure antipode.
The other optically pure antipode may generally be obtained by using a different base to form the diastereomeric salt. It is of advantage to isolate the partially resolved acid from the filtrates of the purification of the first diastereomeric salt and to further purify this substance through the use of another optically active base. It is especially advantageous to use an optically active base for the isolation of the second enantiomer which is the antipode of the base used for the isolation of the first enantiomer. For example, if (+)-α-methylbenzylamine was used first, then (-)-α-methyl-benzylamine is used for the isolation of the second (remaining) enantiomer.
The compounds of Formula I which are esters (i.e. compounds of Formula IC, where R 3 is lower alkyl, alkenyl, alkynyl, cycloalkyl, substituted alkyl, such as carboxyalkyl, alkoxycarbonylalkyl, hydroxyalkyl, carboxycycloalkyl, dihydroxyalkyl, trihydroxyalkyl, oxoalkyl, diloweralkylaminoalkyl, heterocyclic-alkyl, aralkyl and aryl) can be prepared by a variety of methods including one or more of the following seven methods.
The first method involves the etherification of compounds of Formula IV with a haloalkanoic acid ester or halocycloalkanoic acid ester such as, X-A-COOR 3 , where X is halo and A is defined previously to produce compounds of Formula IC. The reaction is illustrated graphically below: ##STR12##
In general, the reaction is conducted in the presence of a base, such as an alkali metal carbonate, hydroxide or alkoxide such as potassium carbonate, sodium carbonate, potassium hydroxide, sodium ethoxide and the like. Solvents which are essentially inert to the reactants and product and in which the reactants and product are reasonably soluble are usually employed. Dimethylformamide, ethanol and acetone, for example, have been found to be especially advantageous to use as solvents. The reaction may be conducted at a temperature in the range from about 25° C. to the boiling point temperature of the particular solvent employed. The reaction is generally complete in about 15 to 60 minutes; but, if lower temperatures are employed or if the particular halo ester is not very reactive, the reaction time may be much longer.
The second method for the synthesis of compounds of Formula IC involves the cyclization of compounds of Formula X to produce those of Formula IC. This method will be discussed later.
The third method for the preparation of compounds of Formula IC involves the esterification of compounds of Formula II. This may be accomplished by well known esterification methods such as those described for the conversion of compounds of Formula VIII to those of Formula IX (vide infra).
A fourth method involves a transesterification process as shown below. ##STR13## This involves heating an ester of Formula ID (where R 4 is selected from the same group as R 3 except it cannot be identical to R 3 in this reaction). The reaction proceeds successfully with a variety of alcohols (R 3 OH) and is generally carried out in the presence of a catalytic amount of R 3 OM where M is a sodium or potassium ion. The reaction is carried out in the presence of an ion-exchange resin, such as, amberlite and the like. Solvents, such as, methylene chloride, chloroform, carbon tetrachloride, are employed and the reaction is conducted at temperatures ranging from 30° C. to the boiling point of the solvent employed. The reaction time varies from 2 hours to one day.
A fifth method consists of the esterification of a salt of the corresponding carboxylic acid (II) with the appropriate alkyl or aralkyl halide (R 3 X) where X represents halogen. ##STR14##
The reaction is carried out in the presence of a base, such as, potassium carbonate, sodium carbonate and the like which generates the corresponding salt of the compound of Formula II. The reaction is generally carried out in the presence of a solvent such as, dimethylformamide, dimethylacetamide, N-methylpyrrolidinone and the like at temperatures usually in the range of 50° to 120° C. The reaction time varies from one to 24 hours depending on the temperature and the nature of the reactants.
A sixth method consists of the reaction of a mixed anhydride of Formula XIX with an appropriate alcohol R 3 OH. ##STR15##
The mixed anhydride is generally generated in situ from the corresponding carboxylic acid (Formula II) and ethyl chloroformate in tetrahydrofuran (or similar solvent) at a low temperature (such as, -10° C. to +10° C.) in the presence of an appropriate base (such as triethylamine and the like). The alcohol, R 3 OH, is added and the reaction mixture gradually increased to ambient temperature over a period of one to 5 hours and finally heated at 50° C. to the boiling point of the solvent for one to 6 hours.
The seventh method involves the reaction of a 1-acylimidazole derivative of Formula XX with an alcohol of Formula R 3 OH. ##STR16##
The acylimidazole (XX) is generally prepared in situ by the reaction of a Compound II with 1,1'-carbonyldiimidazole in a solvent (such as tetrahydrofuran, 1,4-dioxane and the like) at a temperature of -10° to +10° C. Reaction of the alcohol (R 3 OH) with XX is generally conducted in the presence of a catalytic amount of a base (such as sodium hydride, KOC(CH 3 ) 3 and the like). The reaction is generally carried out at temperatures between 0° C. and ambient temperature and requires from one to 24 hours for completion.
It should be pointed out that the R 3 moiety of the esters of Formula IC may possess a chemically reactive function which requires the presence of a chemical protective group during one or another of the seven synthetic methods described. These protective groups may be removed by one of several processes, such as selective hydrolysis, hydrogenolysis and the like.
The preparation of derivatives of the carboxylic acids (Formula II) of the invention are accomplished by methods well known by those skilled in the art. For example, an anhydride of Formula XXI is prepared from a compound of Formula II by reaction with a carbodiimide in an organic solvent. ##STR17##
For example, a compound of Formula II can be reacted with a carbodiimide, such as N,N'-dicyclohexylcarbodiimide or N,N'-di-p-tolylcarbodiimide in a solvent such as benzene, chlorobenzene, methylene chloride or dimethylformamide to produce a compound of Formula XXI.
The amide, hydrazide, guanidide and the like derivatives (Formula XXII) of compounds of the invention are prepared by methods well known to those skilled in the art. For example, a compound of Formula II is converted to the acylimidazole (XX) (described above) which, in turn, is treated with the appropriate base (R 4 R 5 NH) to obtain the desired derivative (Formula XXII). ##STR18## Thus, if R 4 R 5 NH represents ammonia or an amine, i.e., where R 4 and R 5 are hydrogen or lower alkyl, and the like, the product is an amide. If R 4 R 5 NH represents a hydrazide, i.e., R 4 is amino or dilower-alkylamino and R 5 is hydrogen or lower alkyl, the product is a hydrazide. If R 4 is ##STR19## and R 5 is hydrogen the product is guanidide.
The reactions described may be conducted in an excess of the reactant base as a solvent or one may use a conventional solvent, such as dimethylformamide, 1-methylpyrrolidin-2-one and the like.
The acid addition salts of Formula XXIII (where B + represents a cation from a pharmaceutically acceptable base) are prepared by reacting a carboxylic acid of Formula II with an appropriate alkali metal or alkaline earth bicarbonate, carbonate or alkoxide, an amine, ammonia, an organic quaternary ammonium hydroxide, guanidine and the like. The reaction is illustrated below: ##STR20##
The reaction is generally conducted in water but when alkali metal hyroxides and alkoxides and the organic bases are used, the reaction can be conducted in an organic solvent, such as ethanol, dimethylformamide and the like.
The preferred salts are the sodium, ammonium, diethanolamine, 1-methylpiperazine, piperazine and the like salts.
Inasmuch as there is a wide variety of symptoms and severity associated with grey matter edema, particularly when it is caused by blows to the head or spinal chord, the precise treatment protocol is left to the practitioner. It is up to the practitioner to determine the patient's response to treatment and to vary the dosages accordingly. A recommended dosage range is from 1 μg. to 10 mg./kg of body weight as a primary dose and a sustaining dose of half to equal the primary dose, every 4 to 24 hours.
The compounds of this invention can be administered by a variety of established methods, including intravenously, intramuscularly, subcutaneously, and orally. As with dosage, the precise mode of administration is left to the discretion of the practitioner.
Recent studies in experimental head injury by R. S. Bourke et. al. (R. S. Bourke, M. A. Daze and H. K. Kimelberg, Monograph of the International Glial Cell Symposium, Leige, Belgium, Aug. 29-31, 1977 and references cited therein) and experimental stroke by J. H. Garcia et al. (J. H. Garcia, H. Kalimo, Y. Kamijyo and B. F. Trump, Virchows Archiv. [Zellopath.], 25, 191 (1977), indicate that astroglial swelling, a secondary and potentially inhibitable process, is a fundamental pathophysiological response to ischemic/traumatic brain insult in both pathological disorders. Furthermore, astroglial swelling is believed to reduce oxygen available to neurons by prolongation of the oxygen diffusion pathaway. Thus, the damage to cerebral grey matter may be far more extensive as a result of pathological events secondary to astroglial swelling than as a result of damage inflicted by the initial ischemic/traumatic insult. Consequently, it is of prime importance that the treatment commence as soon as possible after the initial trauma in order to minimize the brain cell damage and the possibility of death or permanent paralysis.
One aspect of this invention is the treatment of persons with grey matter edema by concomitant administration of a compound of formula I, IC or II or a pharmaceutically acceptable salt, or amide thereof and an antiinflammatory steroid. These steroids are of some, albeit limited, use in control of white matter edema associated with ischemic stroke and head injury. Steroid therapy is given according to established practice as a supplement to the compound of formula I, IC or II as taught elsewhere herein.
The compounds of formula I, IC, or II are utilized by formulating them in a composition such as tablet, capsule or elixir for oral administration. Sterile solutions or suspensions can be used for parenteral administration. About 70 μg to 750 mg. of a compound or mixture of compounds of formulae I, IC, or II or a physiologically acceptable salt, or amide is compounded with a physiologically acceptable vehicle, carrier, excipient, binder, preservative, stabilizer, flavor, etc. in a unit dosage form as called for by accepted pharmaceutical practice. The amount of active substance in the composition is such that dosage in the range indicated is obtained.
Illustrative of the adjuvants which may be incorporated in tablets, capsules and the like are the following: a binder such as gum tragacanth, acacia, corn starch or gelatin; an excipient such as dicalcium phosphate; a disintegrating agent such as corn starch, potato starch, alginic acid and the like; a lubricant such as magnesium stearate; a sweetening agent such as sucrose, lactose, or saccharin; a flavoring agent such as peppermint, oil of wintergreen or cherry. When the dosage unit form is a capsule, it may contain in addition to materials of the above type a liquid carrier such as a fatty oil. Various other materials may be present as coatings or to otherwise enhance the pharmaceutical elegance of the preparation. For instance, tablets may be coated with shellac, sugar or the like. A syrup or elixir may contain the active compound, sucrose as a sweetening agent, methyl and propyl parabens as preservatives, a dye and a flavoring such as cherry or orange flavor.
Sterile compositions for injection can be formulated according to conventional pharmaceutical practice by dissolving or suspending the active substance in a conventional vehicle such as water for injection, a naturally occurring vegetable oil like sesame oil, coconut oil, peanut oil, cottonseed oil, etc., or a synthetic fatty vehicle like ethyl oleate or the like. Buffers, preservatives, antioxidants and the like can be incorporated as required.
The following examples are included to illustrate the preparation of representative dosage forms.
EXAMPLE 1
[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic Acid
Steps A and B. 5,6-Dichloro-9a-ethyl-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one
6,7-Dichloro-2-ethyl-5-methoxy-2,3-dihydro-1H-inden-1-one (32.4 gm., 0.125 mole) is dissolved in tetrahydrofuran (300 ml.) and 40% triton-B in methanol (3 ml.) is added. Methyl vinyl ketone (12.3 gm., 0.175 moles) is added dropwise to the stirring reaction mixture over a period of 10 minutes. The temperature rises from 26° C. to 35° C. The mixture is stirred for an additional hour and most of the volatile material is removed by evaporation in vacuo using a rotary evaporator.
Water (200 ml.) is added and the mixture extracted with ether (three 100 ml. portions). The combined ether extracts are dried over Na 2 SO 4 and then evaporated in vacuo to give a residual oil which is 6,7-dichloro-2-ethyl-5-methoxy-2-(3-oxobutyl)-2,3-dihydro-1H-inden-1-one. This material is dissolved in dry benzene (200 ml.), placed in a constant water separator (Dean-Stark), treated with acetic acid (1.5 ml.) and pyrrolidine (1.5 ml.). The mixture is refluxed for two hours after which time water ceases to separate. Then the solvent is distilled until only 50 ml. remains and then methanol (100 ml.) is added. Upon chilling in an ice bath, 5,6-dichloro-9a-ethyl-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (16.2 gm.) separates, m.p. 159°-165° C. This material is satisfactory for use in the next step.
Step C. 5,6-Dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one
5,6-Dichloro-9a-ethyl-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (15 gm., 0.048 mole) is mixed with pyridine hydrochloride (120 gm.) in a reaction vessel and heated in a metal bath at 195°-200° C. for 30 minutes. The mixture is cooled somewhat and poured with stirring into cold water (800 ml.). The solid that separates is removed by filtration and washed with water. After drying, the product is triturated with acetonitrile (80 ml.) at 60°, cooled, filtered and dried. The yield of crude 5,6-dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one is 12.2 gm., m.p. 260°-265° C. This material is pure enough for use in the next step.
Step D. Ethyl [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
A mixture of 5,6-dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (6.0 gm., 0.02 mole), ethyl bromoacetate (4.0 gm., 0.025 mole) and potassium carbonate (8.3 gm., 0.06 mole) in dimethyl-formamide (35 ml.) is heated at 50° C. and stirred for one hour. The mixture is cooled and poured into water (300 ml.). The solid product that separates is removed by filtration, then washed with water followed by benzene (10 ml.).
The yield of ethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate after drying, is 6.9 gm. After two recrystallizations from acetonitrile 4.8 gm. remains, m.p. 164°-166° C.
Step E. [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic Acid
Ethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (4.8 gm., 0.012 mole) is dissolved in acetic acid (30 ml.) containing 5% aqueous hydrochloride acid (10 ml.). The mixture is heated and stirred on a steam bath for an hour. The solution is diluted with water (8 ml.) and cooled. The product that separates is recrystallized twice from a 1:6 (v/v) mixture of water and acetic acid. The yield of [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetic acid is 2.6 gm., m.p. 237°-238° C.
Anal. Calcd. for C 17 H 16 Cl 2 O 4 : C, 57.48; H, 4.54. Found: C, 57.97; H, 4.43. C, 57.21; H, 4.29.
Using a procedure similar to that described in Example 1, except in Step A there is substituted for the 6,7-dichloro-2-ethyl-5-methoxy-2,3-dihydro-1H-inden-1-one an equimolar amount of:
EXAMPLE 2
Step A. 6,7-Dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one.
EXAMPLE 3
Step A. 6,7-Dichloro-5-methoxy-2-methyl-2,3-dihydro-1H-inden-1-one.
EXAMPLE 4
Step A. 6,7-Dichloro-5-methoxy-2-propyl-2,3-dihydro-1H-inden-1-one.
EXAMPLE 5
Step A. 6,7-Dichloro-2-isopropyl-5-methoxy-2,3-dihydro-1H-inden-1-one.
EXAMPLE 6
Step A. 2-Butyl-6,7-dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one.
EXAMPLE 7
Step A. 6,7-Dichloro-2-isobutyl-5-methoxy-23-dihydro-1H-inden-1-one.
EXAMPLE 8
Step A. 6,7-Dichloro-2-cyclopentyl-5-methoxy-2,3-dihydro-1H-inden-1-one.
EXAMPLE 9
Step A. 2-Benzyl-6,7-dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one.
EXAMPLE 10
Step A. 6,7-Dichloro-5-methoxy-2-phenyl-2,3-dihydro-1H-inden-1-one.
In Examples 2, Step A through Example 10, Step A, the reaction is carried out as described in Example 1, Step A, then by using each product and conducting the reaction as in Example 1, Step B, there is obtained:
EXAMPLE 2
Steps A and B: 6,7-Dichloro-5-methoxy-2-(3-oxobutyl)-2,3-dihydro-1H-inden-1-one and then 5,6-dichloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 3
Steps A and B. 6,7-Dichloro-5-methoxy-2-methyl-2-(3-oxobutyl)-2,3-dihydro-1H-inden-1-one and then 5,6-dichloro-7-methoxy-9a-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 4
Steps A and B. 6,7-Dichloro-5-methoxy-2-(3-oxobutyl)-2-propyl-2,3-dihydro-1H-inden-1-one and then 5,6-dichloro-7-methoxy-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 5
Steps A and B. 6,7-Dichloro-2-isopropyl-5-methoxy-2-(3-oxobutyl)-2,3-dihydro-1H-inden-1-one and then 5,6-dichloro-9a-isopropyl-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 6
Steps A and B. 2-Butyl-6,7-dichloro-5-methoxy-2-(3-oxobutyl)-2,3-dihydro-1H-inden-1-one and then 9a-butyl-5,6-dichloro-7-methoxy-1,2,9,9a-tetra-hydro-3H-fluoren-one.
EXAMPLE 7
Steps A and B. 6,7-Dichloro-2-isobutyl-5-methoxy-2-(3-oxobutyl)-2,3-dihydro-1H-inden-1-one and then 5,6-dichloro-9a-isobutyl-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 8
Steps A and B. 6,7-Dichloro-2-cyclopentyl-5-methoxy-2-(3-oxobutyl)-2,3-dihydro-1H-inden-1-one and then 5,6-dichloro-9a-cyclopentyl-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 9
Steps A and B. 2-Benzyl-6,7-dichloro-5-methoxy-2-(3-oxobutyl)-2,3-dihydro-1H-inden-1-one and then 9a-benzyl-5,6-dichloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 10
Steps A and B. 6,7-Dichloro-5-methoxy-2-(3-oxobutyl)-2-phenyl-2,3-dihydro-1H-inden-1-one and then 5,6-dichloro-7-methoxy-9a-phenyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
Carrying out the reaction as described in Example 1, Step C, except that the 5,6-dichloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one of Example 1, Step C is substituted by an equimolar quantity of the product of Example 2, Step B, Example 3, Step B, Example 4, Step B, Example 5, Step B, Example 6, Step B, Example 7, Step B, Example 8, Step B, Example 9, Step B, and Example 10, Step B to obtain:
EXAMPLE 2
Step C. 5,6-Dichloro-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 3
Step C. 5,6-Dichloro-7-hydroxy-9a-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 4
Step C. 5,6-Dichloro-7-hydroxy-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 5
Step C. 5,6-Dichloro-7-hydroxy-9a-isopropyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 6
Step C. 9a-Butyl-5,6-dichloro-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 7
Step C. 5,6-Dichloro-9a-isobutyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 8
Step C. 5,6-Dichloro-9a-cyclopentyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 9
Step C. 9a-Benzyl-5,6-dichloro-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 10
Step C. 5,6-Dichloro-7-hydroxy-9a-phenyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
Carrying out the reaction as described in Example 1, Step D, except that the 5,6-dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one of Example 1, Step D, is substituted by an equimolar quantity of the product of Example 2, Step C, Example 3, Step C, Example 4, Step C, Example 5, Step C, Example 6, Step C, Example 7, Step C, Example 8, Step C, Example 9, Step C or Example 10, Step C to obtain:
EXAMPLE 2
Step D. Ethyl [(5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 3
Step D. Ethyl [(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 4
Step D. Ethyl [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 5
Step D. Ethyl [(5,6-dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 6
Step D. Ethyl [(9a-butyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 7
Step D. Ethyl [(5,6-dichloro-9a-isobutyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 8
Step D. Ethyl [(5,6-dichloro-9a-cyclopentyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 9
Step D. Ethyl [(9a-benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 10
Step D. Ethyl [(5,6-dichloro-3-oxo-9a-phenyl1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
Carrying out the reaction as described in Example 1, Step E, except that the ethyl [(5,6-di-chloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren7-yl)oxy]acetate of Example 1, Step E is substituted by an equimolar quantity of the product of Example 2, Step D, Example 3, Step D, Example 4, Step D, Example 5, Step D, Example 6, Step D, Example 7, Step D, Example 8, Step D, Example 9, Step D or Example 10, Step D, there is obtained:
EXAMPLE 2
Step E. [(5,6-Dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 3
Step E. [(5,6-Dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 4
Step E. [(5,6-Dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 5
Step E. [(5,6-Dichloro-3-oxo-9a-isopropyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 6
Step E. [(9a-Butyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 7
Step E. [(5,6-Dichloro-9a-isobutyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 8
Step E. [(5,6-Dichloro-9a-cyclopentyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 9
Step E. [(9a-Benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 10
Step E. [(5,6-Dichloro-3-oxo-9a-phenyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
By carrying out the reaction as described in Example 1, Step D, except that the ethyl bromoacetate is substituted by an equimolar quantity of:
EXAMPLE 11
Step A. Ethyl 2-bromopropanoate.
EXAMPLE 12
Step A. Ethyl 2-bromobutyrate.
EXAMPLE 13
Step A. Ethyl 2-bromo-2-methylpropanoate.
EXAMPLE 14
Step A. Ethyl 1-bromocyclobutane-1-carboxylate.
There is obtained:
EXAMPLE 11
Step A. Ethyl 2-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]propanoate.
EXAMPLE 12
Step A. Ethyl 2-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]butyrate.
EXAMPLE 13
Step A. Ethyl 2-methyl-2-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-propanoate.
EXAMPLE 14
Step A. Ethyl 1-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]cyclobutane-1-carboxylate.
By carrying out the reaction as described in Example 1, Step D, except that the 5,6-dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one is substituted by 5,6-dichloro-7-hydroxy-9a-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (Example 3, Step C) and the ethyl bromoacetate substituted by Example 15, Step A: ethyl 2-bromo-2-methylpropanoate Example 16, Step A: ethyl 1-bromocyclobutane-1-carboxylate. There is obtained:
EXAMPLE 15
Step A. Ethyl 2-methyl-2-[(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]propanoate.
EXAMPLE 16
Step A. Ethyl 1-[(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]cyclobutane-1-carboxylate.
By carrying out the reaction as described in Example 1, Step E, except that the ethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate is substituted by the product of Example 11, Step A, Example 12, Step A, Example 13, Step A, Example 14, Step A, Example 15, Step A, or Example 16, Step A, whereby there is obtained:
EXAMPLE 11
Step B. 2-[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]propanoic acid.
EXAMPLE 12
Step B. 2-[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]butyric acid.
EXAMPLE 13
Step B. 2-Methyl-2-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-propanoic acid.
EXAMPLE 14
Step B. 1-[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]cyclobutane-1-carboxylic acid.
EXAMPLE 15
Step B. 2-Methyl-2-[(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]propanoic acid.
EXAMPLE 16
Step B. 1-[(5,6-Dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]cyclobutane-1-carboxylic acid.
EXAMPLE 17
3-[(5,6-Dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]propanoic acid
5,6-Dichloro-7-hydroxy-9a-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (9.0 gm., 0.03 mole) is dissolved in 10% aqueous sodium hydroxide solution (35 ml.). The solution is heated to boiling with stirring, the heat source is removed and β-propiolactone (23.8 gm., 0.33 mole) is added at such a rate to keep the solution boiling. During the reaction, 10% aqueous sodium hydroxide is added as necessary to keep the reaction mixture alkaline to litmus paper.
When the reaction is complete, the solution is cooled and made acid to Congo red paper with 6 normal hydrochloric acid. The product that separates is removed by filtration and dissolved by treatment with a 5% solution of sodium hydroxide (three 50 ml. portions). The combined aqueous extracts are acidified to Congo red paper with 6 normal hydrochloric acid. The product is removed by filtration, washed with water and dried. Recrystallization from a mixture of acetic acid and water gives pure 3-[(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]propanoic acid.
Carrying out the reaction as described in Example 17 except that the 5,6-dichloro-9a-methyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one is substituted by an equimolar quantity of:
EXAMPLE 18
5,6-Dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
EXAMPLE 19
5,6-Dichloro-7-hydroxy-9a-isopropyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one. There is obtained:
EXAMPLE 18
3-[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]propanoic acid.
EXAMPLE 19
3-[(5,6-Dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]propanoic acid.
EXAMPLE 20
[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Step A. Methyl [(6,7-dichloro-2-ethyl-1-oxo-2,3,-dihydro-1H-inden-5-yl)oxy]acetate
[(6,7-Dichloro-2-ethyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetic acid (31.7 gm. 0.1 mole) is dissolved in dimethylformamide (300 ml.) and potassium carbonate (20.7 gm., 0.15 mole) is added. The mixture is stirred and heated at 60° C. for 10 minutes in a vessel protected from atmospheric moisture. Methyl iodide (12.6 ml., 28.4 gm., 0.2 mole) is added and heating and stirring continued for 3 hours. The mixture is cooled, added, with stirring to water (3 liters) and the solid that separated removed by filtration and dried. Recrystallization from methanol gives 27 gm. of methyl [(6,7-dichloro-2-ethyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
Step B. Methyl{[6,7-dichloro-2-ethyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}-acetate
Methyl [(6,7-dichloro-2-ethyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate (15.8 gm., 0.05 mole) is suspended in dry tetrahydrofuran (100 ml.) containing triton-B (1 ml.). The suspension is stirred at ambient temperature and methyl vinyl ketone (5.02 gm., 0.072 mole) is added. The solution which becomes warm initially, is stirred at ambient temperature for 4 hours. Then, the stirring solution is treated with methyl vinyl ketone (0.3 ml.) and triton-B (0.6 ml.) every 4 hours for the next twenty hours.
The reaction mixture is evaporated in vacuo at 50° C. and the residual material dissolved in ether (100 ml.). The ether solution is washed with water (two 20 ml. portions), dried over anhydrous magnesium sulfate and filtered. The filtrate is evaporated in vacuo and the residue triturated with ether (10 ml.), filtered and dried. The yield of methyl {[6,7-dichloro-2-ethyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}acetate is 12.3 gm., m.p. 78°-79° C. This material is adequate for use in the next step.
Step C. Methyl [(5,6-dichloro-9a -ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
A mixture of methyl {[6,7-dichloro-2-ethyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}acetate (9.0 gm., 0.024 mole), pyrrolidine (1.70 gm., 0.024 mole) and acetic acid (1.42 gm., 0.024 mole) in toluene (100 ml.) is heated at 85° C. for one hour. The solution is concentrated in vacuo at 50° C. to obtain the crude product.
The product is subjected to column chromatography on silica gel (300 gm.) using a mixture of dichloromethane and tetrahydrofuran (100/4 v./v.) as the eluent. The yield of pure methyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetate is 5.05 gm., m.p. 182°-183° C.
Step D. [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Methyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (4.0 gm., 0.011 mole) is added to a solution composed of 20% aqueous sodium hydroxide solution (4.32 ml., 0.022 mole) and methanol (45 ml.). The mixture is stirred and heated at reflux for two hours and then concentrated in vacuo at 50° C. The residue is dissolved in water (50 ml.) and made acid to Congo red paper with 6 normal hydrochloric acid. The solid that separates is removed by filtration, washed with water, then with a little methanol and finally with a little ether. After drying, the product weighs 3.14 gm., m.p. 235° C. After recrystallization from acetic acid, the yield of pure [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid is 2.61 gm., m.p. 237°-239° C.
Anal. Calcd. for C 17 H 16 Cl 2 O 4 : C, 57.48; H, 4.54. Found: C, 57.35; H, 4.62.
Carrying out the reaction as described in Example 20, Step A, except that the [(6,7-dichloro-2-ethyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetic acid is substituted by an equimolar quantity of:
EXAMPLE 21
Step A. [(6,7-Dichloro-1-oxo-2-propyl-2,3,-dihydro-1H-inden-5yl)oxy]acetic acid.
EXAMPLE 22
Step A. [(2-Butyl-6,7-dichloro-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetic acid.
EXAMPLE 23
Step A. [(2-Ethyl-6,7-dimethyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetic acid.
EXAMPLE 24
Step A. [(2-Ethyl-1-oxo-2,3,-dihydro-1H-benz[e]inden-5-yl)oxy]acetic acid. There is obtained.
EXAMPLE 21
Step A. Methyl [(6,7-dichloro-1-oxo-2-propyl-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
EXAMPLE 22
Step A. Methyl [(2-Butyl-6,7-dichloro-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
EXAMPLE 23
Step A. Methyl [(2-ethyl-6,7-dimethyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
EXAMPLE 24
Step A. Methyl [(2-ethyl-1-oxo-2,3-dihydro-1H-benz[e]inden-5-yl)oxy]acetate.
Carrying out the reaction as described in Example 20, Step B, except that the methyl [(6,7-dichloro-2-ethyl-1-oxo-2,3-dihydro-1H-inden-5-yl)-oxy]acetate is substituted by an equimolar quantity of the product of Example 21, Step A, Example 22, Step A, Example 23, Step A or Example 24, Step A. There is obtained:
EXAMPLE 21
Step B. Methyl {[6,7-dichloro-2-propyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}-acetate, m.p., 91°-93° C.
EXAMPLE 22
Step B. Methyl {[6,7-dichloro-2-butyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}acetate, m.p. 92°-93° C.
EXAMPLE 23
Step B. Methyl {[2-ethyl-6,7-dimethyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}-acetate.
EXAMPLE 24
Step B. Methyl {[2-ethyl-1-oxo-2-(3-oxo-butyl)-2,3-dihydro-1H-benz[e]inden-5-yl]oxy}acetate.
Carrying out the reaction as described in Example 20, Step C, except that the methyl {[6,7-di-chloro-2-ethyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}acetate is substituted by an equimolar quantity of the product of Example 21, Step B, Example 22, Step B, Example 23, Step B, or Example 24, Step B, there is obtained:
EXAMPLE 21
Step C. Methyl [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate, m.p. 158°-159° C.
EXAMPLE 22
Step C. Methyl [(9a-butyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate, 153.5°-154° C.
EXAMPLE 23
Step C. Methyl [(9a-ethyl-5,6-dimethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 24
Step C. Methyl [(7a-ethyl-10-oxo-7,7a,8,9-tetrahydro-10H- benzo[c]fluoren-5-yl)oxy]acetate.
Carrying out the reaction as described in Example 20, Step D, except that the methyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate is substituted by an equimolar quantity of the product of Example 21, Step C, Example 22, Step C, Example 23, Step C or Example 24, Step C. There is obtained:
EXAMPLE 21
Step D. [(5,6-Dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 22
Step D. [(9a-Butyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 23
Step D. [(9a-Ethyl-5,6-dimethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 24
Step D. [(7a-Ethyl-10-oxo-7,7a,8,9-tetrahydro-10H-benzo[c]fluoren-5-yl)oxy]acetic acid.
EXAMPLE 25
[(5,6-Dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Step A. Methyl [(6,7-dichloro-2-isopropyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate
[(6,7-Dichloro-2-isopropyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetic acid 33.4 gm. 0.1 mole) is dissolved in dimethylformamide (300 ml.) and potassium carbonate (20.7 gm., 0.15 mole) is added. The mixture is stirred and heated at 60° C. for 10 minutes in a vessel protected from atmospheric moisture. Methyl iodide (12.6 ml., 28.4 gm., 0.2 mole) is added and heating and stirring continued for 3 hours. The mixture is cooled, added, with stirring to water (3 liters) and the solid that separated removed by filtration and dried. Recrystallization from methanol gives methyl [(6,7-dichloro-2-isopropyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
Step B. Methyl {[6,7-dichloro-2-isopropyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}acetate
Methyl [(6,7-dichloro-2-isopropyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate (16.5 gm., 0.05 mole) is suspended in dry tetrahydrofuran (100 ml.) containing triton-B (1 ml.). The suspension is stirred at ambient temperature and methyl vinyl ketone (5.02 gm., 0.072 mole) is added. The solution which becomes warm initially, is stirred at ambient temperature for 4 hours. Then, the stirring solution is treated with methyl vinyl ketone (0.3 ml.) and triton-B (0.6 ml.) every 4 hours for the next twenty hours.
The reaction mixture is evaporated in vacuo at 50° C. and the residual material dissolved in ether (100 ml.). The ether solution is washed with (two 20 ml. portions), dried over anhydrous magnesium sulfate and filtered. The filtrate is evaporated in vacuo and the residue triturated with ether (10 ml.), filtered and dried. The product is methyl [6,7-dichloro-2-isopropyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy acetate.
Step C. Methyl [(5,6-dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-floren-7-yl)oxy]acetate
A mixture of methyl [(6,7-dichloro-2-isopropyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl)oxy]-acetate (9.3 gm., 0.024 mole), potassium tert.-butoxide (2.70 gm., 0.024 mole) and tert.-butyl alcohol (100 ml.) is heated at 85° C. for three hours. The solution is concentrated in vacuo at 50° C. to obtain the crude product.
The product is subjected to column chromatography on silica gel (300 gm.) using a mixture of dichloromethane and tetrahydrofuran (100/4 v./v.) as the eluent. The product is pure methyl [(5,6-dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetate.
Step D. [(5,6-Dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Methyl [(5,6-dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7yl)oxy]acetate (4.2 gm., 0.011 mole) is added to a solution composed of 20% aqueous sodium hydroxide solution (4.32 ml., 0.022 mole) and methanol (45 ml.). The mixture is stirred and heated at reflux for two hours and then concentrated in vacuo at 50° C. The residue is dissolved in water (50 ml.) and made acid to Congo red paper with 6 normal hydrochloric acid. The solid that separates is removed by filtration, washed with water, then with a little methanol and finally with a little ether. After drying, the product is recrystallized from acetic acid to give pure [(5,6-dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3Hfluoren-7-yl)oxy]acetic acid. Using a procedure similar to that described in Example 25, except that in Step A there is substituted for the [(6,7-dichloro-2-isopropyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetic acid, an equimolar amount of:
EXAMPLE 26
Step A. [(6,7-Dichloro-2-cyclopentyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetic acid.
EXAMPLE 27
Step A. [(6,7-Dichloro-1-oxo-2-phenyl-2,3-dihydro-1H-inden-5-yl)oxy]acetic acid.
EXAMPLE 28
Step A. [(2-Benzyl-6,7-dichloro-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetic acid.
In Examples 26, Step A through 28, Step A, the reaction is carried out as described in Example 25, Step A, there is obtained:
EXAMPLE 26
Step A. Methyl [(6,7-dichloro-2-cyclopentyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
EXAMPLE 27
Step A. Methyl [(6,7-dichloro-1-oxo-2-phenyl-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
EXAMPLE 28
Step A. Methyl [(2-benzyl-6,7-dichloro-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
In Example 25, Step B, the starting material is the product from Step A. Using the products from step A of Example 26, 27 and 28 as starting materials but conducting the reaction as in Example 25, Step B, there is obtained:
EXAMPLE 26
Step B: Methyl {[[6,7-dichloro-2-cyclopentyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}acetate
EXAMPLE 27
Step B: Methyl {[6,7-dichloro-1-oxo-2-(3-oxobutyl)-2-phenyl-2,3-dihydro-1H-inden-5-yl]oxy}acetate.
EXAMPLE 28
Step B. Methyl {[2-benzyl-6,7-dichloro-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}acetate.
Using the products from Step B of Example 26, 27, 28 as starting material in place for the Example 25, Step B, and conducting the reaction as in Example 25, Step C there is obtained:
EXAMPLE 26
Step C. Methyl [(5,6-dichloro-9a-cyclopentyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 27 p Step C. Methyl [(5,6-dichloro-3-oxo-9a-phenyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 28
Step C: Methyl [(9a-benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 28
Step C: Methyl [(9a-benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
Using the products from Step C of Examples 26, 27 and 28 as starting materials in place of the product from Example 25, Step C and conducting the reaction as in Example 25, Step D, there is obtained:
EXAMPLE 26
Step D. [(5,6-Dichloro-9a-cyclopentyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 27
Step D. [(5,6-Dichloro-3-oxo-9a-phenyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 28
Step D. [(9a-Benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 29
[(5,6-Dichloro-3-oxo-2-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetic acid.
Step A. Methyl [(6,7-dichloro-2-ethylidene-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate
[(6,7-Dichloro-2-ethylidene-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetic acid (U.S. Pat. No. 3,704,314) (30.1 gm., 0.1 mole) is dissolved in methanol (150 ml.) and conc. sulfuric acid (0.5 ml.) added. The mixture is stirred and refluxed for 2 hours. The solvent is removed in vacuo by evaporation on a rotary evaporator and the residue dissolved in ethyl ether, washed with water and dried over sodium sulfate. The ether is removed by evaporation in vacuo in a rotary evaporator to give methyl[(6,7-dichloro-2-ethylidene-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
Step B. Methyl [6,7-dichloro-1-oxo-2-(3-oxo-butyl)-2-vinyl-2,3-dihydro-1H-inden-5-yl]oxy acetate.
Methyl (6,7-dichloro-2-ethylidene-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate (25.4 gm., 0.08 mole) is dissolved in 1,2-dimethoxyethane (350 ml.) which had been boiled and cooled under dry nitrogen. Maintaining an atmosphere of dry nitrogen, the solution is cooled to 0° C. and potassium tert.-butoxide (900 mg., 0.008 mole) is added. Keeping the temperature at 0°, methyl vinyl ketone (11.2 gm., 0.16 mole) is added with stirring over 30 minutes. After stirring 2 hours at 0° C., the reaction mixture is allowed to warm to ambient temperature overnight. The solvent is removed in vacuo in a rotary evaporator, and the residue dissolved in ether, washed with water and dried over anhydrous magnesium sulfate. Evaporation of the ether in vacuo gave methyl [6,7-dichloro-1-oxo-2-(3-oxobutyl)-2-vinyl-2,3-dihydro-1H-inden-5-yl]oxy acetate.
Step C. Methyl [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
A mixture of methyl {[6,7-dichloro-1-oxo-(3-oxobutyl)-2-vinyl-2,3-dihydro-1H-inden-5-yl]oxy}-acetate (9.0 gm., 0.024 mole), pyrrolidine (1.70 gm., 0.024 mole) and acetic acid (1.42 gm., 0.024 mole) in toluene (100 ml.) is heated at 85° C. for one hour. The solution is concentrated in vacuo at 50° C. to obtain the crude product.
The product is subjected to column chromatography on silica gel (300 gm.) using a mixture of dichloromethane and tetrahydrofuran (100/4 v./v.) as the eluent. The product is methyl [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetate.
Step D. [(5,6-Dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Methyl [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (4.0 gm., 0.011 mole) is added to a solution composed of 20% aqueous sodium hydroxide solution (4.32 ml., 0.022 mole) and methanol (45 ml.). The mixture is stirred and heated at reflux for two hours and then concentrated in vacuo at 50° C. The residue is dissolved in water (50 ml.) and made acid to Congo red paper with 6 normal hydrochloric acid. The solid that separates is removed by filtration, washed with water, then with a little methanol and finally with a little ether. After recrystallization from acetic acid, there is obtained pure [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
Alternatively, [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid may be produced by the following process.
Methyl {[6,7-dichloro-1-oxo-2-(3-oxobutyl)-2-vinyl-2,3-dihydro-1H-inden-5-yl]oxy}acetate (7.3 gm., 0.02 mole) is dissolved in a solution of methanol (100 ml) and water (50 ml.) containing sodium hydroxide (9.43 gm., 0.236 mole), taking care to keep the temperature below 25° C. The solution is kept at ambient temperature for 48 hours. The solution is concentrated in vacuo to 100 ml. in a rotary evaporator at room temperature and poured into water (250 ml.) containing concentrated hydrochloric acid (26 ml.) with cooling. The product is separated by filtration, washed with water, dried and recrystallized from a mixture of acetic acid and water to obtain [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 30
[(5,6-Dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
Step A. Ethyl [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
A solution of [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl-oxy]acetic acid (Example 29, Step D) (8.82 g., 0.025 mole) absolute ethanol (300 ml) and 12 N HCl (5 ml) in ethanol (20 ml) is heated under reflux on the steam bath with stirriing for an hour. The excess solvent is removed under reduced pressure. Ice and water are added to the oily residue and the product extracted into methylene chloride. After drying over MgSO 4 , the solution is concentrated to yield the product.
Recrystallization from tetrahydrofuran-etherpetroleum ether (1:1:2) gives ethyl [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
Step B. Ethyl [(5,6-Dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
To a hot, rapidly stirred solution of cupric acetate monohydrate (7.0 gm., 0.02 mole) in glacial acetic acid is added zinc dust (70 gm., 1.08 gm. atom). After about 30 seconds, all the copper has deposited on the zinc. The couple is allowed to settle for 0.5 to 1 minute, then as much as possible of the acetic acid is decanted, care being taken not to lose the silt-like couple. The dark reddish-gray couple is then washed with one 100 ml. portion of acetic acid followed by three 200 ml. portions of tetrahydrofuran.
A mixture of the zinc-copper couple, prepared as described above, (48 gm.) and methylene iodide (37.5 gm.) in tetrahydrofuran (300 ml.) is heated under reflux in a nitrogen atmosphere for an hour. Ethyl [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetate (8.2 gm., 0.02 mole) is added to the cooled mixture and stirring continued at 25° C. for 24 hours. The mixture is diluted with toluene (200 ml.), filtered and the filtrate is washed successively with saturated aqueous solutions of ammonium chloride and sodium bicarbonate and then with water. The organic lager is dried over anhydrous magnesium sulfate and the solvent removed using a rotary evaporator at reduced pressure. The residue is purified by column chromatography using a silica-gel column to give ethyl [(5,6-dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetate.
Step C. [(5,6-Dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Ethyl [(5,6-dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7yl)oxy]acetate (4.2 gm., 0.011 mole) is added to a solution composed of 20% aqueous sodium hydroxide solution (4.32 ml., 0.022 mole) and methanol (45 ml.). The mixture is stirred and heated at reflux for two hours and then concentrated in vacuo at 50° C. The residue is dissolved in water (50 ml.) and made acid to Congo red paper with 6 normal hydrochloric acid. The solid that separates is removed by filtration, washed with water, then with a little methanol and finally with a little ether. After drying, the product is recrystallized from acetic acid to give pure [(5,6-dichloro-3-oxo-9a-cyclopropyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 31
Resolution of [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Step A. A mixture of racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid (7.1 gm., 0.02 mole) and dextro(+)cinchonine (5.89 gm., 0.02 mole) is dissolved in the minimum volume of boiling acetonitrile, is cooled to 5° C. and aged for 48 hours. The crystalline product is removed by filtration and recrystallized twice from the minimum volume of acetonitrile. (The mother liquors from each recrystallization are combined and saved).
The pure salt is suspended in water (40 ml.) treated with 6 normal hydrochloric acid (5 ml.) and the precipitate that forms is removed by filtration and dried. This pure (+) enantiomer of [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetic is then recrystallized from a mixture of tetrahydrofuran and ethyl ether, m.p. 238°-240° C.;
α 23 ° 589 (C=1.1), +151.2.
Step B. The combined acetonitrile mother liquors from Step A are evaporated at reduced pressure and the residue treated with water (50 ml.) and 6 normal hydrochloric acid (7.5 ml.). The resulting precipitate is removed by filtration and dried.
This residual partially resolved [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (2.86 gm., 0.0118 mole) is treated with 1(-)cinchonidine (3.47 gm., 0.0118 mole) and the mixture dissolved in the minimum quantity of acetonitrile. After cooling for 48 hours, the salt that separates is removed by filtration and recrystallized twice from the minimum volume of acetonitrile. The pure salt is suspended in water (50 ml), treated with 6 normal hydrochloric acid (5 ml) and the precipitate that separates is removed by filtration and dried. This solid is recrystallized from a mixture of tetrahydrofuran and ethyl ether to give the (-) enantiomer of [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid, m.p. 239°-241° C., α 23 ° 589 (C=1.1)=-151.2°.
EXAMPLE 32
Steps A and B. The Two Enantiomers of [(9a-butyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out the resolution as described in Example 31 except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid (Example 1, Step E) is substituted by an equimolar quantity of racemic [(9a-butyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 6, Step E), there is obtained the two enantiomers of [(9a-butyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 33
Steps A and B. The Two Enantiomers of [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out the resolution as described in Example 31, except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid is replaced by an equimolar quantity of racemic [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 47, Step L) there is obtained the two enantiomers of [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9α-tetrahydro-3H-fluoren-7-yl)-oxo]acetic acid.
EXAMPLE 34
Steps A and B. The two Enantiomers of [(5,6-dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetrahydro-3H-7-yl)oxy]acetic acid
Carrying out the resolution as described in Example 31, except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid is replaced by an equimolar quantity of racemic [(5,6-dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 48, Step L), there is obtained the two enantiomers of [(5,6-dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 35
Steps A and B. The two enantiomers of [(5,6-dichloro-9a-cyclopropylmethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
Carrying out the resolution as described in Example 31, except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 1, Step E) is substituted by an equimolar quantity of racemic [(5,6-dichloro-9a-cyclopropylmethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 50, Step L), there is obtained the two enantiomers of [(5,6-dichloro-9a-cyclopropylmethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 36
Steps A and B. The two enantiomers of [(9a-benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out a reaction as described in Example 31, except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 1, Step E) is substituted by an equimolar quantity of racemic [(9a-benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 9, Step E), there is obtained the two enantiomers of [(9a-benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetic acid.
EXAMPLE 37
Steps A and B. The two enantiomers of [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out the resolution as described in Example 31, except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid is substituted by an equimolar quantity of [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 4, Step E) there is obtained the two enantiomers of [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 38
Steps A and B. The two enantiomers of [(5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid
Carrying out the resolution as described in Example 31, except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid is replaced by an equimolar quantity of racemic [(5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetic acid (Example 2, Step E), there is obtained the two enantiomers of [(5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 39
Steps A and B. The two enantiomers of [(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out the resolution as descrived in Example 31, except that the reacemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid is replaced by an equimolar quantity of racemic [(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 3, Step E), there is obtained the two enantiomers of [(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 40
Steps A and B. The two Enantiomers of [(5,6-dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out the resolution as described in Example 31, except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid is replaced by an equimolar quantity of racemic [(5,6-dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 25, Step D), there is obtained the two enantiomers of [(5,6-dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetic acid.
EXAMPLE 41
Steps A and B. The two enantiomers of [(5,6-dichloro-9a-cyclopentyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out the resolution as described in Example 31, except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid is replaced by an equimolar quantity of racemic [(5,6-dichloro-9a-cyclopentyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 26, Step D), there is obtained the two enantiomers of [(5,6-dichloro-9a-cyclopentyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid.
EXAMPLE 42
Steps A and B. The two enantiomers of [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out the resolution as described in Example 31, except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid is replaced by an equimolar quantity of racemic [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 29, Step D), there is obtained the two enantiomers of [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid.
EXAMPLE 43
Steps A and B. The two enantiomers of [(5,6-dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out the resolution as described in Example 31, except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid is replaced by an equimolar quantity of racemic [(5,6-dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 30, Step D), there is obtained the two enantiomers of [(5,6-dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 44
Steps A and B. The two enantiomers of [(5,6-dichloro-3-oxo-9a-phenyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out the resolution as described in Example 31, except that the racemic [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid is replaced by an equimolar quantity of racemic [(5,6-dichloro-3-oxo-9a-phenyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 27, Step D), there is obtained the two enantiomers of [(5,6-dichloro-3-oxo-9a-phenyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 45
1-[(5,6-Dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]cyclopentane-1-carboxylic acid
Step A. 5,6-Dichloro-7-hydroxy-9a-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one
Carrying out a reaction as described in example 1, Step C, except that the 5,6-dichloro-9a-ethyl-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one is replaced by an equimolar quantity of [(5,6-dichloro-oxy]acetic acid (Example 3, Step E), there is obtained 5,6-dichloro-7-hydroxy-9a-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one.
Step B. Ethyl 1-[(5,6-Dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]cyclopentane-1-carboxylate
Carrying out a reaction as described in Example 1, Step D, except that the 5,6-dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one and ethyl bromoacetate are replaced by equimolar quantities of 5,6-dichloro-7-hydroxy-9a-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one and ethyl 1-bromocyclopentane-1-carboxylate, there is obtained ethyl 1-[(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]cyclopentane-1-carboxylate.
Step C. 1-[(5,6-Dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]cyclopentane-1-carboxylic acid
Carrying out a reaction as described in Example 1, Step E, except that the ethyl [(5,6-dichloro-9a-ethyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate is replaced by an equimolar quantity of ethyl 1-[(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]cyclopentane-1-carboxylate, to give 1-[(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]cyclopentane-1-carboxylic acid.
EXAMPLE 46
Fluoro[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Step A. 5,6-Dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one
Carrying out a reaction as described in Example 1, Step C, except that the 5,6-dichloro-9a-ethyl-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one is replaced by an equimolar quantity of [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 20, Step D), there is obtained 5,6-dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-fluoren-3-one.
Step B. Ethyl fluoro[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
Carrying out a reaction as described in Example 1, Step D, except that the ethyl bromoacetate is replaced by an equimolar quantity of ethyl bromofluoroacetate, there is obtained ethyl fluoro[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
Step C. Fluoro[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Ethyl fluoro[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (4.01 gm., 0.02 mole) is dissolved in ethanol (75 ml.) and treated with a solution of sodium bicarbonate (3.36 gm., 0.04 mole) in water (150 ml.). The mixture is heated and stirred on a steam bath for 15 minutes and then concentrated in vacuo to a volume of 50 ml. The residual solution is diluted with water (50 ml.) and acidified to Congo red test paper with 6 normal hydrochloric acid. The precipitate that forms is removed by filtration, washed with water and dried. The product is sufficiently pure for use but it may be further purified by recrystallization from a mixture of acetic acid and water to produce pure fluoro[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 47
[(9a-Allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Step A. 2,3-Dichloro-4-methoxybenzaldehyde
A mixture of 2,3-dichloro-4-hydroxybenzaldehyde (19.1 gm., ;b 0.1 mole) and potassium carbonate (34.4 gm., 0.25 mole) in dimethylformamide (50 ml.) is stirred and treated dropwise over 15 minutes with dimethyl sulfate (14.1 gm., 0.11 mole). The reaction is exothermic; after 45 minutes the mixture is poured with stirring into water (300 ml.). The solid product that separates is removed by filtration, washed with water and then washed with a little methanol. After drying the yield of 2,3-dichloro-4-methoxybenzaldehyde is 16 gm., m.p., 117°-118° C.
Step B. 2,3-Dichloro-4-methoxycinnamic acid
A mixture of 2,3-dichloro-4-methoxybenzaldehyde (158 gm., 0.77 mole), malonic acid (146 gm., 1.4 mole), pyridine (450 ml.) and piperidine (15 ml.) is heated and stirred on a steam bath for 23/4 hours. The hot reaction mixture is poured, with stirring into a mixture of concentrated hydrochloric acid (770 ml.) and crushed ice (3.1 kg.).
The solid that separates is removed by filtration, then washed, first with water and then with a little methanol. After drying, the solid is dissolved in a solution containing sodium hydroxide (61.6 gm.) and water (7.7 liters). The insoluble material is removed by filtration and the filtrate acidified with concentrated hydrochloric acid.
The solid 2,3-dichloro-4-methoxycinnamic acid that separates is removed by filtration, washed with water and dried. The yield is 179 gm. (96%), m.p. 246°-249° C. This crude material is adequate for use in the next step.
Step C. 3-(2,3-Dichloro-4-methoxyphenyl)-propanoic acid
2,3-Dichloro-4-methoxycinnamic acid (200.8 g., 0.813 mole) is dissolved in tetrahydrofuran (1600 ml.) and 5% platinum on charcoal (16.3 gm.) is added. The mixture is divided into 8 separate units and each is placed in a Parr hydrogenation apparatus in an atmosphere of hydrogen at an initial pressure of 50 p.s.i. Upon shaking, the time required for the reduction of each batch is 35 to 60 minutes.
The combined reaction mixtures are filtered and the solvent removed by distillation at reduced pressure to give crude 3-(2,3-dichloro-4-methoxyphenyl)propanoic acid, 176.3 gm., m.p. 141°-143° C. The material is adequate for use in the next step.
Step D. 4,5-Dichloro-6-methoxy-2,3-dihydro-1H-inden-1-one
3-(2,3-Dichloro-4-methoxyphenyl)propanoic acid (176.3 gm., 0.708 mole) is placed in benzene (500 ml.) and thionyl chloride (101.8 ml., 1.42 mole) is added. The mixture is refluxed for 11/2 hours and the volatile materials removed by distillation at reduced pressure. The residual oil is dissolved in benzene (50 ml.) and the solvent again removed at reduced pressure. This process is repeated and the residue is dissolved in dry methylene chloride (500 ml.).
The solution is placed in a flask protected from atmospheric moisture by a calcium chloride drying tube and cooled via an ice bath. Then aluminum chloride (94.4 gm., 0.708 mole) is added portionwise via a vessel attached to the reaction flask by Gooch rubber tubing. After the addition is complete, the cooling bath is removed and stirring at ambient temperature is continued for 3 hours.
The reaction mixture is poured, with stirring into ice water (1635 ml.) containing concentrated hydrochloric acid (218 ml.). The solid that separates is collected by filtration, washed with water and dried. The yield is 160 gm. This material is recrystallized (while treating with decolorizing charcoal) from acetonitrile to give 4,5-dichloro-6-methoxy-2,3-dihydro-1H-inden-1-one, 129.1 gm., m.p. 163°-165°.
Step E. 4,5-Dichloro-6-methoxy-2,3-dihydro-1H-indene
An amalgam of zinc, prepared from zinc (65 gm.) and mercuric chloride (3.5 gm.), is stirred with a mixture of water (20 ml.), ethanol (20 ml.) and concentrated hydrochloric acid (50 ml.). The mixture is heated to boiling and a slurry of 4,5-dichloro-6-methoxy-2,3-dihydro-1H-inden-1-one (23.1 gm., 0.1 mole) in a mixture of hot ethanol (150 ml.), water (20 ml.) and concentrated hydrochloric acid (50 ml.) is added over 15 minutes. Then the boiling mixture is treated with concentrated hydrochloric acid (50 ml.) over an hour. Boiling and stirring is continued for 5 hours longer and then the stirring is terminated and the mixture is cooled. The liquid portion is separated by decantation and concentrated to half its volume in vacuo. The solid portion of the reaction mixture is extracted with ether (four 50 ml. portions). The combined ether extracts and liquid portion of the reaction mixture are united in a separatory funnel and water (250 ml.) is added. The mixture is thoroughly shaken and the ether layer separated, washed with water, then with brine and finally dried over anhydrous magnesium sulfate. Evaporation of the ether gives 15.2 g. of crude 4,5-dichloro-6-methoxy-2,3-dihydro-1H-indene, m.p. 78°-82° C. This material is adequate for use in the next step.
Step F. 6,7-Dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one
4,5-Dichloro-6-methoxy-2,3-dihydro-1H-indene (21 gm., 0.097 mole) is dissolved in acetic acid (280 ml.) and chromium trioxide (14 gm., 0.14 mole) in a mixture of water (15 ml.) and acetic acid (40 ml.) is added dropwise with stirring over a period of one hour. The mixture is poured, with stirring into cold water (1200 ml.) and the solid that separates is removed by filtration, washed with water and dried. The product, which consists of a mixture of the desired material and the isomer described in Step D, is subjected to column chromatographic separation using 225 gm. of silica gel and chloroform is used for elution. Evaporation of the solvent gives 6,7-dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one, 5.2 gm., m.p. 154°-156° C.
Step G. 2-Allyl-6,7-dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one
6,7-Dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one (63.5 gm., 0.274 mole) is dissolved in a mixture of dry tert.-butyl alcohol (500 ml.) and dry benzene (1.5 liters). The solution is refluxed and potassium tert.-butoxide (46 gm., 0.301 mole) in dry tert.-butyl alcohol (1 liter) is added as rapidly as possible. The solution is refluxed for another 1/2 hour, cooled to 20° C., stirred and treated with allyl bromide (36 gm., 0.301 mole). The mixture is stirred and refluxed for 4 hours, cooled and treated with water (250 ml.). The crude 2-allyl-6,7-dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one is separated by filtration, washed with water, dried and recrystallized from a mixture of benzene and hexane.
Step H. 2-Allyl-6,7-dichloro-5-hydroxy-2,3-dihydro-1H-inden-1-one
Dry pyridine hydrochloride (500 gm.) is melted and heated to 195° C. and 2-allyl-6,7-dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one (45.4 gm., 0.167 mole) is added with stirring. The reaction mixture is kept at 195° C. for 45 minutes and then poured with vigorous stirring into crushed ice (2 kg.). The crude product is collected by filtration, washed with water and dried. The 2-allyl-6,7-dichloro-5-hydroxy-2,3-dihydro-1H-inden-1-one is recrystallized from a mixture of ethanol and water.
Step I. Ethyl [(2-allyl-6,7-dichloro-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate
Carrying out a reaction as described in Example 1, Step D, except that the 5,6-dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one is replaced by an equimolar quantity of 2-allyl-6,7-dichloro-5-hydroxy-2,3-dihydro-1H-inden-1-one, there is obtained ethyl [(2-allyl-6,7-dichloro-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
Step J. Ethyl {[2-allyl-6,7-dichloro-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}-acetate
Carrying out a reaction as described in Example 20, Step B, except that the methyl [(6,7-dichloro-2-ethyl-1-oxo-2,3-dihydro-1H-inden-5-yl)-oxy]acetate is replaced by an equimolar quantity of ethyl [(2-allyl-6,7-dichloro-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate, there is obtained ethyl [2-allyl-6,7-dichloro-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy acetate.
Step K. Ethyl [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
Carrying out a reaction as described in Example 20, step C, except that the methyl [6,7-dichloro-2-ethyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy acetate is replaced by an equimolar quantity of ethyl (2-allyl-6,7-dichloro-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl)oxy)acetate, there is obtained ethyl [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
Step L. [(9a-Allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out a reaction as described in Example 20, Step D, except that the methyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate is replaced by an equimolar quantity of ethyl [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate, there is obtained [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 48 [(5,6-Dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetra-3H-fluoren-7-yl)oxy]acetic acid
By carrying out a series of reactions as described in Example 47, except that in Step G, the allyl bromide is replaced by an equimolar quantity of propargyl bromide and using the product from each step in the subsequent step, there is obtained:
Step G. 6,7-Dichloro-5-methoxy-2-propargyl-2,3-dihydro-1H-inden-1-one.
Step H. 6,7-Dichloro-5-hydroxy-2-propargyl-2,3-dihydro-1H-inden-1-one.
Step I. Ethyl [(6,7-dichloro-1-oxo-2-propargyl-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
Step J. Ethyl [6,7-dichloro-1-oxo-2-(3-oxobutyl)-2-propargyl-2,3-dihydro-1H-inden-5-yl]-oxy acetate.
Step K. [5,6-Dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetate.
Step L. [(5,6-Dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 49 [(5,6-Dichloro-9a-(2-methylpropyl)-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out a series of reactions as described in Example 47, except that in Step G, the allyl bromide is replaced by and equimolar quantity of 2-methylpropyl bromide, and using the product from each step in the subsequent one, there is obtained:
Step G. 6,7-Dichloro-2-(2-methylpropyl)-5-methoxy-2,3-dihydro-1H-inden-1-one.
Step H. 6,7-Dichloro-2-(2-methylpropyl)-5-hydroxy-2,3-dihydro-1H-inden-1-one.
Step I. Ethyl {[6,7-dichloro-2-(2-methylpropyl)-1-oxo-2,3-dihydro-1H-inden-5-yl]oxy]}acetate.
Step J. Ethyl [6,7-dichloro-2-(2-methylpropyl)-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy acetate.
Step K. Ethyl [5,6-dichloro-9a-(2-methylpropyl)-3-oxo-1,2,9,9a-tetrahydro-3Hfluoren-7-yl]oxy acetate.
Step L. [5,6-Dichloro-9a-(2-methylpropyl)-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl]oxy acetic acid.
EXAMPLE 50
[(5,6-Dichloro-9a-cyclopropylmethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out a series of reactions as described in Example 47, except that in Step G, the allyl bromide is replaced by an equimolar quantity of (bromomethyl)cyclopropane, and using the product from each step in the subsequent step, there is obtained:
Step G. 6,7-Dichloro-2-cyclopropylmethyl-5-methoxy-2,3-dihydro-1H-inden-1-one.
Step H. 6,7-Dichloro-2-cyclopropylmethyl-5-hydroxy-2,3-dihydro-1H-inden-1-one.
Step I. Ethyl [(6,7-dichloro-2-cyclopropyl-methyl-1-oxo-2,3-dihydro-1H-inden-5-yl)oxy]acetate.
Step J. Ethyl {[6,7-dichloro-2-cyclopropyl-methyl-1-oxo-2-(3-oxobutyl)-2,3-dihydro-1H-inden-5-yl]oxy}acetate.
Step K. Ethyl [(5,6-dichloro-9a-cyclopropyl-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetate.
Step L. [(5,6-Dichloro-9a-cyclopropylmethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 51
[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
5,6-Dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (Example 1, Step C) (15 gm., 0.048 mole), potassium carbonate (13.3 gm., 0.096 mole), dimethylformamide (100 ml.) and iodo-acetic acid (10.6 gm., 0.057 mole) is stirred at room temperature for 24 hours. The reaction mixture is poured into water (150 ml.), stirred, warmed to 50° C., filtered and the filtrate acidified with 6 N hydrochloric acid to obtain [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid, which after recrystallization from acetic acid, melts at 237° C.-238° C.
EXAMPLE 52 [(5,6-Dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out a reaction as described in Example 51, except that the 5,6-dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one is replaced by an equivalent quantity of 5,6-dichloro-7-hydroxy-9a-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (Example 3, Step C), and there is obtained [(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 53
[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Step A. tert.-Butyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetate
A mixture of 5,6-dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (Example 1, Step C) (15 gm., 0.048 mole), tert.-butyl bromoacetate (10.3 gm., 0.0528 mole), potassium carbonate (13.3 gm., 0.096 mole) and dimethylformamide (100 ml.) is stirred at 35° C. for an hour and then cooled and poured into water (100 ml.). The solid that separates is tert.-butyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate, which is separated by filtration, washed with water and dried. This material is adequate for use in the next step.
Step B. [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Tert.-butyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (8.22 gm., 0.02 mole) in benzene (100 ml.) containing p-toluenesulfonic acid (0.6 gm.) is refluxed for 20 minutes. The solid that separates upon cooling is [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid, m.p. 237° C.--238° C.
EXAMPLE 54
[(5,6-Dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Step A. Tert.-butyl [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetate
Carrying out a reaction as described in Example 53, Step A, except that the 5,6-dichloro-9a-ethyl-7-hydroxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one is replaced by an equimolar quantity of 5,6-dichloro-7-hydroxy-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (Example 4, Step C), thereby is obtained tert.-butyl [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
Step B. [(5,6-Dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid
Carrying out a reaction as described in Example 53, Step B, except that the tert.-butyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate is replaced by an equimolar amount of tert.-butyl [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate, thereby is obtained [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
EXAMPLE 55
Benzyl [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
Methyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (Example 20, Step C) (5.8 g., 0.016 mole) is dissolved in a mixture of dry benzyl alcohol (50 ml) and methylene chloride (40 ml.) containing amberlite IRA 400 (ethoxide) (5-6 g.). The mixture is stirred magnetically at reflux for four hours and then filtered. The filtrate is concentrated in vacuo to give a yellow solid (5.3 g.) which upon trituration with ethanol and washing with ether yields the product.
EXAMPLE 56
Ethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
A solution of [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 20, Step D) (0.15 g., 0.004 mole) absolute ethanol (60 ml) and 12 N HCl (5 ml.) in ethanol (20 ml.) is heated under reflux on the steam bath with stirring for an hour. The excess solvent is removed under reduced pressure. Ice and water are added to the oily residue and the product extracted into ether. After drying over MgSO 4 , the solution is concentrated to yield 1.6 g. of product, m.p. 160°-162° C.
Recrystallization from tetrahydrofuran-ether-petroleum ether (1:1:2) gives 1.15 g. of ethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetate, m.p. 164°-166° C.
By carrying out the reaction as described in Example 56, except that the ethanol is replaced by an equal amount of:
EXAMPLE 57
1-Propanol
EXAMPLE 58
Isopropyl alcohol
EXAMPLE 59
1-Butanol
EXAMPLE 60
Cyclobutanol
EXAMPLE 61
Allyl alcohol
EXAMPLE 62
Propargyl alcohol
There is obtained:
EXAMPLE 57
Propyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 58
Isopropyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 59
Butyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 60
Cyclobutyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 61
Allyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 62
Propargyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
By carrying out the reaction as described in Example 56 except that the [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid is replaced by an equimolar amount of:
EXAMPLE 63
(+) [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 31, Step A).
EXAMPLE 64
(-) [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 31, Step B).
There is obtained:
EXAMPLE 63
Ethyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate, m.p. 94°-97° C.
EXAMPLE 64
Ethyl (-) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate, m.p. 94°-97° C.
EXAMPLE 65
Carboxymethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
Step A. Benzyloxycarbonylmethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetate
A mixture containing [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 20, Step D) (1.07 g, 0.003 mole), potassium carbonate (0.41 g, 0.003 mole) and benzyl bromoacetate (0.69 g, 0.003 mole) in dimethylformamide (35 ml) is heated at 80° C. for two hours. Then this mixture is filtered and the filtrate is concentrated in vacuo. The residue is dissolved in methylene chloride, washed with aqueous sodium bicarbonate and then water, dried over anhydrous magnesium sulfate and concentrated in vacuo to give a viscous oil which is triturated with ether to give 1.06 g. of product.
Step B. Carboxymethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
Benzyloxycarbonylmethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetate (1.0 g, 0.002 mole) (Step A) is dissolved in tetrahydrofuran (35 ml) and hydrogenated at ambient temperatures and atmospheric pressure employing 10% Pd/C (0.05 g.) as the catalyst in 2 hours. The catalyst is filtered through super-cel in an atmosphere of nitrogen. Then the filtrate is concentrated in vacuo at 50° C. to give the product (0.74 g) which is purified by recrystallization from methanol (9 ml) to yield 0.50 g of product, m.p. 179°-181° C.
By carrying out the reaction as described in Example 65, Step A, except that the benzyl bromoacetate is replaced by an equimolar quantity of:
EXAMPLE 66
Step A. Benzyl 5-bromopentanoate
EXAMPLE 67
Step A. Benzyl 2-bromopropanoate
EXAMPLE 68
Step A. Benzyl 4-bromobutanoate
There is obtained:
EXAMPLE 66
Step A. 4-(Benzyloxycarbonyl)butyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 67
Step A. 1-(Benzyloxycarbonyl)ethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-yl)oxy]acetate.
EXAMPLE 68
Step A. 3-(Benzyloxycarbonyl)propyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
By carrying out the reaction as described in Example 65, Step B, except that the benzyloxycarbonylmethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate is replaced separately by the compounds produced in Example 66, Step A, Example 67, Step A, and in Example 68, Step A, there is produced:
EXAMPLE 66
Step B. 4-Carboxybutyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxyl]-acetate.
EXAMPLE 67
Step B. 1-Carboxyethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetate.
EXAMPLE 68
Step B. 3-Carboxypropyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetate.
By carrying out the reaction as described in Example 65, Step A, except that the [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxyl]-acetic acid is replaced by an equimolar quantity of:
EXAMPLE 69
Step A. (+) [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate acid (Example 31), there is obtained:
EXAMPLE 69
Step A. Benzyloxycarbonylmethyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
By carrying out the reaction as described in Example 65, Step B, except that the benzyloxycarbonylmethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate is replaced by the product of Example 69, Step A, there is obtained:
EXAMPLE 69
Step B. Carboxymethyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetate.
EXAMPLE 70
1-Carboxy-1-methylethyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
Step A. (+) 1-{[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetyl}imidazole.
(+) [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 31, Step A) (0.71 g., 0.002 mole) is suspended in dry tetrahydrofuran (20 ml) and cooled to 0° C. A solution of 1,1'-carbonyldiimidazole (0.32 g, 0.002 mole) in tetrahydrofuran (5 ml) is added. The solution of 1-{[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetyl}imidazole that is formed is used in the next step without isolation.
Step B. 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
To the solution of (+) 1-{[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetyl}imidazole (0.002 mole) prepared in Step A at 0° C. is added with stirring 2-hydroxyisobutyric acid (0.21 g., 0.002 mole). After stirring overnight at the ambient temperature, the colorless reaction mixture is concentrated in vacuo at 50° C. The resultant yellow liquid is chromatographed using a silica-gel (60 gm) column and eluted with a mixture of methylene chloride and isopropyl alcohol (100/5 v.v.). The product is obtained by evaporation of the solvent in vacuo.
By carrying out the reaction as described in Example 70, Steps A and B, except that the (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid is replaced by an equimolar amount of:
EXAMPLE 71 (+) [(5,6-Dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 38, Step A).
EXAMPLE 72 (+) [(5,6-Dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 39, Step A).
EXAMPLE 73 (+) [(5,6-Dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 37, Step A).
EXAMPLE 74 (+) [(5,6-Dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 40, Step A).
EXAMPLE 75 (+) [(9a-Butyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 32, Step A).
EXAMPLE 76 (+) [(5,6-Dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 43, Step A).
EXAMPLE 77 (+) [(5,6-Dichloro-9a-cyclopropylmethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 35, Step A).
EXAMPLE 78 (+) [(5,6-Dichloro-9a-cyclopentyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 41, Step A).
EXAMPLE 79 (+) [(5,6-Dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 42, Step A).
EXAMPLE 80 (+) [(9a-Allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 33, Step A).
EXAMPLE 81 (+) [(5,6-Dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 34, Step A).
EXAMPLE 82 (+) [(9a-Benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 36, Step A).
EXAMPLE 83 (+) [(5,6-Dichloro-3-oxo-9a-phenyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 44, Step A).
There is obtained:
EXAMPLE 71 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 72 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-9a-methyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 73 1-Carboxy-1-methylethyl (+) [(dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 74 1-Carboxy-1-methylethyl (+) [(dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 75 1-Carboxy-1-methylethyl (+) [(9a-butyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 76 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 77 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-9a-cyclopropylmethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 78 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-9a-cyclopentyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 79 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-3-oxo-9a-vinyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 80 1-Carboxy-1-methylethyl (+) [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 81 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 82 1-Carboxy-1-methylethyl (+) [(9a-benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7 -yl)oxy]acetate.
EXAMPLE 83 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-3-oxo-9a-phenyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 84
2-(4-Morpholinyl)ethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
Step A. 1-{[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetyl}imidazole
[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 20, Step D) (0.71 g., 0.002 mole) is suspended in dry tetrahydrofuran (20 ml) and cooled to 0° C. A solution of 1,1'-carbonyldiimidazole (0.32 g, 0.002 mole) in tetrahydrofuran (5 ml) is added. The solution of 1-{[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetyl}imidazole that is formed is used in the next step without isolation.
Step B. 2-(4-Morpholinyl)ethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
To the solution of 1-{[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetyl}imidazole (0.002 mole) prepared in Step A at 0° C. is added with stirring 4-(2-hydroxyethyl)morpholine (0.26 g., 0.002 mole) and a catalytic amount of sodium hydride (10 mg). After stirring overnight at the ambient temperature, the colorless reaction mixture is concentrated in vacuo at 50° C. The resultant yellow liquid is chromatographed using a silica-gel (60 gm) column and eluted with a mixture of methylene chloride and isopropyl alcohol (100/5 v.v.). The product is triturated with ether to give analytically pure product, 0.58 g, m.p. 133°-133.5° C.
By carrying out the reaction as described in Example 84, Step B, except that the 4-(2-hydroxyethyl)morpholine is replaced by an equimolar amount of:
EXAMPLE 85: 2-Dimethylaminoethanol
EXAMPLE 86: 3-Diethylaminopropanol
EXAMPLE 87: 1-(2-Hydroxyethyl)pyrrolidine
EXAMPLE 88: 1-Methyl-3-hydroxypiperidine
EXAMPLE 89: 1-Methyl-4-hydroxypiperidine
There is obtained:
EXAMPLE 85
2-Dimethylaminoethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 86
3-Diethylaminopropyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 87
2-(1-pyrrolidinyl)ethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 88
1-Methyl-3-piperidyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 89
1-Methyl-4-piperidyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 90
(5-Hydroxymethyl-2-furyl)methyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 20, Step D) (1.43 g, 0.004 mole) is suspended in dry tetrahydrofuran (10 ml) and then triethylamine (0.401 g., 0.004 mole) is added. The resulting solution is cooled at 0° C. followed by the addition of ethyl chloroformate (0.438 g, 0.004 mole) in tetrahydrofuran (5 ml) to form the mixed anhydride and triethylamine hydrochloride which precipitates. To this mixture is added 2,5-di(hydroxymethyl)furan (1.03 g, 0.008 mole) in tetrahydrofuran (5 ml). The reaction mixture is then allowed to rise to ambient temperature before refluxing for one hour. The triethylamine hydrochloride that separates (0.55 g) is filtered and the filtrate is concentrated in vacuo to give a brown solid (2.71 g) which is purified by column chromatography over silica gel (100 g) by elution with a mixture of methylene chloride-tetrahydrofuran (100/4 v.v.) followed by a mixture of methylene-chloride-isopropanol (100/5 v.v.) to give 0.55 g. of product which is recrystallized first from isopropanol and then from acetonitrile to give an impure material which melts at 135.5°-137° C. This material is further purified by high pressure liquid chromatography using a Whatman Partisil M9 10/25 PAC column and methylene chloride-isopropyl alcohol (100/2 v.v.) at a flow rate of 5 ml./min. The yield of analytically pure product is 280 mg., m.p. 142°-143° C.
By carrying out the reaction as described in Example 90, except that the 2,5-di(hydroxymethyl)furan is replaced by an equimolar amount of:
EXAMPLE 91: Dihydroxyacetone
EXAMPLE 92: 2-Methoxyethanol
EXAMPLE 93: Tetrahydrofurfuryl alcohol
EXAMPLE 94: 1,1,1-Tris(hydroxymethyl)ethane
There is obtained:
EXAMPLE 91
3-Hydroxy-2-oxopropyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 92
2-Methoxyethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 93
Tetrahydrofurfuryl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 94
2,2-Bis(hydroxymethyl)propyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 95
2-Oxopropyl [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7yl)oxy]acetate
Potassium carbonate (0.2 g) is suspended in a solution of [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 20, Step D) (0.4 g, 0.0011 mole) in dimethylformamide (3 ml). After warming the suspension on a steam bath for 15 minutes, chloroacetone (0.5 g, 0.005 mole) is added and the mixture heated for an additional 15 minutes. The reaction mixture is cooled, poured into water (50 ml) and the product extracted into ether (three 15 ml portions. The extract is dried over Na 2 SO 4 . After filtration, the extract is concentrated to give a yellow oil. Trituration with cold ether causes crystallization to occur. The crystalline product weighs 0.1 g and melts at 153°-155° C.
EXAMPLE 96
3-Hydroxypropyl [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
By substitution of an equimolar amount of 3-bromo-1-propanol for the chloroacetone in Example 95, there is obtained a crude product which is column chromatographed on silica gel and eluted with a mixture of acetic acid, acetone and toluene (5/5/90 v.v.v.). The product weighs 100 mg and melts at 114°-117° C.
By carrying out the reaction as described in Example 95, except that the chloroacetone is replaced by an equimolar amount of:
EXAMPLE 97: 2-Bromoethanol
EXAMPLE 98: 2-Bromo-1,3-propanediol
EXAMPLE 99: 2-Bromoethanesulfonamide
EXAMPLE 100: 1-Bromo-2,3-propanediol
There is obtained:
EXAMPLE 97
2-Hydroxyethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 98
1-(Hydroxymethyl)-2-hydroxyethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 99
2-Sulfamoylethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 100
2,3-Dihydroxypropyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 101
3-Pyridylmethyl [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
A mixture of methyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (Example 20, Step C) (0.74 g, 0.002 mole), 3 A molecular sieves (10 g) and 3-hydroxymethylpyridine (0.65 g, 0.006 mole) in methylene chloride (40 ml) is stirred at ambient temperature overnight.
The reaction mixture is then filtered through super-cel and washed with methylene chloride. The filtrate is concentrated in vacuo at 50° C. This residue is chromatographed over silica gel (30 g) by elution with a methylene chloride-isopropanol mixture (100/3 v.v.) to give 0.36 g of product which is recrystallized from isopropanol (7 ml) to yield 0.23 g of product containing isopropanol. This sample is dried at 83° C. for 13 hours in vacuo to remove the solvent. The yield of product is 0.20 g., m.p. 120°-121° C.
By carrying out the reaction as described in Example 101 except that the 3-hydroxymethylpyridine is replaced by an equimolar quantity of:
EXAMPLE 102: 2-Hydroxymethylpyridine
EXAMPLE 103: 4-Hydroxymethylpyridine
EXAMPLE 104: 3-Hydroxymethylpyridine-N-oxide
There is obtained:
EXAMPLE 102
2-Pyridylmethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 103
4-Pyridylmethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 104
3-Pyridylmethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate-N-oxide.
EXAMPLE 105
[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic Acid Anhydride
A stirred suspension of 5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]acetic acid (14.2 gm., 0.04 mole) in methylene chloride (1.5 liters) is treated with a solution of N,N-dicyclohexylcarbodiimide (4.33 gm., 0.021 mole) in methylene chloride (100 ml.). After an hour, the solvent is removed by distillation and the residue treated with dry ether (150 ml.). The dicyclohexyl-urea is removed by filtration and the ether removed by evaporation at reduced pressure to give [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid anhydride.
EXAMPLE 106
[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetamide
1-{[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetyl}imidazole (Example 84, Step A) (0.81 gm, 0.002 mole) in tetrahydrofuran (20 ml) is treated with 25% aqueous ammonium hydroxide (5 ml). After warming for an hour at 35° C., the solvent is removed in vacuo whereby the product remains which is washed with water and recrystallized from acetic acid.
By carrying out the reaction as described in Example 106, except that the 25% aqueous ammonium hydroxide is replaced by:
EXAMPLE 107A: (t-Butoxycarbonyl)methylamine
EXAMPLE 108A: 2-(t-Butyoxycarbonyl)ethylamine
There is obtained:
EXAMPLE 107
Step A. N-(t-Butoxycarbonylmethyl)-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetamide
EXAMPLE 108
Step A. N-[2-(t-Butoxycarbonyl)ethyl]-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetamide.
EXAMPLE 107
Step B. N-Carboxymethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetamide. N-(t-Butyoxcarbonylmethyl)-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetamide (Example 107, Step A) (600 mg) is dissolved in toluene (100 ml), treated with p-toluenesulfonic acid (50 mg) and the mixture refluxed for 2 hours. The solvent is removed and the product dissolved in an aqueous sodium bicarbonate solution, filtered and acidified to Congo-red paper with dilute hydrochloric acid. The solid that separates is removed by filtration, washed with water and dried. The yield is 300 mg.
EXAMPLE 108
Step B. N-(2-Carboxyethyl)-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetamide
By carrying out the reaction as described in Example 107, Step B, except that the N-(t-butoxycarbonylmethyl)-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetamide is replaced by an equimolar amount of N-[2-(t-butoxycarbonyl)ethyl]-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetamide. There is obtained N-(2-carboxyethyl)-[(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetamide.
EXAMPLE 109
2,3-Dihydroxypropyl [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
Step A. (2,2-Dimethyl-1,3-dioxolan-4-yl)methyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
A mixture of 2 gm. of [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]-acetic acid, 3 ml. of 2,2-dimethyl-4-hydroxymethyl-1,3-dioxolane and 0.5 g. of p-toluenesulfonic acid hydrate are heated on the steam bath for 3 hours. The dark reaction mixture then is chromatographed on 300 g of silica, and eluted with acetic acid-acetone-toluene (5:5:90). Fractions containing a single component (Rf˜0.4) are pooled and concentrated to a yellow oil. On standing overnight, a mixture of crystalline solid and yellow oil resulted. The mixture is filtered and the solid recrystallized from tetrahydrofuran-ether-petroleum ether (5:15:25). The yield of pure product is 0.3 g., m.p. 143°-145° C.
Step B. 2,3-Dihydroxypropyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
A mixture of 165 mg of (2,2-dimethyl-1,3-dioxolan-4-yl)methyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate from Example 109, Step A is dissolved in 100 ml. of 0.075 N hydrochloric acid and 20 ml. of acetone and heated, with stirring at 50°-55° C. for 2 hours. The mixture is cooled and neutralized with a solution of sodium bicarbonate. The solution is saturated with sodium chloride and extracted two times with 100 ml. portions of 20% tetrahydrofuran in ether. The extract is dried over Na 2 SO 4 . After filtration, the filtrate was concentrated to a yellow oil that solidified on standing. After recrystallization from tetrahydrofuran-ether-petroleum ether, there is obtained 110 mg. of product, m.p. 135°-138° C.
EXAMPLE 110
1-(Hydroxymethy)-2-hydroxyethyl [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
Step A. (2-Phenyl-1,3-dioxan-5-yl) [(5,6-dichloro-9a-ethyl-3 -oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
By substituting the 2,2-dimethyl-4-hydroxymethyl-1,3-dioxolane used in Example 109, Step A, with an equimolar quantity of 5-hydroxy-2-phenyl-1,3-dioxane and conducting the reaction, as described in Example 109, Step A, there is obtained (2-phenyl-1,3-dioxan-5-yl) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
Step B. 1-(Hydroxymethyl)-2-hydroxyethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
By substituting the (2,2-dimethyl-1,3-dioxolan-4-yl)methyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate used in Example 109, Step B by an equimolar amount of (1-phenyl-1,3-dioxan-5-yl) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate and conducting the reaction as described in Example 109, Step B, there is obtained 1-(hydroxymethyl)-2-hydroxyethyl [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 111
[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid hydrazide
By conducting a reaction as described in Example 106, except that an equimolar quantity of anhydrous hydrazine is used in place of the ammonium hydroxide, there is obtained [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid hydrazide.
By carrying out a reaction as described in Example 70, Step B, except the 2-hydroxyisobutyric acid is replaced by an equimolar amount of:
EXAMPLE 112: 2-Ethyl-2-hydroxybutyric acid
EXAMPLE 113: L(+)-lactic acid
EXAMPLE 114: 5-Hydroxypentanoic acid
EXAMPLE 115: 1-Hydroxycyclobutanecarboxylic acid
EXAMPLE 116: 1-Hydroxycyclopentanecarboxylic acid
There is obtained:
EXAMPLE 112
1-Carboxy-1-ethylpropyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 113
L(+)1-Carboxyethyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
EXAMPLE 114
4-Carboxybutyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 115
1-Carboxycyclobutyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 116
1-Carboxycyclopentyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate.
EXAMPLE 107
Parenteral Solution of the Sodium Salt of (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
(+) [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 31, Step A) (100 mg) is dissolved by stirring and warming in a solution of 0.05 N sodium bicarbonate (6 ml). The solution is the diluted to 10 ml. and sterilized by filtration. All the water used in the preparation is pyrogen-free.
EXAMPLE 118
Parenteral Solution of the Sodium Salt of (+) [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
(+) [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 37, Step A) (100 mg) is dissolved by stirring and warming in a solution of 0.05 N sodium bicarbonate (6 ml). The solution is then diluted to 10 ml. and sterilized by filtration. All the water used in the preparation is pyrogen-free.
EXAMPLE 119
Parenteral Solution of the Sodium Salt of (+) [(5,6-dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
(+) [(5,6-Dichloro-3-oxo-9a-propargyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 34, Step A) (100 mg) is dissolved by stirring and warming in a solution of 0.05 N sodium bicarbonate (6 ml). The solution is then diluted to 10 ml. and sterilized by filtration. All the water used in the preparation is pyrogen-free.
EXAMPLE 120
Parenteral solution of the Sodium Salt of (+) [(5,6-dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
(+) [(5,6-Dichloro-9a-cyclopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 43, Step A) (100 mg) is dissolved by stirring and warming in a solution of 0.05 N sodium bicarbonate (6 ml). The solution is then diluted to 10 ml. and sterilized by filtration. All the water used in the preparation is pyrogen-free.
EXAMPLE 121
Parenteral Solution of the Sodium Salt of (+) [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H fluoren-7-yl)oxy]acetic acid.
(+) [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 33, Step A) (100 mg.) is dissolved in 0.05 N sodium bicarbonate solution (6 ml.) by warming and stirring. The solution is then diluted to 10 ml with water and sterilized by filtration. All the water used in the preparation is pyrogen-free.
EXAMPLE 122
Parenteral Solution of the 1-Methylpiperazinium Salt of (+) [(9a-benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid.
(+) [(9a-Benzyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (100 mg.) Example 36, Step A) is dissolved by warming and stirring in a solution of 0.05 N 1-methylpiperazine (6 ml). The solution is then diluted to 10 ml with water and sterilized by filtration. All the water used in the preparation is pyrogen-free.
Similar parenteral solutions can be prepared by replacing the active ingredient of the above example by any of the other carboxylic acid compounds of this invention.
EXAMPLE 123
Parenteral Solution of the Sodium Salt of 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
1-Carboxy-1-methylethyl (+) [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (Example 70, Step B) (100 mg.) is dissolved by stirring and warming in a solution of 0.05 N sodium bicarbonate (6 ml). The solution is then diluted to 10 ml and sterilized. All the water used in the preparation is pyrogen-free.
EXAMPLE 124
Parenteral Solution of the Sodium Salt of 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
1-Carboxy-1-methylethyl (+) [(5,6-Dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (Example 73) (100 mg.) is dissolved by stiring and warming in a solution of 0.05 N sodium bicarbonate (6 ml). The solution is then diluted to 10 ml and sterilized. All the water used in the preparation is pyrogen-free.
EXAMPLE 125
Parenteral Solution of the Sodium Salt of 1-Carboxy-1-methylethyl (+) [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
1-Carboxy-1-methylethyl (+) [(9a-allyl-5,6-dichloro-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (Example 80) (100 mg.) is dissolved in 0.05 N sodium bicarbonate solution (6 ml.) by warming and stirring. The solution is then diluted to 10 ml with water and sterilized by filtration. All the water used in the preparation is pyrogen-free.
EXAMPLE 126
Parenteral Solution of the Ammonium Salt of 1-Carboxy-1-methylethyl (+) [(5,6-dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate
1-Carboxy-1-methylethyl (+) [(5,6-dichloro-9a-isopropyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (100 mg.) (Example 74) is dissolved by warming and stirring in a solution of 0.05 N ammonium hydroxide (6 ml). The solution is then diluted to 10 ml with water and sterilized by filtration. All the water used in the preparation is pyrogen-free.
EXAMPLE 127
Dry-filled capsules containing 50 mg. of active ingredient per capsule
______________________________________ Per Capsule______________________________________(+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetra-hydro-3H-fluoren-7-yl)oxy]-acetic acid 50 mg.Lactose 149 mg.Magnesium Stearate 1 mg.Capsule (Size No. 1) 200 mg.______________________________________
The (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 31, Step A) is reduced to a No. 60 powder and then lactose and magnesium stearate are passed through a No. 60 bolting cloth onto the powder and the combined ingredients admixed for 10 minutes and then filled into a No. 1 dry gelatin capsule.
EXAMPLE 128
Dry-filled capsules containing 50 mg. of active ingredient per capsule
______________________________________ Per Capsule______________________________________(+) [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetra-hydro-3H-fluoren-7-yl)oxy]-acetic acid 50 mg.Lacetose 149 mg.Magnesium Stearate 1 mg.Capsule (Size No. 1) 200 mg.______________________________________
The (+) [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 37, Step A) is reduced to a No. 60 powder and then lactose and magnesium stearate are passed through a No. 60 bolting cloth onto the powder and the combined ingredients admixed for 10 minutes and then filled into a No. 1 dry gelatin capsule.
EXAMPLE 129
Dry-Filled Capsules Containing 50 mg. of Active Ingredient Per Capsule
______________________________________ Per Capsule______________________________________1-Carboxy-1-methylethyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetra-hydro-3H-fluoren-7-yl)oxy]acetate 50 mg.Lacetose 49 mg.Magnesium Stearate 1 mg.Capsule (Size No. 1) 100 mg.______________________________________
The 1-carboxy-1-methylethyl (+) [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (Example 70, Step B) is reduced to a No. 60 powder and then lactose and magnesium stearate are passed through a No. 60 bolting cloth onto the powder and the combined ingredients admixed for 10 minutes and then filled into a No. 2 dry gelatin capsule.
EXAMPLE 130
Dry-Filled Capsules Containing 50 mg. of Active Ingredient Per Capsule
______________________________________ Per Capsule______________________________________1-Carboxy-1-methylethyl(+)[(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate 50 mg.Lactose 49 mg.Magnesium Stearate 1 mg.Capsule (Size No. 1) 100 mg.______________________________________
The 1-carboxy-1-methylethyl (+) [(5,6-dichloro-3-oxo-9a-propyl-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate (Example 73) is reduced to a No. 60 powder and then lactose and magnesium stearate are passed through a No. 60 bolting cloth onto the powder and the combined ingredients admixed for 10 minutes and then filled into a No. 2 dry gelatin capsule.
Similar dry-filled capsules can be prepared by replacing the active ingredient of the above example by any of the other compounds of this invention. | The invention relates to novel [(5,6,9a-substituted-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)-oxy]alkanoic and cycloalkanoic acids and their analogs, esters, salts and derivatives. These compounds are synthesized by methods selected from a number of synthetic routes depending on the particular structure, choice of intermediate or preferred reaction sequence. The compounds are useful in the treatment and prevention of injury to the brain and spinal chord due to accidents, ischemic stroke and hydrocephalus; compositions for such uses are also disclosed. | 2 |
DESCRIPTION OF THE INVENTION
Recently a revolution occurred in the industrial electrolysis field due to the development and commercialization of ion-exchange polymeric membranes, such as Nafion®/Du Pont de Nemours, Flemion®/Asahi Glass and others. Such ion-exchange membranes are produced in the form of sheets, even of considerable dimensions, with a thickness that ranges from 0.2 to 0.5 mm max. Although provided with a reinforcement fabric, membranes are still affected by a low mechanical resistance, especially to abrasion and bending.
Due to the availability of membranes in sheet-form, electrolysis cells had to be redesigned into an essentially flat shape, reducing their thickness and volume. As a consequence of this new design, membrane electrolysis cells may present problems concerning uneven internal distribution of the electrolyte as well as inefficient removal of the liquid-gas mixture when the products of electrolysis are gaseous such as for example in chlor-alkali or water electrolysis. The problem of removing the gas-liquid mixtures from both cathodic and anodic compartments of said cells is of great concern. In fact, strong pressure fluctuations in both compartments would be experienced with an improper design of the outlets causing damages to the membranes in very short periods of time. These anomalous pressure fluctuations may be ascribed to the alternating of the gas-liquid phases entering the outlet duct on the top of the cell. The inconvenience connected to the pressure fluctuations, although typical of membrane cells, is also common to other types of cells, generally cells of the divided type, where the anode and the cathode together with the relevant compartments are divided by any kind of separator, such ion exchange membranes as discussed above, porous diaphragms and the like.
Technical literature discloses several ways to face this problem, leading substantially to the following two solutions:
collecting the gas-liquid phase through a downcomer, that can be positioned inside the cell itself (Uhde GmbH), or outside the same (Chlorine Engineers), as described in `Modern Chlor-Alkali Technology`, vol. 4, Society of Chemical Industry, Elsevier 1990. This kind of device produces a flow of the falling film type with a constant-with-time flow of liquid (a falling film covering the internal surface of the duct) and gas (in the central section, free from liquid) and efficaciously eliminates pressure fluctuations. Nevertheless, the aforesaid device can be utilized only in cells working under forced circulation, and not in cells with a natural circulation, caused by the produced gas (gas lift or gas draft). This limitation is of great relevance as natural circulation membrane cells offer particular advantages due to their high recirculation capacity, eg. the possibility of easily controlling the electrolyte acidity (pH), which, in chlor-alkali electrolysis for instance, permits to properly adjust the oxygen content in the produced chlorine gas.
removal of gas and liquid phases through a duct positioned inside the cell itself (U.S. Pat. No. 4,839,012, assigned to The Dow Chemical Co.) This collector, consisting in a horizontal pipe duct of the same length as that of the cell, is parallel to the higher edge of the cell and as close to it as possible. The collector, connected to the port through which gas and liquid phases are removed, is provided with suitable holes, approximately set by the superior generatrix. This device, referred to as pressure fluctuation dampening device, is fit for installation both in forced and in natural circulation cells. Nevertheless, the efficiency of such a device is only partial, since the residual absolute pressure pulses are in the range of 200-300 mm of water which could induce in the worst case a pressure pulse differential in the order of 600 mm of water between the two surfaces of the membrane with the possibility of experiencing damages due to fatigue caused by the membrane flexing near the edges, and abrasion of the membrane as a consequence of the rubbing against the electrode surface.
The present invention discloses a device for the removal of gas and liquid phases in membrane electrolysis cells to substantially eliminate pressure fluctuations, consequently prolonging the useful lifetime of the membrane by practically preventing the risk of damages due to abrasion or fatigue. More generally, said device is useful in all types of the so-called divided cells.
This surprising result, of extreme importance both under a technical and an economical point of view, can be attained by supplying each compartment of the electrolytic cell (whose products are gaseous) with two separate ducts for removing respectively the gas-rich and the liquid-rich phases which separate in the top of the cell compartment. The gas phase duct enters the cell above the connection between the cell itself and the liquid phase duct; furthermore the other end of said gas duct is inserted into the liquid phase duct in a position not at all critical, the only requirement concerning its distance from the point of connection of the liquid phase duct to the top of the cell, such distance should substantially be kept at least to a multiple (for instance three times) of the equivalent diameter of the connection itself. The insertion of the other end of the gas-rich phase duct inside the liquid-rich phase duct represents an important feature of the present invention; in this way a suitable pressure is maintained in the top of the cell filled by the gas-rich phase, and the liquid level is stabilized in such a position as to prevent the liquid itself from flowing into the gas phase duct and the gas-rich phase from being injected into the liquid phase duct. As a consequence, the minimum level of the liquid should never drop below the superior tangent to the section of the connection between the cell and the liquid phase duct. The height of the cell area filled with gas should not exceed a critical value in the range of a few centimeters, in order to ensure a constant wetting of the ion-exchange membrane, caused by sprays and waves naturally ensuing from the separation of gas from liquid. Said condition is essential for a regular and prolonged operation of the membrane which, on the contrary, would quickly embrittle due to drying and gas diffusion. Said pressure in the top of the cell may be obtained with alternative embodiments, such hydraulic heads and regulating valves, as will be discussed later on.
The invention will now be described in details by referring to the following figures.
FIG. 1 is a front view of a cell of membrane electrolyzer equipped with the device of the invention.
FIG. 2 shows a detail of the device of the invention.
FIG. 3 is a cross section of a cell illustrated in FIG. 2 of a bipolar electrolyzer
FIG. 4 is a similar cross section of a cell of a monopolar electrolyzer.
FIG. 5, 6 and 7 are front views of a membrane cell with different embodiments of the device of the invention.
FIG. 1 shows a cell of a membrane electrolyzer equipped with a frame (1) to ensure, together with suitable gaskets, a waterproof sealing along the edges of the several cells assembled to form the electrolyzer in the so-called "filter-press configuration". The cell comprises also an electrode (2) consisting in a foraminous sheet, such as expanded or perforated sheet or a screen provided, if necessary, with an appropriate electrocatalytic coating; an inlet (6) and an outlet duct (3); flanges (7, 5) for connection to feeding and removal loops, as known in the art. The cell is also supplied, according to the present invention, with a duct (4) for the removal of gas-rich products, one end of which is connected to the top of the cell and the other to the middle portion of outlet duct (3) for the removal of the liquid-rich phase.
FIG. 2 shows a detail of the cell comprising the two ducts (4, 3).
With reference to FIG. 3, it can be seen that the electrodes (2) are mechanically fastened or welded to the studs (8) protruding from the central body (9) providing both for the rigidity of the cell and for the transmission and distribution of electric current. The body (9) and the studs (8) may have different designs other than those illustrated in FIG. 3, 4, 7, without reducing the usefulness of the present invention. The generation of gas on the electrode surface (2) causes the formation of a gas-electrolyte mixture in an upward movement. In the top of the cell the mixture tends to separate back into a gasrich and a liquid-rich phase; in the prior art, characterized by a single type of outlet (duct (3) shown in FIG. 3 or a similar device), the removal of the two phases involved the generation of pressure fluctuations, negatively affecting the useful lifetime of the ion-exchange membrane (11) adjacent to the electrode (2).
The utilization of the device of the present invention surprisingly minimizes the pressure fluctuations, thus preventing their negative effect on the useful lifetime of the ion-exchange membrane. The reasons for such a positive and highly important result cannot be clearly understood at present; an explanation could be found in the fluid mechanics of the top of the cell. As it can be seen in FIG. 3, if the level of the liquid phase is maintained above the tangent line (10) over the outlet but below the inferior edge of the flange (1), where the outlet (4) is positioned, then a constant fluid removal is obtained. In particular, the gaseous phase contained in the top of the cell between line (10) and the inferior edge of the flange (1), is conveyed exclusively into duct (4) together with small quantities of liquid. The liquid phase, still containing gas residues, is withdrawn from duct (3). Said situation fundamentally differs from the prior art where a single outlet is provided and the gaseous and liquid phases, once separated in the top of the cell, alternate forcedly. The stabilization of the liquid level between line (10) and the edge of the flange (1) requires an appropriate balancing of the section and the length of the ducts (3, 4), in the area comprised between the outlet from the cell and the point wherein the two pipes meet, with the aim of maintaining said pressure in top of the cell below the pressure drop which occurs inside the duct for the liquid-rich phase removal; on the other hand the minimum value of said pressure in the top of the cell should never decrease below the value of the total pressure drop inside the duct for the liquid-rich phase removal subtracted by the height of liquid defined by line (10) and the edge (1) of the flange.
FIG. 5 and 6 show further embodiments of the present invention, wherein the elements are equipped with an outlet duct for the liquid-rich phase situated in a horizontal position.
As it can be noted in FIG. 5a, the duct for the gas-rich phase (4) is connected to the liquid-rich phase duct (3) at a distance from the cell outlet significantly greater than the usual distance in cells with a vertical outlet (FIG. 1, 2, 3, 4). As a matter of fact, the insertion of the gaseous phase duct (4) into the liquid phase duct (3) is made in a position which is not at all critical with the only requirement that the cross section and length of ducts (3, 4) between the outlet from the cell and the conjunction of the two ducts meet the above discussed condition necessary for stabilization of the liquid level inside the cell. FIG. 5b and 6a schematize two embodiments of a large size cell provided with more than one gas-rich phase ducts (4) with two different types of connections to the liquid phase duct, respectively before the gas-disengager (12) (FIG. 5b), provided with a gas and a liquid outlet, and directly into the gas-disengager (12) under an appropriate hydraulic head (FIG. 6a).
FIG. 6b shows alternative embodiments of the present invention, wherein the gas phase duct is connected to a hydraulic seal system (15) containing a suitable quantity of electrolyte and equipped with an outlet for gas (16).
From a practical point of view, said embodiment can be obtained by connecting all the gas-rich phase ducts (4) to a common collector, wherein the pressure is controlled by a single hydraulic seal system or an equivalent device.
FIG. 7 schematizes a further embodiment of the invention, wherein the two ducts ((3) and (4)) for separately removing the liquid and the gas phases are coaxial; this embodiment presents the advantage of eliminating the connection between the gas phase duct (4) and the flange (1), with a consequent reduction of production costs and an increase of the element mechanical reliability.
EXAMPLE 1
An experimental electrolyzer of monopolar type was assembled using 6 anodic elements, 5 cathodic elements, 2 terminal cathodic elements of the type schematized in FIG. 1, each of them being 1200 mm high and 1500 mm wide, with a resulting area of 1.8 m 2 ; the anodic elements were connected through the ducts (3) to an anodic gas-disengager, the cathodic elements were similarly connected to a cathodic gas-disengager.
The top of each element was provided with two connections (3, 4) for separately removing the gas-rich and the liquid-rich phases as described in the present invention. In particular, the diameter of the two ducts (3, 4) was respectively of 40 and 10 mm, the length of the portion of duct (3) comprised between the outlet from the element and the point of insertion of duct (4) being 150 mm, the maximum height of the gas area comprised between line (10) and the edge of the flange (1) being 30 mm.
3 anodic elements and 3 cathodic elements were also provided with pressure gauges. The electrolyzer was equipped with 12 ion-exchange membranes, Nafion® 961 produced by Du Pont.
The anodic compartments were fed with a solution of sodium chloride at 300 g/l and the cathodic compartments with a solution of sodium hydroxide at about 30%. Current density was 3000 Ampere/m 2 , for a total current of 66,000 Ampere fed at the electrolyzer; the average temperature under operation was 85° C., with a voltage of 3.1 Volts. The electrolyzer circulation under these conditions was in the range of 0.5 m 3 /h per m 2 of membrane and the pressure fluctuations had a maximum excursion of about 20 mm of water column, the frequency being approximately of 0.1 -0.2 Hertz. Similar measurement were taken on a similar industrial electrolyzer, equipped with a single outlet for the gas/liquid mixture, respectively chlorine/sodium chloride brine for the anodic elements and hydrogen/sodium hydroxide solution for the cathodic elements. Pressure fluctuations had in this case a maximum intensity of 200 mm in the anodic elements and around 250 mm in cathodic elements, with a frequence ranging around 0.5-0.6 Hertz.
EXAMPLE NO. 2
The chlor-alkali electrolysis, as described in Example 1, was carried out in a bipolar electrolyzer consisting of 10 bipolar elements and 2 end elements as shown in FIG. 5b, 1200 mm high and 3000 mm long, equipped with 12 membranes, Nafion® 961 produced by Du Pont.
The current density was also in this case 3000 Ampere/m®, for a total current of 11000 Ampere and an overall voltage of 36 Volt.
2 bipolar elements were provided with pressure gauges in their top.
With an electrolyte circulation of 0.4 m 3 /h per m 2 of membrane, the pressure fluctuations showed a maximum intensity in the range of 20-30 mm of water column, the frequency varying from 0.1 to 0.2 Hertz.
For comparison purposes, measurements were also carried out on a similar industrial electrolyzer, the elements of which were equipped with a single outlet for the gas-liquid mixture. The pressure fluctuations, both anodic and cathodic, had a significant intensity, ranging from 500 to 600 mm of water column, with a frequency of 0.6-0.8 Hertz. | The present invention relates to a device for removing gas-liquid mixtures from electrolysis cells divided into compartments, particularly membrane type cells, without producing pressure fluctuations, wherein each compartment of said cells is characterized in that it is provided with two different ducts for removing the mixture after separation into liquid-rich and gas-rich phases, each duct being connected with its first end to the upper part of the cell, while the other end of the gas-rich phase duct (4) is inserted into the liquid-rich phase duct (3) so that liquid is present only in the portion of the duct comprised between the connection to the cell and the point of inlet of the gas-rich phase. In the subsequent portion the flow consists in the gas-liquid mixture which is forwarded to a gas-disengaging vessel. As said second end of the gas-rich phase duct (4) is inserted into the liquid-rich phase duct (3), sufficient pressure is maintained in the upper gas-separating area of the cell to prevent the liquid-rich phase from entering the gas-rich phase duct (4). | 2 |
BACKGROUND OF THE INVENTION
This invention is generally directed to photoconductive imaging members with organic polymers as charge transport components. More specifically, the present invention is directed to layered imaging members with organic charge transport components selected from diaryl biarylylamine-based charge transport polymers. The aforementioned charge transport polymers possess a number of advantages including excellent charge transporting characteristics; they are environmentally safe, non-hazardous and non-toxic; and their structural simplicities render their synthesis easily executable by economic processes. In addition, the charge transport polymers of the present invention can be utilized as a single-component transport layer, that is wherein a binder resin is not used in the transport layer of layered imaging devices. Single-component transport layers provide, for example, long-term structural stability since they are devoid of the problem of small molecule crystallization commonly associated with charge transport molecules-in-binder transport layers. In addition, the charge transport polymers illustrated herein enable photoconductive imaging members that can be selected for electrophotographic imaging and printing processes for an extended number of imaging cycles, while avoiding or minimizing charge transport molecule crystallization. The imaging members of the present invention are especially suitable for imaging and printing apparatuses wherein liquid developers are selected, primarily since a single-component transport layer can be utilized, that is a resin binder is not needed in this embodiment, and the polymer, or polymers illustrated herein are selected, thereby eliminating the problem of charge transport molecule leaching and bleeding when the imaging members are in contact with liquid developers. Furthermore, the charge transport polymers of the present invention possess acceptable solubility in common organic solvents such as halogenated, especially chlorinated hydrocarbons, tetrahydrofuran, toluene, xylene, and the like, thus enabling improved coatability thereof by various processes such as spray, dip, and draw-down coating techniques. In one embodiment of the present invention, the imaging member is comprised of a supporting substrate, a photogenerating layer, and in contact therewith a charge transport layer comprised of diaryl biarylylamine-based charge transport polymers optionally, but not preferably, dispersed in inactive resinous binders, such as the optional binders selected for the photogenerating layer including polycarbonates. The charge transport layer can be located as the top layer of the imaging member, or alternatively it may be situated between the supporting substrate and the photogenerating layer.
The formation and development of electrostatic latent images on the imaging surfaces of photoconductive materials by electrostatic means is well known. Numerous different photoconductive members for use in xerography are known such as selenium, alloys of selenium, layered imaging members comprised of aryl amine charge transport layers, reference U.S. Pat. No. 4,265,990, and imaging members with charge transport layers comprised of polysilylenes, reference U.S. Pat. No. 4,618,551. The disclosures of the aforementioned patents are totally incorporated herein by reference. However, the layered imaging members with transport layers incorporating the diaryl biarylylamine-based polymers of the present invention are, for example, economically more attractive in most instances than, for example, the members of the '790 and '551 patents in respect of material and fabrication costs, and possess the other advantages illustrated herein. Further, the diaryl biarylylamine-based charge transport polymers of the present invention can be synthesized from readily available inexpensive starting materials via cost-effective synthetic processes. Also, in regard to photochemical stability, the charge transport polymers of the present invention are superior to, for example, polysilylenes, and the aforementioned transport polymers do not photodegrade when exposed to ultraviolet radiations.
There are also known photoreceptor materials comprised of inorganic or organic materials wherein the charge carrier generation and charge carrier transport functions are accomplished by discrete contiguous layers. Additionally, photoreceptor materials are disclosed in the prior art which include an overcoating layer of an electrically insulating polymeric material and in conjunction with this overcoated type photoreceptor there have been proposed a number of imaging methods.
Specifically, layered photoresponsive devices including those comprised of photogenerating layers and transport layers are disclosed as indicated herein in U.S. Pat. No. 4,265,990, and overcoated photoresponsive materials containing a hole injecting layer overcoated with a transport layer, followed by an overcoating of a photogenerating layer and a top coating of an insulating organic resin, reference U.S. Pat. No. 4,251,612. Examples of generating layers disclosed in these patents include trigonal selenium and vanadyl phthalocyanine, while examples of the charge transport layer that may be employed are comprised of the aryldiamines as mentioned therein. The '990 patent is of particular interest in that it discloses layered photoresponsive imaging members similar to those illustrated in the present application with the exception that the charge transporting component of the members of the present invention are comprised of charge transport polymers of the formulas illustrated herein. These members can be utilized in an electrophotographic method by, for example, initially charging the member with an electrostatic charge and imagewise exposing to form an electrostatic latent image which can be subsequently developed to form a visible image. Other representative patents disclosing layered photoresponsive devices include U.S. Pat. Nos. 4,115,116; 4,047,949 and 4,081,274.
As a result of a patentability search there was located (1) U.S. Pat. No. 4,025,341 which discloses imaging members with photoconductive polymers comprised of the condensation products of a tertiary amine having at least two phenyl groups, and a carbonyl-containing compound of the formula as illustrated in column 3, with examples of condensation polymers being provided in column 4, reference Formula II, noting especially the polymers when R 5 , R 9 , and R 10 are each aryl(phenyl), however, it is believed that the polymers of the present invention are substantially different from those described in the '341 patent in that the invention polymers are polar charge transport polymers selected from, for example, the group consisting of polyesters, polycarbonates, polyurethanes and their copolymeric derivatives, while in contrast the polymers of U.S. Pat. No. 4,025,341 are nonpolar polymers whose backbones do not contain any carbonyl functions (C═O bond). Furthermore, the polymers of the present invention are formed from covalently linking suitable charge transport monomers via the C--O bonds rather than the C--C bonds as in the polymers of the '341 patent; (2) U.S. Pat. No. 4,725,518 which discloses imaging members wherein the charge transport layer is comprised of an aromatic amine compound and a protonic or Lewis acid; and (3) U.S. Pat. Nos. 3,567,450; 3,658,520; 4,025,341; 4,540,651; 4,606,988 and 4,769,302.
There is also disclosed in Belgium Patent No. 763,540 an electrophotographic member having at least two electrically operative layers, the first layer comprising a photoconductive layer which is capable of photogenerating charge carriers, and injecting the photogenerated holes into an active layer containing a transport organic material which is substantially nonabsorbing in the spectral region of intended use, but which is active and that allows injection of photogenerating holes from the photoconductive layer and allows these holes to be transported through the active layer. The active polymers may be mixed with inactive polymers or non-polymeric materials. Also, there is disclosed in U.S. Pat. Nos. 4,232,102 and 4,233,383, the disclosures of which are totally incorporated herein by reference, the selection of sodium carbonate doped and barium carbonate doped photoresponsive imaging members containing trigonal selenium.
U.S. Pat. No. 4,869,988, and copending patent application U.S. Ser. No. 274,160, entitled, respectively, PHOTOCONDUCTIVE IMAGING MEMBERS WITH N,N-BIS(BIARYLYL)ANILINE, OR TRIS(BIARYLYL)AMINE CHARGE TRANSPORTING COMPONENTS, and PHOTOCONDUCTIVE IMAGING MEMBERS WITH BIARYLYL DIARYLAMINE CHARGE TRANSPORTING COMPONENTS, the disclosures of which are totally incorporated herein by reference, there are described layered photoconductive imaging members with transport layers incorporating biarylyl diarylamines, N,N-bis(biarylyl)anilines, and tris(biarylyl)amines as charge transport compounds. More specifically, in this application and patent there are disclosed improved layered photoconductive imaging members comprised of a supporting substrate, a photogenerating layer, optionally dispersed in an inactive resinous binder, and in contact therewith a charge transport layer comprised of the above-mentioned charge transport compounds, or mixtures thereof dispersed in resinous binders. Examples of specific charge transporting components disclosed in the U.S. Pat. No. 4,869,988 include N,N-bis(4-biphenylyl)-3,5-dimethoxyaniline (Ia); N,N-bis(4-biphenylyl)-3,5-dimethylaniline (Ib); N,N-bis(4-methyl-4'-biphenylyl)-3-methoxyaniline (Ic); N,N-bis(4-methyl-4'-biphenylyl)-3-chloroaniline (Id); N,N-bis(4-methyl-4'-biphenylyl)-4-ethylaniline (Ie); N,N-bis(4-chloro-4'-biphenylyl)-3-methylaniline (If); N,N-bis(4-bromo-4'-biphenylyl)-3,5-dimethoxyaniline (Ig); 4-biphenylyl bis(4-ethoxycarbonyl-4'-biphenylyl)amine (IIa); 4-biphenylyl bis(4-acetoxymethyl-4'-biphenylyl)amine (IIb); 3-biphenylyl bis(4-methyl-4'-biphenylyl)amine (IIc); 4-ethoxycarbonyl-4'-biphenylyl bis(4-methyl-4'-biphenylyl)amine (IId); and the like.
Examples of specific charge transporting compounds disclosed in copending application U.S. Ser. No. 274,160 include bis(p-tolyl)-4-biphenylylamine (IIa); bis(p-chlorophenyl)-4-biphenylylamine (IIb); N-phenyl-N-(4-biphenylyl)-p-toluidine (IIc); N-(4-biphenylyl)-N-(p-chlorophenyl)-p-toluidine (IId); N-phenyl-N-(4-biphenylyl)-p-anisidine (IIe); bis(m-anisyl)-4-biphenylylamine (IIIa); bis(m-tolyl)-4-biphenylylamine (IIIb); bis(m-chlorophenyl)-4-biphenylylamine (IIIc); N-phenyl-N-(4-biphenylyl)-m-toluidine (IIId); N-phenyl-N-(4-bromo-4'-biphenylyl)-m-toluidine (IVa); diphenyl-4-methyl-4'-biphenylylamine (IVb); N-phenyl-N-(4-ethoxycarbonyl-4'-biphenylyl)-m-toluidine (IVc); N-phenyl-N-(4-methoxy-4'-biphenylyl)-m-toluidine (IVd); N-(m-anisyl)-N-(4-biphenylyl)-p-toluidine (IVe); bis(m-anisyl)-3-biphenylylamine (Va); N-phenyl-N-(4-methyl-3'-biphenylyl)-p-toluidine (Vb); N-phenyl-N-(4-methyl-3'-biphenylyl)-m-anisidine (Vc); bis(m-anisyl)-3-biphenylylamine (Vd); bis(p-tolyl)-4-methyl-3'-biphenylylamine (Ve); N-p-tolyl-N-(4-methoxy-3'-biphenylyl)-m-chloroaniline (Vf); and the like.
The following patent applications and U.S. patents are mentioned: (1) U.S. Pat. No. 4,818,650 describes layered imaging members with novel polymeric, hydroxy and alkoxy aryl amines, wherein m is a number of between about 4 and 1,000, reference for example claims 1 and 2; (2) U.S. Ser. No. 061,247 now abandoned and U.S. Pat. No. 4,871,634 illustrate imaging members with novel dihydroxy terminated aryl amine small molecules, reference claims 1 and 2, for example; (3) U.S. Pat. No. 4,806,444, the disclosure of which is totally incorporated herein by reference, describes layered imaging members with novel polycarbonate polymeric aryl amines, reference claims 1 and 2, for example; (4) U.S. Pat. No. 4,806,443, the disclosure of which is totally incorporated herein by reference, illustrates novel polycarbonate polymeric amines useful in layered imaging members, reference claims 1 and 2, for example; and (5) U.S. Pat. No. 4,801,517, the disclosure of which is totally incorporated herein by reference, which discloses imaging members with novel polycarbonate aryl amines, reference claims 1 and 2, for example.
While imaging members with various charge transporting substances, including the aryl amines of the above mentioned U.S. patents are suitable for their intended purposes, there continues to be a need for improved members, particularly layered members, which are comprised of single-component transport layers of charge transport polymers, thereby ensuring the long-term stability of the members. Another need resides in the provision of layered imaging members that are compatible with liquid developer compositions. Further, there continues to be a need for layered imaging members wherein the layers are sufficiently adhered to one another to allow the continuous use of such members in repetitive imaging systems. Also, there continues to be a need for improved layered imaging members whose transport layers are devoid of the problems of transport molecule crystallization. Furthermore, there continues to be a need for charge transporting copolymers which are also useful as protective overcoating layers, and as interface materials for various imaging members. Additionally there is a need for charge transport compounds or copolymers that are nontoxic, and wherein such members are inert to the users thereof. A further need resides in the provision of novel efficient charge transport copolymers which are readily accessible synthetically from inexpensive commercial starting materials.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide layered photoresponsive imaging members with many of the advantages indicated herein.
It is also another object of the present invention to provide novel, efficient charge transport polymers which can function as single-component transport media, that is where a resin binder is avoided for layered photoconductive imaging members.
It is yet another object of the present invention to provide improved layered photoresponsive imaging members with copolymer charge transport layers in contact with a photogenerating layer, which members are suitable for use with liquid or dry developer compositions.
In a further object of the present invention there is provided an improved layered photoresponsive imaging member with a photogenerating layer situated between a supporting substrate, and a charge transport layer comprised of the charge transport polymers illustrated herein.
In yet another object of the present invention there is provided an improved photoresponsive imaging member comprised of a charge transporting copolymer layer situated between a supporting substrate and a photogenerating layer.
In another object of the present invention there are provided imaging and printing methods with the layered imaging members disclosed herein.
Another object of the present invention resides in the provision of charge transport polymers which are nontoxic and inert to the users of the devices within which they are incorporated.
A further object of the present invention is to provide improved layered imaging members which avoid the problem of transport molecule crystallization enabling their selection, for example, in imaging apparatuses with liquid developer compositions, and which members are insensitive to changes in environmental conditions, such as humidity.
In yet a further object of the present invention there are provided novel efficient charge transport copolymers which are readily accessible by simple synthetic processes.
A further object of the present invention resides in the provision of improved layered imaging members with a charge transport layer comprised of charge transport copolymers doped with charge transport small molecules, such as bis-(p-tolyl)-4-biphenylylamine, bis(m-anisyl)-4-biphenylylamine, N-phenyl-N-(4-biphenylyl)-p-toluidine, N-phenyl-N-(4-biphenylyl)-p-toluidine, N-phenyl-N-(4-biphenylyl)-m-anisidine, bis(m-tolyl)-4-biphenylylamine, and the like, enabling such devices to be utilized in very high speed, that is for example more than 135 copies per minute, copying and printing processes.
These and other objects of the present invention are accomplished by the provision of layered imaging members comprised of diaryl biarylylamine-based polymers. More specifically, the present invention is directed to layered imaging members comprised of photogenerating layers, and in contact therewith charge transport layers comprised of the diaryl biarylylamine-based polymers of Formula (I) as illustrated herein.
In one specific embodiment, the present invention is directed to an improved layered photoconductive imaging member comprised of a supporting substrate, a photogenerating layer comprised of organic or inorganic, photoconductive pigments, optionally dispersed in an inactive resinous binder, and in contact therewith a charge transport layer comprised of a diaryl biarylylamine-based polymer, or copolymers of the following Formula I, optionally doped with suitable charge transport small molecule compounds. ##STR2## wherein A is independently selected from a bifunctional linkage such as --O--, alkyleneoxy with from, for example, a carbon chain length of from 1 to about 15 carbon atoms, and preferably from 1 to about 10 carbon atoms such as --OCH 2 --, --OCH 2 CH 2 --, --OCH 2 CH 2 OCH 2 CH 2 --, aryleneoxy with from, for example, a carbon chain length of from 6 to about 24 carbon atoms, and preferably from 6 to about 20 carbon atoms such as --OC 6 H 4 --, alkylenedioxy with from, for example, a carbon chain length of from 1 to about 15 carbon atoms, and preferably from 1 to about 10 carbon atoms, such as --OCH 2 CH 2 O--, --OCH 2 CH 2 OCH 2 CH 2 O--, arylenedioxy with from, for example, a carbon chain length of from 6 to about 24 carbon atoms, and preferably from 6 to about 20 carbon atoms, such as --OC 6 H 4 O--, and the like; B is independently selected from the group of bifunctional linkages such as CO--R"--CO--, --COO--R"--OCO--, --CONH--R"--NHCO--, wherein R" is alkylene with from, for example, a carbon chain length of from 1 to about 15 carbon atoms, or arylene with from, for example, a carbon chain length of from 6 to about 24 carbon atoms such as methylene, dimethylene, trimethylene, tetramethylene, pentamethylene, 2-methyltetramethylene, 3,3-dimethylpentamethylene, phenylene, tolylene, ether, or a polyether segment such as --CH 2 CH 2 OCH 2 CH 2 --, --(CH 2 CH 2 O) 2 CH 2 CH 2 --, and the like; Z is alkylenedioxy, arylenedioxy, substituted derivatives thereof containing from 2 to about 30 carbon atoms, such as trimethylenedioxy, tetramethylenedioxy, pentamethylenedioxy, phenylenedioxy, bis(oxyphenyl) propane, bis(oxyphenyl) cyclohexane, bis(oxyphenyl) methane, and the like; R and R' are independently selected from aliphatic and aromatic substituents, such as alkyl, aryl, alkoxy, aryloxy functions with from 1 to about 24 carbon atoms, halogen, such as chlorine, bromine, fluorine, and iodine; and the like; x and y are mole fractions with the provision that x and y are greater than 0; and that the sum of x+y is equal to 1.0; a and b are the numbers 0,1 or 2; and n is the number of monomer units ranging preferably from about 10 to about 300.
Specific examples of charge transporting copolymers include, but are not limited to, those represented by the following formulas: ##STR3##
Examples of alkyl and alkoxy groups include those with from 1 carbon atom to about 25 carbon atoms, and preferably from about 1 carbon atom to about 8 carbon atoms, inclusive of methyl, methoxy, ethyl, ethoxy, propyl, propoxy, butyl, butoxy, pentyl, pentoxy, hexyl, octyl, octoxy, nonyl, nonoxy, decyl, decoxy, pentadecyl, stearyl, and other similar substituents. Specific preferred alkyl and alkoxy groups are methyl, methoxy, ethyl, ethoxy, propyl, propoxy, butyl and butoxy. Aryl and aryloxy include those with from about 6 to about 24 carbon atoms such as phenyl, phenoxy, naphthyl, and the like. Other examples of alkylene are those groups with from 1 to about 20 carbon atoms such as ethylene, propylene, butylene, hexylene, and the like.
The photoresponsive imaging members of the present invention can be prepared by a number of known methods, the process parameters and the order of the coating of the layers being dependent on the member desired. Thus, for example, the photoresponsive members of the present invention can be prepared by providing a conductive substrate with an optional charge blocking layer and an optional adhesive layer, applying thereto a photogenerating layer, and overcoating thereon a charge transport layer of the diaryl biarylylamine charge transport copolymer illustrated herein, optionally doped with from about 1 to about 20 percent by weight of charge transport molecules such as bis-(p-tolyl)-4-biphenylylamine, bis(m-anisyl)-4-biphenylylamine, N-phenyl-N-(4-biphenylyl)-p-toluidine, N-phenyl-N-(4-biphenylyl)-p-toluidine, N-phenyl-N-(4-biphenylyl)-m-anisidine, bis(m-tolyl)-4-biphenylylamine, and the like. The improved photoresponsive imaging members of the present invention can be fabricated by common known coating techniques such as by dip coating, wet coating, draw-down coating, or by spray coating process, depending largely on the type of imaging devices desired. Each coating, however, can be usually dried, for example, in a convection or forced air oven at a suitable temperature before a subsequent layer is applied thereto.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 represents a partially schematic cross-sectional view of a photoresponsive imaging member of the present invention;
FIGS. 2 and 3 represent partially schematic cross-sectional views of photoresponsive imaging members of the present invention; and
FIG. 4 represents a partially schematic cross-sectional view of a specific photoresponsive imaging member of the present invention wherein the charge transporting layer is situated between a supporting substrate, and the photogenerating layer.
Illustrated in FIG. 1 is a photoresponsive imaging member of the present invention comprising a 50 micron to 5,000 micron thick supporting substrate 3, a charge carrier photogenerating layer 5 of thickness of 0.1 micron to 5 microns comprised of a photogenerating pigment 6, optionally dispersed in inactive resinous binder composition 7, and a 5 micron to 60 micron thick charge transport layer 9 comprised of a diaryl biarylylamine copolymer of Formula I as illustrated herein as a charge transporting substance 11 optionally doped with 1 percent to 20 percent by weight of a suitable charge transport molecule 14, such as bis(m-tolyl) biphenylylamine, bis(m-anisyl) biphenylylamine, and the like. In an alternative embodiment of the present invention, and in further regard to FIG. 1, the charge transporting layer can be situated between the supporting substrate and the photogenerating layer.
Illustrated in FIG. 2 is a photoresponsive imaging member of the present invention comprised of a conductive supporting substrate 15 of aluminized Mylar of a thickness of about 50 microns to 100 microns, a 0.5 micron to about 5 micron thick photogenerating layer 17 comprised of trigonal selenium photogenerating pigments 19 optionally dispersed in a resinous binder 21 in the amount of 10 percent to about 80 percent by weight, and a charge transport layer 23 comprised of the charge transport copolymers 24 of Formulas II, III, IV, V, VI, VII, VIII or IX optionally doped with 1 percent to 20 percent by weight of the charge transport molecule 25, such as bis(m-tolyl) biphenylylamine, or bis(m-anisyl) biphenylylamine primarily to enhance the transport efficiency of the transport layer.
Another photoresponsive imaging member, reference FIG. 3, is comprised of a conductive supporting substrate 31 of aluminum of a thickness of 50 microns to about 5,000 microns, a photogenerating layer comprised of amorphous selenium or an amorphous selenium alloy 33, especially selenium arsenic, with 99.9 percent by weight of selenium, and selenium tellurium with from about 70 to about 85 percent by weight of selenium of thickness of 0.1 micron to about 5 microns, and a 10 micron to 50 micron thick charge transport layer 37 comprised of the charge transport copolymers 38 of Formulas II, III, IV, V, VI, VII, VIII or IX optionally doped with 1 percent to 20 percent by weight of a charge transport molecule 39.
Illustrated in FIG. 4 is a photoresponsive imaging member of the present invention comprised of a 25 micron to 100 micron thick conductive supporting substrate 41 of aluminized Mylar a 10 micron to 50 micron thick charge transport layer 47 comprised of the charge transport copolymers 48 of Formulas II, III, IV, V, VI, VII, VIII or IX optionally doped with 1 percent to about 20 percent by weight of a suitable charge transport molecule 49, such as bis(m-tolyl) biphenylylamine, or bis(m-anisyl) biphenylylamine, and a 0.5 micron to about 5 micron thick photogenerating layer 50 comprised of vanadyl phthalocyanine photogenerating pigments 53 optionally dispersed in a polyester resinous binder 55 (49,000 available from Goodyear Chemical) in the amount of 25 percent to 80 percent by weight.
The supporting substrate layers may be opaque or substantially transparent and may comprise any suitable material having the requisite mechanical properties. The substrate may comprise a layer of an organic or inorganic material having a conductive surface layer arranged thereon or a conductive material such as, for example, aluminum, chromium, nickel, indium, tin oxide, brass or the like. The substrate may be flexible or rigid and many have any of many different configurations such as, for example, a plate, a cylindrical drum, a scroll and the like. The thickness of the substrate layer is dependent on many factors including, for example, the components of the other layers, and the like; generally, however, the substrate is of a thickness of from about 50 microns to about 5,000 microns.
Examples of preferred photogenerating layer components, especially since they permit imaging members with a photosensitivity of from about 400 to about 700 nanometers, for example, include those comprised of known photoconductive charge carrier generating materials, such as amorphous selenium alloys, halogen doped amorphous selenium, halogen doped amorphous selenium alloys, trigonal selenium, mixtures of Groups IA and IIA, elements, selenite and carbonates with trigonal selenium, reference U.S. Pat. Nos. 4,232,102 and 4,233,283, the disclosures of each of these patents being totally incorporated herein by reference, copper, and chlorine doped cadmium sulfide, cadmium selenide and cadmium sulfur selenide and the like. Examples of specific alloys include selenium arsenic with from about 95 to about 99.8 weight percent selenium; selenium tellurium with from about 70 to about 90 weight percent of selenium; the aforementioned alloys containing halogens such as chlorine in amounts of from about 100 to about 1,000 parts per million; ternary alloys, and the like. The thickness of the photogenerating layer is dependent on a number of factors, such as the materials included in the other layers, and the like; generally, however, this layer is of a thickness of from about 0.1 micron to about 5 microns, and preferably from about 0.2 micron to about 2 microns depending on the photoconductive volume loading, which may vary from 5 percent to 100 percent by weight. Generally, it is desirable to provide this layer in a thickness which is sufficient to absorb about 90 percent or more of the incident radiation which is directed upon it in the imagewise exposure step. The maximum thickness of this layer is dependent primarily upon factors such as mechanical considerations, for example whether a flexible photoresponsive device is desired. Optional transport molecules suitable as dopants for the charge transport present, for example, in an amount of 1 percent to about 20 percent by weight are comprised, for example, of those illustrated in the aforementioned U.S. Pat. No. 4,869,988, and aforementioned copending application U.S. Ser. No. 274,160, the disclosures of which are totally incorporated herein by reference, such as bis(p-tolyl)-4-biphenylylamine, bis(p-chlorophenyl)-4-biphenylylamine, N-phenyl-N-(4-biphenylyl)-p-toluidine, N-(4-biphenylyl)-N-(p-chlorophenyl)-p-toluidine, N-phenyl-N-(4-biphenylyl)-m-anisidine, bis(m-anisyl)-4-biphenylylamine, bis(m-tolyl)-4-biphenylylamine, bis(m-chlorophenyl)-4-biphenylylamine, N-phenyl-N-(4-biphenylyl)-m-toluidine, N-phenyl-N-(4-bromo-4'-biphenylyl)-m-toluidine, and the like. Also, there may be selected as photogenerators, provided the objectives of the present invention are achieved, organic components such as squaraines, perylenes, reference for example U.S. Pat. No. 4,587,189, the disclosure of which is totally incorporated herein by reference, metal phthalocyanines, metal free phthalocyanines, vanadyl phthalocyanine, dibromoanthanthrone, and the like.
The transport layer is usually comprised of at least one of the charge transport polymers illustrated herein, which polymer or polymers may be optionally doped with suitable charge transport molecules to further improve the photosensitivity of the imaging members for very high speed copying and printing applications. The optional dopants, which are intended to further enhance the electrical performance of the imaging members, may be present in an amount of from about 1 to about 50 percent by weight, and preferably from about 1 percent to about 20 percent by weight. The thickness of this layer is, for example, from about 5 microns to about 50 microns with the thickness depending predominantly on the nature of intended applications, thus other thicknesses outside these ranges can be selected in some instances. In addition, a layer of adhesive material to promote the adhesion of the transport layer to the photogenerating layer can be utilized. This layer may comprise common known adhesive materials such as polyester resins, reference 49,000 polyester available from Goodyear Chemical Company, polysiloxane, acrylic polymers, and the like. A thickness of from about 0.001 micron to about 0.1 micron for this layer is generally employed. Hole blocking layers such as those derived from the polycondensation of aminopropyl trialkoxysilane or aminobutyl trialkoxysilane may optionally be introduced between the substrate and the photogenerating layer to improve the dark decay characteristics of the imaging member. Typically, this layer has a thickness of from about 0.001 micron to about 5 microns or more in thickness depending on the effectiveness with which this layer prevents the dark injection of charge carriers into the photogenerating layer.
The charge transporting diaryl biarylylamine copolymers of the present invention can be readily synthesized by the copolycondensation of stoichiometric quantities of a bifunctionalized monomer such as the corresponding dihydroxy derivatives and a suitable dihydroxy comonomer such as bisphenol A, bisphenol Z, and other similar bisphenols, with appropriate bifunctional reagents. The latter can be selected from the group consisting of diacyl halide such as adipoyl chloride, bishaloformates such as ethylene glycol bischloroformate or diethylene glycol bischloroformate, and diisocyanates such as benzene diisocyanate, toluene diisocyanate, and the like. For the charge transport copolyesters and copolycarbonates, the polymerization is conducted in an inert atmosphere at temperatures ranging from about 0° C. to about 40° C., and preferably from 10° C. to about 30° C., in the presence of an excess organic base such as triethylamine, tripropylamine, tributylamine, and the like. Typically, a slight excess of bishaloformate or diacyl chloride is employed to compensate for the propensity of the reagent to undergo hydrolysis, and about a 2 to 10 fold excess of the base is utilized. The polycondensation is carried out in a suitable solvent such as aliphatic halogenated and aromatic solvents including methylene chloride, ethyl acetate, tetrahydrofuran, dioxane, and the like. For the charge transport copolyurethanes, the reaction is accomplished with or without a catalyst in a suitable solvent such as dimethylsulfoxide, dimethylformamide, and the like, at temperatures ranging from ambient to about 80° C. The preferred catalyst for polyurethane preparation is di-n-butyltin dilaurate, although other catalysts such as di-n-butyltin disulfite, tri-n-butyltin acetate, ferric acetyl acetonate, triethylenediamine, triethylamine, and the like, can also be selected. The charge transport copolymers are usually isolated and purified by repeated precipitation of tetrahydrofuran solutions of said copolymers from a non-solvent such as methanol or water.
Examples of diacyl halides for the preparation of the charge transport copolyesters include succinyl chloride, glutaryl chloride, adipoyl chloride, pimeloyl chloride, 3-methyladipoyl chloride, suberoyl chloride, azelaoyl chloride, sebacoyl chloride, and the like. Examples of bishaloformates for the synthesis of the charge transport copolycarbonates include ethylene glycol bischloroformate, diethylene glycol bischloroformate, triethylene glycol bischloroformate, propylene glycol bischloroformate, butylene glycol bischloroformate, and the like. For the preparation of charge transport copolyurethanes, the diisocyanates that can be selected for the reaction include benzene diisocyanate, toluene diisocyanate, hexane diisocyanate, diphenylmethane diisocyanate, cyclohexane diisocyanate, and the like. Examples of dihydroxy comonomers include bis(p-hydroxyphenyl)methane, 2,2-bis(p-hydroxyphenyl)propane, 1,1-bis(p-hydroxyphenyl)cyclohexane, 1,4-xylene diol, ethylene glycol, diethylene glycol, and the like.
The diaryl biarylylamine-based charge transport copolymers of the present invention display very high hole mobility in the order of 10 -5 cm 2 /volts per second at an electric field of 2×10 5 volts/centimeter. Accordingly, layered imaging members incorporating the charge transport copolymers of the present invention exhibit excellent photosensitivity with a half-decay exposure sensitivity in the order of 1 to 3 ergs/cm 2 , and possess very low dark decay characteristics, typically in the order of less than 20 volts/second. Also, the electrical characteristics of the aforementioned imaging members and imaging performance in some embodiments are equal to or superior to those exhibited by imaging members containing the aryl amine charge transport materials such as tritolylamine, substituted N,N,N',N'-tetraarylbenzidine, and the like. Also, the charge transport copolymers of the present invention are generally utilized as a single component with no resin binder, thereby ensuring the long-term stability of the transport layer. Imaging members with a single-component transport layer are especially suitable for use with liquid developer compositions without the problem of crystallization, bleeding or leaching of transport small molecules. As the transport layer of the present invention is transparent to the visible light, all or substantially most of the visible radiations used in the exposure reaches the photogenerating layer without noticeable loss. Also, the imaging members of the present invention possess high photosensitivity with a half-decay exposure sensitivity being in the range of 1.0 to about 3.0 ergs/cm 2 as indicated herein, very low residual potential of less than 50 volts, and cycling stability of over 10,000 cycles.
The following examples are being supplied to further define specific embodiments of the present invention, it being noted that these examples are intended to illustrate and not limit the scope of the present invention. Also, parts and percentages are by weight unless otherwise indicated.
EXAMPLE I
Synthesis of Bis(m-hydroxyphenyl)-4-Biphenylylamine
A mixture of 70.0 grams of m-iodotoluene, 7.0 grams of copper bronze powder, and 55 grams of potassium carbonate in 200 milliliters of Soltrol 220 was mechanically stirred and heated in a 300 milliliter round-bottomed flask fitted with a reflux condenser. When the temperature of the mixture reached 160° C., 16.9 grams of 4-aminobiphenyl was added, and the resulting reaction mixture was heated under reflux at 220° C. for two hours. At this stage, another mixture of 8.0 grams of potassium carbonate and 4.0 grams of copper bronze powder was added to the reaction mixture, and heating was continued at this temperature for another three hours. The hot reaction mixture was filtered, and the filtrate was cooled to room temperature, yielding an off-white precipitate. Recrystallization twice from isopropanol afforded 19.5 grams of analytically pure bis(m-anisyl)-4-biphenylylamine, and melting point (m.p.) of 98° C. to 98.5° C.
1 H-NMR (CDCl 3 ), δ (ppm): 3.75(s, 6H); 6.5 to 6.8(m, 6H); 7.1 to 7.6(m, 11H).
Elemental Analysis, Calculated for C 26 H 23 NO 2 : C, 81.86; H, 6.08; N, 3.67. Found: C, 81.77; H, 6.09; N, 3.70.
A mixture of 9.06 grams of the obtained bis(m-anisyl)-4-biphenylylamine, and 21.5 grams of sodium iodide in 50 milliliters of sulfolane was heated to 120° C. in a round-bottomed flask with constant stirring. After 15 minutes of heating at this temperature, the mixture was cooled to about 70° C., and 0.35 milliliter of water was added. Subsequently, 18 milliliters of chlorotrimethylsilane was added over a period of 15 minutes. The resulting mixture was then heated for another 3.5 hours before pouring the mixture carefully into 600 milliliters of cold water with stirring. The crude solid product was filtered, dried, and purified by column chromatography on silica gel using a 1:50 mixture of acetone and methylene chloride as an eluent. The yield of pure bis(m-hydroxyphenyl)-4-biphenylylamine was 7.3 grams, m.p. of 176.5° C. to 178° C.
1 H-NMR (CDCl 3 ), δ (ppm): 4.55(s, 2H); 6.4 to 7.6(m, 17H).
Elemental Analysis, Calculated for C 24 H 19 NO 2 : C, 81.56; H, 5.42; N, 3.96. Found: C, 81.43; H, 5.12; N, 4.03.
EXAMPLE II
Synthesis of Copolycarbonate (II)
A mixture of 2.85 grams of bis(m-hydroxyphenyl)biphenylylamine obtained from Example I and 0.1 gram of 2,2-bis(p-hydroxyphenyl)propane was dissolved in a mixture of 10 milliliters of methylene chloride and 3.5 milliliters of triethylamine in a round-bottomed flask under a nitrogen atmosphere. The resulting solution was cooled to about 10° C., and a solution of 2.1 grams of diethylene glycol bischloroformate in 3.0 milliliters of methylene chloride was added dropwise over a period of 20 minutes. After addition, the reaction mixture was stirred at room temperature for 3 hours before 2 milliliters of absolute ethanol and 1 milliliter of triethylamine were added. After stirring for another 1 hour, the reaction mixture was evaporated to dryness under reduced pressure. The residue was dissolved in 20 milliliters of tetrahydrofuran, and the resulting solution was added dropwise into 500 milliliters of water with constant stirring. The solid polymer was filtered, dried, dissolved in 20 milliliters of tetrahydrofuran, and precipitated from water as illustrated herein. Final purification was carried out by precipitating twice from 500 milliliters of methanol using 25 milliliters of tetrahydrofuran solution. The copolycarbonate of Formula II obtained was dried in vacuo at 60° C. overnight, and the yield was 3.7 grams. The number average molecular weight of the copolycarbonate (II) as determined by GPC analysis was 19,800 (relative to a polystyrene standard).
EXAMPLE III
Synthesis of Copolyester (III)
The preparation of the copolyester of Formula (III) was accomplished in accordance with the procedure of Example II with the exception that 2.40 grams of bis(m-hydroxyphenyl)biphenylylamine and 0.46 gram of 1,1-bis(p-hydroxyphenyl)cyclohexane were employed in place of the biphenylyl amine, and that 1.92 grams of freshly distilled azelaoyl chloride was used instead of diethylene glycol bischloroformate. In addition, the polymerization was carried out for 8 hours instead of 3 hours. The yield of copolyester (III) was 3.3 grams, and its number average molecular weight was 17,500.
EXAMPLE IV
Synthesis of Copolycarbonate (VI)
The preparation of copolycarbonate of Formula VI was accomplished in accordance with the procedure of Example II with the exceptions that a mixture of 1.5 gram of bis(m-hydroxyphenyl)biphenylylamine and 0.97 gram of 2,2-bis(p-hydroxyphenyl)propane was employed in place of the 2.85 grams of bis(m-hydroxyphenyl)biphenylylamine. The yield of copolycarbonate VI was 3.6 grams, and the number average molecular weight was 21,400.
EXAMPLE V
A layered photoresponsive imaging member with a hole transport layer comprised of the copolycarbonate II of Example II, and a photogenerating layer comprised of trigonal selenium was prepared as follows:
A photoresponsive imaging member was fabricated by providing an aluminized Mylar substrate in a thickness of 75 microns, followed by applying thereto with a multiple-clearance film applicator in a wet thickness of 0.5 mils, a layer of silane blocking layer derived from N-methyl-3-aminopropyl-trimethoxysilane (available from PCR Research Chemicals) in ethanol in a 1:20 volume ratio. This layer was dried for 5 minutes at room temperature, followed by curing for 10 minutes at 110° C. in a forced air oven. There was then applied to the silane layer a solution of 0.5 percent by weight of 49,000 polyester (Dupont Chemical) in a mixture of methylene chloride and 1,1,2-trichloroethane(4:1 volume ratio) with a multiple-clearance film applicator to a wet thickness of 0.5 mils. The layer was allowed to dry for one minute at room temperature, and 10 minutes at 100° C. in a forced air oven. The resulting adhesive layer had a dry thickness of 0.05 micron.
A dispersion of trigonal selenium and poly(N-vinylcarbazole) was prepared by ball milling 1.6 grams of trigonal selenium and 1.6 grams of poly(N-vinyl carbazole) in 14 milliliters each of tetrahydrofuran and toluene. Thereafter, 10 grams of the resulting slurry was then diluted with a solution of 0.25 gram of bis(m-anisyl)-4-biphenylylamine in 5 milliliters each of tetrahydrofuran and toluene. A 1.0 micron thick photogenerator layer was then fabricated by coating the above dispersion onto the adhesive layer present on the Mylar substrate with a multiple-clearance film applicator, followed by drying in a forced air oven at 135° C. for 5 minutes.
A solution for the hole transport layer was then prepared by dissolving 1.0 gram of copolycarbonate II in 7 milliliters of methylene chloride. This solution was then coated over the above photogenerator layer by means of a multiple-clearance film applicator. The resulting member was subsequently dried in a forced air oven at 130° C. for 30 minutes resulting in a 27 microns thick transport layer.
The fabricated imaging member was electrically tested by negatively charging it with a corona, and discharged by exposing to white light of wavelengths of from 400 to 700 nanometers. Charging was accomplished with a single wire corotron in which the wire was contained in a grounded aluminum channel and was strung between two insulating blocks. The acceptance potential of this imaging member after charging, and its residual potential after exposure were recorded. The procedure was repeated for different exposure energies supplied by a 75 watt Xenon arc lamp of incident radiation, and the exposure energy required to discharge the surface potential of the member to half of its original value was determined. This surface potential was measured using a wire loop probe contained in a shielded cylinder, and placed directly above the photoreceptor member surface. This loop was capacitively coupled to the photoreceptor surface so that the voltage of the wire loop corresponds to the surface potential. Also, the cylinder enclosing the wire loop was connected to the ground.
For the above prepared imaging member the acceptance potential was 1,000 volts, the residual potential was 10 volts, and the half decay exposure sensitivity was 2.5 ergs/cm 2 . Further, the electrical properties of the above prepared photoresponsive imaging member remained essentially unchanged for 1,000 cycles of repeated charging and discharging.
EXAMPLE VI
A layered photoresponsive imaging member with a hole transport layer of the copolycarbonate of Formula II, reference Example II, and an amorphous selenium photogenerator layer was fabricated as follows:
A 0.5 micron thick layer of amorphous selenium on a ball grained aluminum plate substrate of a thickness of 7 mils (175 microns) was prepared by conventional vacuum deposition techniques. Vacuum deposition was accomplished at a vacuum of 10 -6 Torr, while the substrate was maintained at about 50° C. A hole transport layer in contact with and on top of the amorphous selenium layer was obtained by coating a solution of 1.0 gram of the copolycarbonate of Formula II in 6.5 milliliters of methylene chloride using a multiple-clearance film applicator with a wet gap of 8 mils. Thereafter, the resulting imaging device was dried in a forced air oven at 40° C. for 1 hour to form a 24-micron thick transport layer. Subsequently, the imaging member was cooled to room temperature, followed by electrical testing by repeating the procedure of Example V with the exception that a 450 nanometer monochromatic light was selected for irradiation. Specifically, this imaging member was negatively charged to 850 volts and discharged to a residual potential of 2 volts. The dark decay of this device was about 10 volts/second and the half decay exposure sensitivity was 2.4 ergs/cm 2 . This device exhibited excellent cyclic stability, that is no noticeable degradation in electrical performance, for more than 10,000 cycles at which time the test was terminated.
EXAMPLE VII
An imaging member with a 10 micron-thick transport layer of the copolycarbonate of Formula II and 0.5 micron-thick amorphous selenium photogenerator layer was prepared in accordance with the procedure of Example VI with the exception that a wet gap of 5 mils was used to coat the transport layer.
The resulting imaging device was negatively charged to 850 volts, reference Example VI, and discharged using a 450 nanometer monochromatic light. The dark decay of this device was less than 15 volts/second; its residual voltage after exposure was about 2 volts, and its half decay exposure sensitivity was 2.6 ergs/cm 2 .
EXAMPLE VIII
A layered photoresponsive imaging member with a hole transport layer of the copolycarbonate VI of Example IV, and an amorphous selenium photogenerator layer was fabricated as follows:
A 0.5 micron thick layer of amorphous selenium on a ball grained aluminum plate substrate of a thickness of 7 mils was prepared in accordance with the procedure of Example VI. A hole transport layer in contact with and on top of the amorphous selenium layer was obtained by coating a solution of 1 gram of the copolycarbonate of Formula VI in 10 milliliters of methylene chloride by means of a multiple-clearance film applicator. Thereafter, the resulting imaging member was dried in a forced air oven at 40° C. for 1 hour to form an 18 microns thick transport layer. Subsequently, the imaging member was cooled to room temperature, followed by electrical testing by repeating the procedure of Example V with the exception that a 450 nanometers monochromatic light was selected for irradiation. Specifically, this imaging member was negatively charged to 900 volts and discharged to a residual potential of 90 volts. The half decay exposure sensitivity for this member was 3.5 ergs/cm 2 . The electrical performance of this imaging member remained essentially the same after 1,000 cycles of repeated charging and discharging.
EXAMPLE IX
A photoresponsive device with a transport layer of the copolycarbonate of Formula II, reference Example II, and a squarylium pigment as the photogenerator was prepared as follows:
A ball grained aluminum substrate was coated with a solution of 1 milliliter of 3-aminopropyltrimethoxysilane in 100 milliliters of ethanol. The coating was heated at 110° C. for 10 minutes resulting in the formation of a 0.1 micron thick polysilane layer. A dispersion of a photogenerator prepared by ball milling a mixture of 0.075 gram of bis(N,N'-dimethylaminophenyl)squaraine and 0.13 gram of Vitel PE-200 polyester (Goodyear) in 12 milliliters of methylene chloride for 24 hours was then coated on top of the above silane layer. After drying the coating in a forced air oven at 135° C. for 6 minutes, a 0.5 micron thick squarylium photogenerating layer was obtained.
A solution for the transport layer was prepared by dissolving 1.0 gram of the copolycarbonate of Formula II in 8 milliliters of methylene chloride. This solution was then coated over the above photogenerator layer using a multiple-clearance film applicator. The resulting device was dried in a forced air oven at 135° C. for 30 minutes resulting in a 22 microns thick transport layer.
Electrical testing was accomplished by repeating the procedure of Example V. Specifically, the above prepared imaging member was charged negatively to 1,000 volts and discharged with 830 nanometers monochromatic light. For this imaging device, the dark decay was less than 25 volts/second, and the half decay exposure sensitivity was 2.7 ergs/cm 2 .
EXAMPLE X
A layered photoresponsive imaging member with a transport layer of the copolycarbonate of Formula II doped with bis(m-anisyl)-4-biphenylylamine, and a trigonal selenium photogenerator was prepared as follows:
An aluminized Mylar substrate of a thickness of 75 microns with a silane charge blocking layer and an adhesive layer was prepared in accordance with the procedure of Example V. A dispersion of trigonal selenium and poly(N-vinylcarbazole) was prepared by ball milling 1.6 grams of trigonal selenium and 1.6 grams of poly(N-vinylcarbazole) in 14 milliliters each of tetrahydrofuran and toluene. Thereafter, 10 grams of the resulting slurry was diluted with a solution of 0.25 gram of bis(m-methoxyphenyl)-4-biphenylylamine in 5 milliliters each of tetrahydrofuran and toluene. A 1.0 micron thick photogenerator layer was fabricated by coating the above dispersion onto the adhesive layer present on the above Mylar substrate using a multiple-clearance film applicator, followed by drying in a forced air oven at 135° C. for 5 minutes. A solution for the hole transport layer was then prepared by dissolving 0.15 gram of bis(m-anisyl)-4-biphenylylamine and 1.0 gram of the copolycarbonate of Formula II in 10 milliliters of methylene chloride. This solution was then coated over the photogenerator layer by means of a multiple-clearance film applicator. The resulting member was dried in a forced air oven at 130° C. for 30 minutes resulting in an 25 microns thick transport layer.
Electrical testing of the above prepared imaging member was then accomplished by repeating the procedure of Example V. Specifically, this imaging member was negatively charged to 1,100 volts and exposed to white light of wavelengths of 400 to 700 nanometers. The dark decay was less than 30 volts/second, and the half decay exposure sensitivity of this device was 2.3 ergs/cm 2 . The electrical properties of this device remained substantially the same after 1,000 cycles of repeated charging and discharging.
Latent images may be developed on the above imaging members with known dry or liquid developers, including those illustrated in U.S. Pat. Nos. 4,298,672; 3,590,000; 4,560,635 and 4,797,342, the disclosures of which are totally incorporated herein by reference, and the like; subsequently transferring the image to a substrate such as paper and affixing the image thereto with, for example, heat.
Although the invention has been described with reference to specific preferred embodiments, it is not intended to be limited thereto, rather those skilled in the art will recognize variations and modifications may be made therein which are within the spirit of the invention and within the scope of the following claims. | A photoconductive imaging member comprised of a photogenerating layer, and a charge transport layer comprised of diaryl biarylylamine copolymers of the formula ##STR1## wherein A and B are independently selected from bifunctional linkages; Z is alkylenedioxy, arylenedioxy, or substituted derivatives thereof; R and R' are alkyl, aryl, substituted alkyl, substituted aryl, alkoxy, or halogen; x and y are mole fractions wherein x and y are greater than 0 and the sum of x and y is equal to 1.0; a and b are the numbers 0, 1 or 2; and n represents the number of monomer segments. | 2 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates generally to transmitting data to a playback device. More particularly, the present invention relates to transmitting a services list to a playback device.
[0003] 2. Background Art
[0004] Blu-ray players and other digital video disc playback devices allow users to connect to the Internet to access additional features and data during playback of Blu-ray Discs and other digital discs. Many digital video discs have incorporated capabilities to allow users to access their accounts on numerous third-party services, including social networking services such as Facebook, Twitter, and Google Plus (Google+).
[0005] Presently, a digital video disc, such as a Blu-ray Disc, provides capability for users to access accounts on a fixed number of third-party services. While the availability of new and existing third-party services may change over time, present digital video discs are hard-coded with a fixed set of supported third-party services that may be managed from menu options. In order to gain access to additional third-party services unavailable on a particular digital video disc, users may have to purchase or exchange for newly updated discs with updated support code, which may be costly and inconvenient.
[0006] Accordingly, there is a need to overcome the drawbacks and deficiencies in the art by providing a method that provides updated access to third-party services on digital video discs without resorting to replacement discs.
SUMMARY OF THE INVENTION
[0007] There is provided systems and methods for transmitting a services list to a playback device, substantially as shown in and/or described in connection with at least one of the figures, as set forth more completely in the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] The features and advantages of the present invention will become more readily apparent to those ordinarily skilled in the art after reviewing the following detailed description and accompanying drawings, wherein:
[0009] FIG. 1 presents an environment in which a mediator server may support transmitting a services list to a playback device, according to one embodiment of the present invention;
[0010] FIG. 2 presents a diagram of a menu displaying the services list transmitted to a playback device;
[0011] FIG. 3 a presents a diagram of the menu from FIG. 2 presenting the updated services list, according to one embodiment of the present invention;
[0012] FIG. 3 b presents a diagram of the menu from FIG. 3 a displaying an activation interface for creating an activation request, according to one embodiment of the present invention;
[0013] FIG. 3 c presents a diagram of the menu from FIG. 3 b displaying a login success interface in response to a successful verification of an activation request, according to one embodiment of the present invention;
[0014] FIG. 4 a presents a diagram of a display device displaying a pop-up menu and a text message dialog, according to one embodiment of the present invention;
[0015] FIG. 4 b presents a diagram of a display device displaying the pop-up menu from FIG. 4 a and a services interface, according to one embodiment of the present invention;
[0016] FIG. 4 c presents a diagram of a display device displaying the pop-up menu from FIG. 4 b and a success dialog, according to one embodiment of the present invention; and
[0017] FIG. 5 shows a flowchart describing the steps, according to one embodiment of the invention, by which a services list may be transmitted to a playback device, according to one embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0018] The present application is directed to a system and method for transmitting a services list to a playback device. The following description contains specific information pertaining to the implementation of the present invention. One skilled in the art will recognize that the present invention may be implemented in a manner different from that specifically discussed in the present application. Moreover, some of the specific details of the invention are not discussed in order not to obscure the invention. The specific details not described in the present application are within the knowledge of a person of ordinary skill in the art. The drawings in the present application and their accompanying detailed description are directed to merely exemplary embodiments of the invention. To maintain brevity, other embodiments of the invention, which use the principles of the present invention, are not specifically described in the present application and are not specifically illustrated by the present drawings.
[0019] FIG. 1 presents an environment in which a mediator server may support transmitting a services list to a playback device, according to one embodiment of the present invention. Environment 100 includes display device 101 , playback device 102 , network 140 , servers 141 , 142 , and 143 , application programming interface (API) 150 , and mediator server 161 . Playback device 102 includes device memory 103 , digital video disc 107 , and device processor 106 . Device memory 103 includes credential file 104 and device application 105 . Digital video disc 107 includes disc application 108 . Mediator server 161 includes processor 162 and memory 163 . Memory 163 includes services list 164 and mediator application 165 .
[0020] Display device 101 may be any type of visual output device such as a liquid crystal display (LCD) television, for example. Display device 101 may be connected to playback device 102 through a wireless or physical connection. Playback device 102 may be any type of device capable of presenting audio and visual contents stored in digital video disc 107 onto display device 101 . In one embodiment as shown in FIG. 1 , playback device 102 may be a Blu-ray Disc player. Device memory 103 may be any type of computer readable storage device. Credential file 104 may comprise any type of data file. Credential file 104 may store prior history information such as, for example, previously used account login information, including usernames and passwords for prior accessed third-party services. Credential file 104 may be encrypted or otherwise protected from unauthorized access. Device processor 106 may be any type of computing processor. Device application 105 may be a software application executed by device processor 106 to direct the behavior of playback device 102 . Digital video disc 107 may comprise any type of optical data disc or another physical media format, such as a flash memory card. In one embodiment, digital video disc 107 may be a Blu-ray Disc. Disc application 108 may be a software application used by playback device 102 for media playback or to present other functionalities, such as menu options, from digital video disc 107 .
[0021] In one embodiment, mediator server 161 may be any type of server machine. Processor 162 may be any type of processor. Memory 163 may be any type of machine-readable digital data storage device. Services list 164 may be an updatable data file comprising a list of third-party services presently recognized by mediator server 164 . Mediator application 165 may be a software application executed and controlled by processor 162 . Application programming interface 150 may comprise a data file containing a set of rules and specifications for implementing the interfaces of software applications. Both disc application 108 and mediator application 165 may be implemented in conformity to a common application programming interface 150 . Accordingly, mediator server 161 , using mediator application 165 , and playback device 102 , using disc application 108 , may communicate through a common application programming interface 150 . Accordingly, when mediator application 165 is updated to reflect additional functionalities, mediator application 165 may still fully communicate with device processor 106 , executing disc application 108 . In one embodiment, application programming interface 150 may reside within mediator server 161 .
[0022] In one embodiment, network 140 may comprise any type of network, such as the Internet. Servers 141 - 143 may represent server hardware clusters or data centers connected to network 140 . In one embodiment, servers 141 - 143 may host the third-party services listed in services list 164 . In alternative embodiments, other servers (not shown) may host some third-party services listed in services list 164 . Third-party services may be social networking services such as, for example, Facebook, Twitter, and Google Plus, respectively. In alternative embodiments, servers 141 - 143 may host other types of third-party services, for example e-commerce sites and other services.
[0023] In one embodiment, device processor 106 , executing disc application 108 , may send a service request for services list 164 through network 140 to mediator server 161 , and mediator application 165 may be configured to receive, from playback device 102 , that service request for services list 164 or a subset of the contents of services list 164 . In the present embodiment, the general service request may be transmitted to request the entire services list 164 . In other embodiments, a specific service request may be transmitted to request a subset of the contents of services list 164 . As an example, a specific service request may seek a list of third-party services that may perform a specific function. That specific functionality may be the capability to allow users to create and retrieve an online cash account with a balance so the user may make online purchases, for example. The returned list of third-party services may include Amazon.com or any other e-commerce sites with similar functionalities but may not include social networking sites such as Facebook, for example. The specific functionality may be associated with a category in the metadata file, as will be explained below. Therefore, in alternative embodiments, service requests may be specific service requests that contain a specific functionality, and the associated transmitted services list may comprise contents associated with that specific functionality.
[0024] In the present embodiment, the service request may comprise a BD-Live (Blu-ray Disc Live) access request from playback device 102 . When playback device 102 attempts to acquire any contents or features associated with digital video disc 107 across network 140 or to gain access to a third-party service across network 140 , playback device 102 may transmit a BD-Live access request across network 140 , as is known in the art. In alternative embodiments, a service request may comprise other types of access requests that may be transmitted to and received by mediator application 165 .
[0025] In the present embodiment, mediator application 165 may be further configured to send services list 164 for presenting on display device 101 in response to receiving the service request from playback device 102 . Sending services list 164 may cause mediator application 165 to duplicate services list 164 and send the duplicated service list 164 to playback device 102 . In one embodiment, prior to sending services list 164 , mediator application 165 may be further configured to dynamically update services list 164 to reflect a present availability of third-party services. Since some third-party services may be created and other third-party services may become inaccessible, service list 164 may require updating in order to reflect such changes. Device processor 106 , executing disc application 108 , may present services list 164 on display device 102 in response to receiving the services list 164 . Device processor 106 , executing disc application 108 , may present services list 164 by displaying services list 164 through a built-in menu of digital video disc 107 or other graphical components. In one embodiment, sending services list 164 may further comprise delivering a metadata file associated with services list 164 , wherein the metadata file comprises information categorizing the contents within services list 164 .
[0026] In other embodiments, the metadata file may be initially and automatically transmitted to playback device 102 when the user accesses a main menu setting in order to populate the main menu with selectable categories. A category may be selected and such a selection may result in a specific service request requesting a subset of the list of third-party services listed in services list 164 matching the specific function associated with the category.
[0027] In the present embodiment, even if a transmitted services list contains less than all of the contents listed in services list 164 , the metadata file may still contain all of the category information. Using the metadata file, device processor 106 , using disc application 108 , may display the contents of services list 164 in several categories based on, for example, the operational functionalities associated with the contents. In order to use display area economically, device processor 106 may not present all categories in the metadata list.
[0028] In one embodiment, after presenting services list 164 onto display device 101 , device processor 106 , executing disc application 108 , may transmit an activation request for a third-party service listed in services list 164 . Transmitting the activation request from playback device 102 may further comprise accessing credential file 104 in order to obtain an account login information. As previously explained, credential file 104 may contain prior history information including an account login information. The account login information may be stored within the activation request and transmitted to mediator server 161 to facilitate activating a third-party service from the mediator server 161 .
[0029] In one embodiment, mediator application 165 may be configured to receive from playback device 102 , an activation request for a third-party service listed in services list 164 . In order for mediator application 165 to access a third-party service listed in services list 164 , a user of playback device 102 may be initially required to create and send an activation request for that third-party service listed in services list 164 to mediator server 161 . Descriptions for FIGS. 3 a , 3 b , and 3 c below will further describe how to create an activation request. Mediator server 161 , using mediator application 165 , may activate that third-party service associated with the activation request in response to receiving the activation request. In this instance, the third-party service may be a social networking service, such as Facebook, for example. In one embodiment, mediator server 161 , using mediator application 165 , may activate the third-party service by establishing a connection to that third-party service, which may be hosted within any one of server 141 - 143 or within another location in network 140 . In one embodiment, activating the third-party service may comprise mediator application 165 , using the activation request, logging into a user account within that third-party service. As explained previously, an activation request may comprise an account login information, for example. In alternative embodiments, mediator server 161 , using mediator application 165 , may activate a third-party service by using the activation request to log into a plurality of user accounts of the third-party service. Some users may have multiple user accounts within the same third-party service, and mediator application 165 may use an appropriately created activation request to log into all of the multiple user accounts.
[0030] In one embodiment, whenever mediator server 161 , using mediator application 165 , successfully activates a third-party service, mediator server 161 may transmit a successful verification to playback device 102 through network 140 . Device processor 106 , executing disc application 108 , may update display device 101 with a login success interface in response to receiving a successful verification of the activation request. The successful verification may be any type of appropriate digital notification. Login success interface may comprise a message regarding the successful activation of the third-party service. In the present embodiment, updating display device 101 in response to a successful verification may comprise storing an account login information of the activation request back into credential file 104 if such account login information does not already exist in credential file 104 .
[0031] FIG. 2 presents a diagram of a menu displaying the services list transmitted to a playback device. Diagram 200 of FIG. 2 includes display device 250 . Display device 250 includes menu 210 . Menu 210 includes settings component 201 , account settings component 202 , share settings component 204 , and plurality of service components 205 . Plurality of service components 205 comprises service components 206 and 207 . Display device 250 corresponds to display device 101 of FIG. 1 .
[0032] In one embodiment, menu 210 may comprise a graphical user interface (GUI) of options shown on display device 250 while disc application 108 of FIG. 1 may be executing in playback device 102 of FIG. 1 . Menu 210 may be a subsection of a main menu generated from digital video disc 107 of FIG. 1 using disc application 108 of FIG. 1 . Thus, rather than being accessed through a separate application, the third-party services listed in services list 164 of FIG. 1 may be integrated directly into the built-in main or pop-up menus of digital video disc 107 . Settings component 201 may be a graphical component of menu 210 . Settings component 201 may be a conventional graphical drop down bar with additional components. Account settings component 202 may be another drop down bar within settings component 201 . Share settings component 204 may also be a drop down bar under account settings component 202 . Plurality of service components 205 may comprise the graphical presentation of services list 164 of FIG. 1 . Each of service components 206 and 207 may comprise a graphical component associated with a third-party service listed in services list 164 . Service components 206 or 207 may be used to cause mediator server 161 to access the associated third-party service that may be hosted on servers 141 - 143 of FIG. 1 , or on any other locations connected to network 140 of FIG. 1 .
[0033] As previously explained, device processor 106 of FIG. 1 may present services list 164 as plurality of service components 205 on display device 250 . In the embodiment shown in FIG. 2 , device processor 106 may present plurality of service components 205 through a built-in menu 210 . Presently, services list 164 may contain a list of the Facebook and Twitter services. Thus, service components 206 and 207 may be associated with Facebook and Twitter services, respectively. In the present embodiment of the invention as shown in FIG. 2 , service components 206 and 207 under share settings component 204 may only be used to cause mediator server 161 of FIG. 1 to activate the third-party services associated with service components 206 and 207 . Other uses for the plurality of service components 205 may be performed at other areas of menu 210 or through other built-in pop-up menus of digital video disc 107 .
[0034] In FIG. 2 , share settings component 204 may represent a category of third-party services with the specific functionality to share contents, such as status updates, across a social network. No other categories are shown in FIG. 2 . However, as previously explained, information for all available categories may be stored in the metadata file associated with services list 164 and transmitted to playback device 102 . In alternative embodiments, a user may request account settings component 202 to display more categories in the metadata file, if any exists. The user may select any of these additional categories, which may be populated with contents listed in services list 164 . Various categories may even comprise overlapping third-party service components. Therefore, in alternative embodiments, a user may have numerous categories to choose from in menu 210 in order to search for and activate a third-party service that can perform a desired functionality or service. As previously explained, the categories may be pre-determined by mediator server 161 and each displayed category may represent a functionality or service with a list of associated third-party components. For example, the categories may include any e-commerce service, online banking service, movie streaming service, or any other types of services recognized by mediator server 161 . Each of the displayed categories may be populated with additional relevant third-party components associated with existing third-party services.
[0035] FIG. 3 a presents a diagram of the menu from FIG. 2 presenting an updated services list, according to one embodiment of the present invention. Diagram 300 a of FIG. 3 includes display device 350 . Display device 350 includes menu 310 . Menu 310 comprises settings component 301 , account settings component 302 , share settings component 304 , and plurality of service components 305 . Plurality of service components 305 comprises service components 306 , 307 , and 309 . Display device 350 , menu 310 , settings component 301 , account settings component 302 , share settings component 304 , and service components 306 and 307 may correspond to display device 250 , menu 210 , settings component 201 , account settings component 202 , share settings component 204 , and service components 206 and 207 of FIG. 2 , respectively.
[0036] Menu 310 may correspond to menu 210 of FIG. 2 being accessed at a later time. Mediator server 161 of FIG. 1 may have become aware of a new third-party service since the most recent access of services list 164 , and services list 164 may be dynamically updated with new information to reflect a present availability of third-party services. Presently, device processor 106 , executing disc application 108 , may once again send a service request to mediator server 161 and may receive in return a dynamically updated services list 164 . Accordingly, plurality of service components 305 , being the graphical presentation of an updated services list 164 , may also be different from plurality of service components 205 of FIG. 2 . Plurality of service components 305 may comprise not only service components 306 and 307 , but also service component 309 . Service component 309 may be associated with a new third-party service, such as, for example, Google Plus service.
[0037] FIG. 3 b presents a diagram of the menu from FIG. 3 a displaying an activation interface for creating an activation request, according to one embodiment of the present invention. Diagram 300 b of FIG. 3 b includes display device 350 . Display device 350 includes menu 310 . Menu 310 includes settings component 301 , account settings component 302 , share settings component 304 , service components 306 , 307 , and 309 , and activation interface 320 . With respect to FIG. 3 b , elements with like numbers may correspond to similar elements in FIG. 3 a.
[0038] In FIG. 3 b , service component 306 may be selected for activation. As previously explained, in order to initially activate any third-party service, device processor 106 of FIG. 1 , using disc application 108 of FIG. 1 , may transmit an activation request to mediator server 161 of FIG. 1 for activating the third-party service associated with service component 306 . In one embodiment, the activation request may be created using activation interface 320 . Activation interface 320 may comprise GUI components that may allow the user to input any required information, such as credential information. The types of credential information required may be contained in services list 164 of FIG. 1 . In one embodiment, activation interface 320 may provide text fields for inputting a username and password of a user account of a third-party service. Activation request may be created to contain the username and password. Once the activation request is transmitted to mediator server 161 , mediator application 165 may activate the third-party service associated with service component 306 by using the activation request to log into an account within that third-party service. In the present embodiment, device processor 106 may obtain the username, password and other relevant credential information from credential file 104 and automatically input the username, password, and other relevant credential information into activation interface 320 .
[0039] FIG. 3 c presents a diagram of the menu from FIG. 3 b displaying a login success interface in response to a successful verification of an activation request, according to one embodiment of the present invention. Diagram 300 c of FIG. 3 c includes display device 350 . Display device 350 includes menu 310 . Menu 310 includes settings component 301 , account settings component 302 , share settings component 304 , service components 306 , 307 , and 309 , and login success interface 321 . With respect to FIG. 3 c , elements with like numbers may correspond to similar elements in FIG. 3 a.
[0040] Mediator server 161 of FIG. 1 , using mediator application 165 of FIG. 1 , may be configured to transmit a successful verification to playback device 102 of FIG. 1 upon successfully activating the third-party service associated with service components 306 . As explained previously, a successful activation may entail that third-party service successfully verifying the activation request and allowing mediator server 161 to log into a user account of that third-party service. Accordingly, upon a successful verification, mediator server 161 may establish access to a user account within that third-party service.
[0041] Playback device 102 , upon receiving the successful verification, may update display device 350 with login success interface 321 . If service component 306 may have already been activated or activation results in failure, then service component 306 may simply display a message stating that activation for the associated third-party service has previously been performed or has presently failed. In one embodiment, service components 306 , 307 , and 309 may only be used to activate or deactivated their associated third-party services under menu 310 .
[0042] FIG. 4 a presents a diagram of a display device displaying a pop-up menu and a text message dialog, according to one embodiment of the present invention. Diagram 400 a of FIG. 4 a includes display device 401 . Display device 401 includes movie scene 402 , selection cursor 403 , share button 404 , viewing options button 406 , exit button 408 , and text message dialog 409 . Text message dialog 409 includes individual message 407 , post message button 410 , and cancel button 411 . Display device 401 may correspond to display device 101 of FIG. 1 .
[0043] Mediator application 165 of FIG. 1 may be further configured to implement a user induced interaction for a third-party service that has been activated. The user induced interaction may comprise posting a public status update or any other interactive actions allowed by the plurality of service components during playback of content from digital video disc 107 of FIG. 1 in playback device 102 of FIG. 1 . Together, share button 404 , viewing options button 406 , and exit button 408 may comprise a pop-up menu that may be accessible while playback device 102 may be presenting movie scene 402 from digital video disc 107 . Share button 404 , viewing options button 406 , and exit button 408 may be any type of conventional graphical button. Share button 404 may be used to share a text message or post a status update with any third-party services that may be activated. Using share button 404 may cause text message dialog 409 , containing a predetermined message, to appear. Individual message 407 may be used to replace any predetermined messages in text message dialog 409 . Post message button 410 , which may be any type of graphical button, may be used to cause mediator application 165 to post individual message 407 into a third-party service. In the present embodiment, the user may direct pop-up menu to display additional buttons corresponding to additional categories from the metadata file associated with services list 164 of FIG. 1 .
[0044] FIG. 4 b presents a diagram of a display device displaying the pop-up menu from FIG. 4 a and a services interface, according to one embodiment of the present invention. Diagram 400 b of FIG. 4 b includes display device 401 . Display device 401 includes movie scene 402 , selection cursor 403 , share button 404 , viewing options button 406 , exit button 408 , and services interface 412 . Services interface 412 includes service components 413 , 414 , and 415 . With respect to FIG. 4 b , elements with like numbers may correspond to similar elements in FIG. 4 a.
[0045] In one embodiment, after using post message button 410 in FIG. 4 a , services interface 412 may appear. Any combination of service components 413 - 415 may be selected to cause mediator application 165 of FIG. 1 to transmit individual message 407 of FIG. 4 a to the third-party services associated with the selected service components 413 - 415 . In one embodiment, service component 413 may be associated with Twitter, service component 414 may be associated with Google Plus, and service component 415 may be associated with Facebook. In one embodiment, service component 415 may be selected to receive individual message 407 . Such a selection may cause mediator server 161 of FIG. 1 to post individual message 407 into an account in Facebook.
[0046] FIG. 4 c presents a diagram of a display device displaying the pop-up menu from FIG. 4 b and a success dialog, according to one embodiment of the present invention. Diagram 400 c of FIG. 4 c includes display device 401 . Display device 401 includes movie scene 402 , selection cursor 403 , share button 404 , viewing options button 406 , exit button 408 , and success dialog 416 . With respect to FIG. 4 c , elements with like numbers may correspond to similar elements in FIG. 4 a.
[0047] When mediator application 165 of FIG. 1 successfully implements a user induced interaction such as posting a status update by using service components 413 - 415 of FIG. 4 b , the status update may be displayed in the appropriate third-party services, such as a social networking service like Facebook, for example, and success dialog 416 may appear within display device 401 . Success dialog 416 may be any type of dialog with a text message indicating a successful implementing of the user induced interaction. In one embodiment, if mediator server 161 fails to post the text message into the selected third-party service, then mediator server 161 , using mediator application 165 , may display an error message on display device 401 . Furthermore, in one embodiment of the invention, if the selected third-party service has not been activated, then mediator server 161 , using mediator application 165 , may transmit a notification to playback device 102 indicating that the selected third-party service requires activation, and device processor 106 of FIG. 1 may automatically replace pop-up menu with display menu 310 of FIG. 3 b in order to allow the user to create an activation request for a selected third-party service.
[0048] FIG. 5 shows a flowchart describing the steps, according to one embodiment of the invention, by which a services list may be transmitted to a playback device, according to one embodiment of the present invention. Certain details and features have been left out of flowchart 500 that are apparent to a person of ordinary skill in the art. Thus, a step may comprise one or more sub-steps or may involve specialized equipment or materials, for example, as known the art. While steps 510 through 540 indicated in flowchart 500 are sufficient to describe one embodiment of the present method, other embodiments may utilize steps different from those shown in flowchart 500 , or may include more, or fewer steps.
[0049] Referring to step 510 of flowchart 500 in FIG. 5 and environment 100 of FIG. 1 , step 510 of flowchart 500 comprises mediator application 165 receiving, from playback device 102 , a service request for services list 164 . As previously explained, a service request, such as a BD-Live access request, for example, may contain a request services list 164 in mediator server 161 .
[0050] Referring to step 520 of flowchart 500 in FIG. 5 , environment 100 of FIG. 1 , step 520 of flowchart 500 comprises mediator application 165 sending services list 164 for presenting on display device 101 in response to receiving the service request from step 510 . As previously explained, mediator server 161 , using mediator application 165 , may transmit services list 164 to playback device 102 in response to receiving service request. Mediator server 161 may create an exact duplicate of services list 164 to send to playback device 161 .
[0051] Referring to step 530 of flowchart 500 in FIG. 5 , environment 100 of FIG. 1 and diagram 300 b of FIG. 3 b , step 530 of flowchart 500 comprises mediator application 165 receiving an activation request for a third-party service listed in services list 164 . As previously explained, playback device 102 may transmit an activation request to mediator server 161 . The activation request may be associated with a particular third-party service listed in services list 164 .
[0052] Referring to step 540 of flowchart 500 in FIG. 5 , environment 100 of FIG. 1 , step 540 of flowchart 500 comprises mediator application 165 activating a third-party service in response to receiving the activation request from step 530 . As previously explained, mediator application 165 may use information contained in the activation request to connect to the third-party service associated with the activation request by logging into an account within that third-party service.
[0053] Thus, a system and method for transmitting a services list to a playback device for a digital video disc has been disclosed. By storing an updatable services list containing information on available third-party services, mediator server may send such services list to playback device in order for playback device to present a list of dynamically adjustable third-party services for a digital video disc on a display device. Accordingly, by programming a digital video disc such as a Blu-ray disc according to an API using a mediator server, a dynamically adjustable services list may be supported without changing the disc application code.
[0054] From the above description of the invention it is manifest that various techniques can be used for implementing the concepts of the present invention without departing from its scope. Moreover, while the invention has been described with specific reference to certain embodiments, a person of ordinary skills in the art would recognize that changes can be made in form and detail without departing from the spirit and the scope of the invention. As such, the described embodiments are to be considered in all respects as illustrative and not restrictive. It should also be understood that the invention is not limited to the particular embodiments described herein, but is capable of many rearrangement, modifications, and substitutions without departing from the scope of the invention. | There is provided a device including a display and a processor to receive, from a user, a user selection of a message share setting for enabling the user to post across a plurality of social networking services, send, to a server, the user selection for enabling the user to post across the plurality of social networking services, play a video on the display, in response to a video request by the user, and receive, from the user, a request to post across the plurality of social networking services, provide a dialog entry on the display, in response to receiving the request, receive, from the user, via the dialog entry on the display, a message to be shared across the plurality of social networking services, and send, to the server, the message from the user to be posted on the plurality of social networking services. | 7 |
BACKGROUND
This invention relates generally to the art of vacuum coating, and more particularly to the art of producing vacuum coatings which maintain a metallic appearance throughout high temperature processes such as bending and laminating.
U.S. Pat. No. 3,962,488 to Gillery discloses a colorless transparent electrically conductive coating made by vacuum depositing a first layer of titanium suboxide, a second layer of silver, and a third layer of titanium suboxide. Deposition of the titanium in a less than completely oxidized state prevents the silver layer from becoming discontinuous. While the titanium suboxide may be slightly colored, it becomes colorless upon oxidation.
U.S. Pat. No. 4,990,408 to Gillery discloses a transparent article for reflecting solar energy comprising a tin/antimony oxide film which exhibits color by interference effects and a reflective metal film preferably comprising chromium, and especially chromium nitride.
Most vacuum coatings on glass which have a desirable metallic appearance as deposited lose their characteristic metallic appearance when subjected to high temperature processing. Vacuum coatings with a metallic appearance are generally metals, metal nitrides or metal carbides which oxidize when heated in air to form metal oxides which are more transparent and less absorbing. While many metals can be heated in air to the forming temperature of glass (600° to 700° C.) developing a protective oxide surface layer, the thinness of transparent metallic coatings and their consequent non-bulk, even porous nature prevent the formation of a suitable protective coating. Thus thin transparent metallic appearing films generally cannot be heated to temperatures at which glass can be bent.
SUMMARY OF THE INVENTION
Vacuum coatings with a metallic appearance as deposited can be made to retain their metallic appearance upon bending by overcoating with a different metal which forms a dense oxide. Further improvement in oxidation resistance of the metallic film can be attained by introducing additional interfaces formed by another layer of a different material, particularly an amorphous metal oxide.
DESCRIPTION OF THE DRAWINGS
FIG. 1 compares the reflectance of a heated but unoxidized metallic layer in accordance with the present invention (A) with the reflectance of an oxidized metal layer (B) and the reflectance of an unheated metallic layer (C).
FIG. 2 compares the transmittance of a heated but unoxidized metallic layer in accordance with the present invention (A) with the transmittance of a heated oxidized metallic layer (B) and the transmittance of an unheated metallic layer (C).
DESCRIPTION OF PREFERRED EMBODIMENTS
In accordance with the present invention, some of the more oxidation resistant coatings, preferably chromium nitride and titanium nitride, which nevertheless normally oxidize quite quickly at 700° C., can be protected from such oxidation by another oxidation resistant metal. The protective layer must be dense to prevent oxidation of the underlying metallic layer. Since metal oxides are generally not sufficiently dense as deposited in vacuum, the protective layer is deposited as a metal which forms a dense oxide surface layer which prevents oxidation of the underlying material. The metal of the protective layer must be different from the metal of the metallic layer in order to prevent oxidation from proceeding through the interface. Thus, for example, a titanium protective layer will prevent oxidation of a chromium nitride layer, whereas a chromium layer will not. Similarly, a titanium protective layer will not protect a titanium nitride layer from oxidation, whereas a silicon protective layer will.
An unprotected coating oxidizes upon heating, which results in higher transmittance and lower reflectance than a metallic coating protected in accordance with the present invention, as shown in FIGS. 1 and 2, as well as a hazy and translucent appearance. In contrast, a metallic appearing vacuum coating of e.g. chromium nitride or titanium nitride, protected by a different oxidation resistant layer such as titanium or silicon respectively, in accordance with the present invention, will retain its characteristic metallic reflectance, transmittance and absorbence properties upon heating to glass bending temperatures as shown in FIGS. 1 and 2. The slightly lower reflectance and higher transmittance of the heated coating are the result of oxidation of the surface of the protective layer.
Further improvement in oxidation resistance can be attained by introducing additional interfaces formed by yet another different type of material. This material is preferably glassy, e.g. an amorphous metal oxide, such as zinc-tin oxide, preferably of approximate composition Zn 2 SnO 4 .
In preferred embodiments of the present invention, the coatings are produced on a large-scale magnetron sputtering device capable of coating glass up to 100×144 inches (2.54×3.66 meters). In the following examples, the coatings are deposited on a smaller scale, using planar magnetron cathodes having 5×17 inch (12.7×43.2 centimeter) metal targets of chromium or titanium, or a 3 inch (7.6 centimeter) diameter rotating cathode of silicon. In each example, 6 millimeter thick glass substrates pass the targets on a conveyor roll at a speed of 120 inches (3.05 meters) per minute. The present invention will be further understood from the descriptions of specific examples as follows:
EXAMPLE 1
A coating of chromium nitride about 380 Angstroms thick is made by sputtering a chromium metal target (2 passes) at 7.5 kilowatts, 587 volts in pure nitrogen gas at a pressure of 4 millitorr until the luminous transmission is 9%. The coated glass is then heated for 10 minutes at 570° C. The coating is oxidized by the heat, and its transmittance curve is similar to B in FIG. 2.
EXAMPLE 2
For comparison with Example 1, a coating of chromium nitride about 380 Angstroms thick is made by sputtering a chromium metal target (2 passes) at 7.5 kilowatts, 586 volts in pure nitrogen gas until the luminous transmission is 10%. Then a layer of titanium metal about 40 Angstroms thick is deposited by sputtering a titanium target (one pass) at 0.5 kilowatts, 346 volts, until the transmission of the sample decreases to 8.9%. The sample is heated for 10 minutes at 570° C. and the coating, although its transmittance increases slightly, still has a metallic appearance, and shows spectrophotometric curves similar to (A) in FIGS. 1 and 2. When heated for 10 minutes at 625° C. the coating oxidizes.
EXAMPLE 3
A film of chromium nitride about 380 Angstroms thick applied as in the above examples to 9.6% transmission is overcoated with a layer about 60 Angstroms thick of zinc/tin oxide of approximate composition Zn 2 SnO 4 made by sputtering a zinc-tin alloy target of Zn-2Sn composition at 1.8 kilowatts, 346 volts in a mixture of 50% oxygen, 50% argon by volume. The transmittance is 10.2%. Finally a layer of titanium metal about 40 Angstroms thick is applied as in Example 2 until the transmittance is 8.7%. The coating remains metallic in appearance after heating for 10 minutes at 570° C. and 10 minutes at 625° C.
EXAMPLE 4
For comparison with Example 3, a coating with the same chromium nitride and titanium layers as in Example 3, but having a layer of titanium oxide about 40 Angstroms thick between the other two layers, is made by sputtering a titanium target at 8 kilowatts, 532 volts, in a 50% argon-oxygen mixture at a pressure of 4 millitorr (2 passes). The transmittance rises from 9.5% to 10.4%. The coating is oxidized after heating for 10 minutes at 625° C.
EXAMPLE 5
A coating with the same chromium nitride and titanium layers as in Example 3, but having a layer of titanium nitride about 40 Angstroms thick between the other two layers, is made by sputtering a titanium target (one pass) at 6 kilowatts, 598 volts, in an atmosphere of pure nitrogen at a pressure of 4 millitorr. The coating is completely oxidized after heating for 10 minutes at 625° C.
EXAMPLE 6
A layer of titanium nitride about 450 Angstroms thick is deposited by sputtering a titanium metal target in pure nitrogen gas at a pressure of 4 millitorr. The voltage is 764 volts and the power 8 kilowatts. After 4 passes the transmittance is 23.5%. The color is bluish metallic. After heating in air for 10 minutes at 570° C., the coating is completely oxidized.
EXAMPLE 7
For comparison with Example 6, a layer of titanium nitride about 500 Angstroms thick is deposited as in Example 6. The transmittance is 20.2%. A layer of silicon about 200 Angstroms thick is deposited by sputtering an Airco Coatings Technology C-Mag rotary cathode having silicon target material at 1 kilowatt, 583 volts (2 passes). The transmittance is 10.8%. After heating for 10 minutes at 625° C., the coating is still bluish and metallic appearing.
EXAMPLE 8
A layer of titanium nitride about 470 Angstroms thick is applied as in Example 6. The transmittance is 22.8%. A layer of silicon nitride about 100 Angstroms thick is applied from a C-Mag cathode as in Example 7, by sputtering a silicon target at 3 kilowatts, 416 volts in pure nitrogen gas at 4 millitorr. The transmittance rises to 25% after a single pass. The appearance of the sample is unchanged after heating for 10 minutes at 625° C.
The above examples are offered only to illustrate the present invention. Other metal, metal nitride and metal carbide metallic appearing films may be protected from oxidation by dense oxide surface forming metal layers as described above. Deposition conditions will vary according to equipment and material being deposited. Coating thicknesses can be varied to produce the desired reflectance and transmittance properties. The scope of the present invention is defined by the following claims. | A heat processable metallic appearing coated article is prepared by coating a glass substrate with a metal-containing film such as chromium or titanium nitride, which ordinarily oxidizes at high temperature, and overcoating with a protective layer of a different metal which forms a dense oxide surface layer. The coated article is subjected to high temperature processing such as bending without losing its metallic appearance to oxidation. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to a powertrain for a motor vehicle, and, more particularly, to a powertrain having multiple power sources including an electric motor for driving a set of vehicle wheels.
2. Description of the Prior Art
In a powertrain for a hybrid electric vehicle (HEV), inertial masses and drag losses offset the fuel economy, performance, and dynamic response gains of the hybrid system. These offsets are greater when the hybrid drive components are not substituted for standard powertrain components.
Electric rear axle drive units for front wheel drive vehicles add additional components and thus inertias and drag losses in both electric all wheel drive and shaft-driven mechanical all wheel drive systems. Electric front axle or rear axle drives for rear wheel drive vehicles added on top of the existing longitudinal driveline present the same problems.
The inertial masses include the added motor/generator rotor, gear assemblies, and shaft and hub assemblies. The drag losses include the additional gear and bearing losses of the drive components and electromagnetic drag losses in motor assemblies. The various drag losses can be reduced by design detail, but cannot be eliminated.
These inertias and drag torques are further multiplied by the gear ratios often present between the motor/generator and their mechanical outputs to the drivetrain.
It would be desirable to reduce the effects of inertial masses and drag torques, especially when the electric drive is not in operation. A need exists for a technique to connect and disconnect an electric motor for a front axle drive or rear axle drive motor from the driveline or the respective axle so that inertia and drag losses can be reduced. Controlled hydraulically-actuated friction clutches for this purpose increase the complexity of a hydraulic system and fluidic drag losses.
SUMMARY OF THE INVENTION
A drive unit for transmitting power to the wheels of a motor vehicle includes an input driveably connectable to a first power source, a final drive gear set driveably connectable to the wheels, a motor/generator including a stator and a rotor arranged about an axis, the rotor being able to rotate about the axis and to move along the axis relative to the stator, a gear unit arranged about the axis and driveably connected to the gear set for driving the gear set at a speed that is less than a speed of the rotor, and a coupler secured to the rotor for alternately coupling the rotor and the gear unit mutually and transmitting power therebetween and decoupling the rotor and the gear unit mutually.
The drive unit improves fuel efficiency, performance, and dynamics of a HEV with an electric front axle drive unit or a rear axle drive unit by connecting and disconnecting an electric motor from the driveline or the respective axle thereby reducing inertia and drag losses.
The drive coupling and decoupling can be used in a powertrain that includes a modular hybrid transmission (MHT) and an integrated starter generator (ISG). In a MHT system, the ISG motor is coupled or decoupled to the engine and transmission depending on the relative magnitudes of motoring, electric power generating and engine starting or braking desired.
The motor provides both axial displacement and rotation in one unit. Rotation and displacement can be controlled separately, providing two fully independent degrees of freedom.
The scope of applicability of the preferred embodiment will become apparent from the following detailed description, claims and drawings. It should be understood, that the description and specific examples, although indicating preferred embodiments of the invention, are given by way of illustration only. Various changes and modifications to the described embodiments and examples will become apparent to those skilled in the art.
DESCRIPTION OF THE DRAWINGS
The invention will be more readily understood by reference to the following description, taken with the accompanying drawings, in which:
FIG. 1 is a schematic diagram of a powertrain for a hybrid electric vehicle, whose rear axle shafts are driven by an electric rear axle drive (ERAD) unit;
FIG. 2 is a schematic diagram of a drive unit that includes a motor having two degrees of freedom;
FIG. 3 is a schematic diagram of the drive unit of FIG. 2 , in which the motor is decoupled from the output;
FIG. 4 is a schematic diagram of a second embodiment of a drive unit that includes a motor having two degrees of freedom;
FIG. 5 is a schematic diagram of the drive unit of FIG. 4 , in which the motor is decoupled from the prop shaft and engine input; and
FIG. 6 is a schematic diagram of a third embodiment of a drive unit, in which the motor is decoupled from both the output and the prop shaft and engine input.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The powertrain 10 for a hybrid electric motor vehicle illustrated in FIG. 1 includes an IC engine 12 , a transmission 14 , which drives a front final drive unit 16 connected to a pair of front wheels 18 , 19 by front drive shafts 20 , 21 . Transmission 14 may be a manual gearbox or any type of automatic transmission. The front final drive unit 16 also drives a rear drive take-off unit 22 , which is connected to an electric rear drive unit 24 by a longitudinal prop shaft 26 . Drive unit 24 is driveably connected to a pair of rear wheels 28 , 29 by rear drive shafts 30 , 31 . Drive unit 24 includes a casing 32 , which is prevented from rotating by being secured to the vehicle chassis, contains the inboard ends of the rear drive shafts 30 , 31 .
FIG. 2 shows an electric machine, such as a motor/generator 34 , arranged longitudinally in a drive unit 16 , 24 and having two degrees of freedom including rotation of rotor 36 about axis 37 and displacement of the rotor along the axis.
The rotor 36 of electric machine 34 is a hollow rotor, which is connected by a sleeve shaft 38 to a speed reduction planetary gear unit 40 . The stator 42 of electric machine 34 is secured to casing 32 . The drive unit input, prop shaft 26 , is driveably connected to a shaft 44 , which is secured to a final drive gear set that includes bevel pinion 46 . A bevel gear 48 meshing with bevel pinion 46 is secured to a ring gear of a differential mechanism 50 , which drives the axle shafts 30 , 31 and wheels 28 , 29 .
Differential 50 may be of the type comprising a ring gear that rotates about the laterally directed axis of drive shafts 30 , 31 , a spindle driven by the ring gear and revolving about the lateral axis, bevel pinions secured to the spindle for revolution about the lateral axis and rotation about the axis of the spindle, and side bevel gears meshing with the bevel pinions, each side bevel gear being secured to one of the drive shafts 30 , 31 .
Under low vehicle speed driving conditions, the electric motor/generator 34 is used to drive the vehicle with the engine 12 stopped, in which case the rear wheels 28 , 29 are driven through the speed reduction planetary gear unit 40 and the differential mechanism 50 . Under heavier load at low vehicle speed, the motor/generator 34 can be used to supplement power produced by the engine 12 . At higher vehicle speed, engine 12 is the primary power source for driving wheels 28 , 29 through prop shaft 26 , shaft 44 , bevel pinion 46 , bevel gear 48 , and differential mechanism 50 .
The motor/generator 34 is controlled by an electronic control unit (ECU) 52 . Electric power and rotating power are generated by the motor/generator 34 and by a starter/generator 54 , which alternately drives and is driven by the engine 12 . Both the motor/generator 34 and the starter/generator 54 alternately draw electric current from and supply electric current to a traction battery 64 and an auxiliary battery 66 . The traction battery 64 is a high voltage unit. The auxiliary battery 66 is a 12V unit for the supply and control of the vehicle electrical systems.
The engine 12 drives the front wheels 18 , 19 through transmission 14 , the front final drive unit 16 and the front drive shafts 20 , 21 , while also driving the rear wheels 28 , 29 through the rear take-off unit 22 , prop shaft 26 , drive unit 24 and the rear drive shafts 30 , 31 .
The speed reduction planetary gear unit 40 includes a sun gear 70 , ring gear 72 , a carrier 74 secured to shaft 44 , and a set of planet pinions 76 , supported for rotation on carrier 74 and meshing with ring gear 72 and sun gear 70 . Ring gear 72 is grounded on casing 32 . Sun gear is connected by a spline 78 to shaft 38 , which is secured to rotor 36 . The angular velocity of rotor 36 , shaft 38 and sun gear 70 is preferably about three times greater than that of carrier 98 , shaft 44 and bevel pinion 46 , although a greater speed reduction can be provided by gear unit 40 between rotor and pinion 46 .
FIG. 3 shows rotor 36 displaced leftward from the position of FIG. 2 along the axis of prop shaft 26 while supported by bearings 80 , 82 , located between the prop shaft and rotor. The spline 84 on the end of shaft 38 is formed with axially-directed teeth that disengage the axially-directed teeth of the spline 78 that is formed on sun gear.
In operation, when rotor 36 is in the position shown in FIG. 2 , engine 12 and rotor 36 are driveably connected to sun gear 70 . When electric power is provided to motor/generator 34 and engine 12 is operating, they transmit power to axle shafts 30 , 31 through differential 50 . Carrier 74 drives shaft 44 at a reduced speed compared to that of rotor 36 and sun gear 70 , and the bevel pair 46 , 48 produces an additional speed reduction at the input of differential 50 .
When rotor 36 is in the position shown in FIG. 3 , motor/generator 34 is driveably disconnected from axle shafts 30 , 31 , which are driven by engine 12 through bevel pinion 46 , bevel gear 48 and differential 50 . The rotor 36 of motor/generator 34 , therefore, has two degree of freedom: rotation about the axis of prop shaft 26 and axial displacement along the prop shaft. Such motors are often referred to as “helical” or “X-theta” (X-θ) motors. Alternatively, a standard rotary motor/generator can be used as a replacement for motor/generator 34 to drive the axle shafts 30 , 31 and for regenerative braking, and a separate linear mechanism, such as an actuated shift rail, alternately connects its rotor to shaft 44 and disconnects its rotor from shaft 44 .
FIG. 4 illustrates a motor/generator 34 , whose rotor 36 rotates about axis 37 and moves along the axis. A prop shaft 84 , functionally similar to prop shaft 26 , is formed with a spline 86 having axial teeth, which alternately engage and disengage the axial spline teeth 88 formed on rotor shaft 90 . The opposite end of rotor shaft 90 is a spline 92 having axial teeth, which continually engage the long axial spline teeth 94 formed on shaft 96 , which is secured to sun gear 78 .
FIG. 5 illustrates the rotor 36 and rotor shaft 90 displaced axially rearward such that rotor shaft 90 is disconnected from prop shaft 84 and remains connected to sun gear 78 .
In operation, when rotor 36 is in the position shown in FIG. 4 , rotor 36 and prop shaft 84 are driveably connected to sun gear 70 . When electric power is provided to motor/generator 34 , it transmits power to gear unit 40 . When engine 12 is operating, the engine transmits power to gear unit 40 . Carrier 74 drives shaft 44 at a reduced speed compared to that of rotor 36 , and the bevel pair 46 , 48 produces an additional speed reduction at the input of differential 50 . Axle shafts 30 , 31 are driven through differential 50 .
When rotor 36 is in the position shown in FIG. 5 , the engine 12 and prop shaft 84 are disconnected from gear unit 40 and the axle shafts 30 , 31 . When electric power is provided to motor/generator 34 , rotor 36 drives gear unit 40 , which transmits power to axle shafts 30 , 31 through differential 50 .
FIG. 6 illustrates a motor/generator 34 , whose rotor 36 rotates about axis 37 and moves along the axis. The prop shaft 84 is formed with a spline 86 having axial teeth, which alternately engage and disengage the axial spline teeth 88 formed on rotor shaft 90 . The opposite end of rotor shaft 90 is formed with a spline having axial teeth 92 , which alternately engage and disengage the long axial spline teeth 98 formed on shaft 100 , which is secured to sun gear 78 .
In operation, when the power unit of FIG. 6 is in the position shown in FIG. 4 , rotor 36 and prop shaft 84 are driveably connected to sun gear 70 . When electric power is provided to motor/generator 34 , it transmits power to gear unit 40 . When engine 12 is operating, the engine transmits power to gear unit 40 . Carrier 74 drives shaft 44 at a reduced speed compared to that of rotor 36 , and the bevel pair 46 , 48 produces an additional speed reduction at the input of differential 50 . Axle shafts 30 , 31 are driven through differential 50 .
When the power unit is in the position shown in FIG. 6 , both the engine 12 and rotor 36 are disconnected from gear unit 40 and the axle shafts 30 , 31 .
Although FIG. 1 illustrates a drive unit 24 and axle shafts 30 , 31 located at the rear of the vehicle, the drive unit illustrated in FIGS. 2-6 may also be used to drive the front shafts 20 , 21 , in which case the drive unit is located in the front final drive unit 16 .
The drive units of FIGS. 1-6 can be driven by a permanent magnet motor, induction motor, switched reluctance motor, variable reluctance motor, Halbach array, stepper, Sawyer, or other motor types. The drive unit may include one or more of the following: one moving translational rotor shaft assembly with both a one degree-of-freedom rotary stator and a one degree-of-freedom linear stator core; multiple standard rotary stator cores used to add a thrust on one rotor shaft; multiple standard linear stator cores used to add rotation on one rotor shaft; and a standard inside stator and outside stator with one moving rotor shaft assembly. Using Halbach array motors for inside and outside system designs can add higher strength and efficiency and easier field decoupling.
A suitable multiple degree-of-freedom motor system could include dual, helically wound, in-line cores with helical flux that can be controlled by variable frequency for independent thrust and rotation. HEV use would tend towards angles set primarily in the rotational direction, with field harmonics, such as in the lower frequencies, controlling axial thrust and position.
In accordance with the provisions of the patent statutes, the preferred embodiment has been described. However, it should be noted that the alternate embodiments can be practiced otherwise than as specifically illustrated and described. | A drive unit for transmitting power to wheels of a motor vehicle includes an input driveably connectable to a first power source, a final drive gear set driveably connectable to the wheels, a motor/generator including a stator and a rotor arranged about an axis, the rotor being able to rotate about the axis and to move along the axis relative to the stator, a gear unit arranged about the axis and driveably connected to the gear set for driving the gear set at a speed that is less than a speed of the rotor, and a coupler secured to the rotor for alternately coupling the rotor and the gear unit mutually and transmitting power therebetween and decoupling the rotor and the gear unit mutually. | 1 |
The U.S. Government has certain rights in this invention pursuant to a contract with the Department of Energy No. DE-AC02-80ER10588. A002.
TECHNICAL FIELD
This invention relates to chemical synthesis and, in particular, to the production of fine powders of metallic oxides, such as titania, zirconia, zinc oxides and the like.
BACKGROUND OF THE INVENTION
Advances in ceramic processing have permitted the replacement of various components of electrical and mechanical equipment with sintered ceramic parts. For example, ceramics have found widespread use in electronic components, cutting tools and, to a lesser degree, as structural substitutes for metal parts in engines and other machinery. Lightweight ceramic parts are, in fact, preferable in many applications because of their refractory properties and chemical inertness. However, the properties exhibited by ceramic materials are determined by the sintered microstructure and under present processing techniques the properties can be highly variable depending, in large part, upon the quality of the starting powder. In some industries the cost of rejection of ceramic parts at various processing stages (i.e., raw material inspection, part shaping, firing and finishing) can approach a cumulative 50 percent of the total manufacturing cost.
Typically, the process of manufacturing ceramic parts begins with the packing of a metallic oxide powder into a mold (or otherwise shaping and compressing) to form a so-called "green body" that is subsequently sintered at high temperature to yield the ceramic material.
In some applications, a porous ceramic body is desired, for example, chemically inert porous structures can serve as filter membranes, chromatography substrates, catalytic substrates and gas sensors (when appropriately doped). For such porous applications, the green bodies are typically formed at about 40 to 50 percent of their maximum density. In other applications, where structural strength is most important, the preferred density of the green body ranges from about 60 to about 70 percent so that the final ceramic part can approach its theoretical maxiumum density upon sintering.
A wide variety of prior art techniques for producing sinterable powders are known. Most conventional techniques begin with the heating (calcining) of metallic nitrates or hydroxides followed by pulverizing and further grinding to yield metallic oxide powders. Two basic problems with these techniques have been the large size distributions (i.e., from about 0.5 micron to about 10 micron) and the irregular shape of the particles. Because of these factors, orderly packing of powders into green bodies has been difficult and sintering at high temperatures (i.e., 1700° C.) has been necessary. Accordingly, sintered microstructures (and properties) have not been readily controlled.
It has also been suggested that metallic oxides can be precipitated by hydrolysis of metal alkoxides from liquid solutions. See generally, Mazdiyasni et al., "Preparation of Ultra-High-Purity Submicron Refractory Oxides", Vol. 48, J. of Am. Ceramic Society, pp. 372-375 (1965). However, the particles formed by this method are extremely small (average size: 100 to 200 angstroms) and tend to agglomerate, which makes effective sintering difficult unless sintering additives are utilized.
There exists a need for better methods for making fine metallic oxide powders and the like. Preferably, the powders should be monosized (or have a very small size distribution), spherical, non-agglomerated and have an optimal size of about 0.05 to about 0.7 microns (depending upon the material and specific processing plans). Such powders would find widespread use and satisfy a variety of long-felt needs in forming ceramic parts for advanced electrical, structural, and energy conversion applications.
SUMMARY OF THE INVENTION
We have discovered that uniform-size, high-purity, spherical oxide powders can be formed by hydrolysis of alkoxide precursors in dilute alcoholic solutions. Under controlled conditions (concentrations of 0.03 to 0.2M alkoxide and 0.2 to 1.5M water, for example) oxide particles on the order of about 0.05 to about 0.7 microns can be produced.
Our invention can be used to manufacture monosized, dispersed particles of a wide variety of ceramic materials, such as titania, zirconia, or zinc oxide. These materials may be doped during the production process or subsequently to yield powders suitable for electrical ceramic parts (ZnO, TiO 2 ). Moreover, because of the ideal size of our particles, sintering without additives to near their theoretical densities at lower temperatures (e.g, less than 1100° C. for TiO 2 ) is possible.
In general, the formulae for carrying out our syntheses can be described as follows: first, the metallic alkoxides react with water in the dilute alcoholic solutions according to the following reaction: ##STR1## where M is the metallic ion and x is determined by valence balancing constraints. The resulting hydroxide then condenses to form the oxides according to the formula:
M(OH).sub.x →MO.sub.y.nH.sub.2 O+H.sub.2 O (II)
Again where x and y are determined by valence considerations; the oxides then are collected as precipitates.
The invention will next be described in connection with certain preferred emodiments; however, it should be clear that various changes and modifications can be made by those skilled in the art without departing from the spirit and scope of the invention.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 is a photomicrograph of titania particles formed according to our invention. FIG. 1a is a photomicrograph of a porous titania ceramic part formed by sintering a low density compact of our particles. FIG. 1b is a photomicrograph of a non-porous titania ceramic part formed by sintering a higher density compact of our particles.
FIG. 2 is a photomicrograph of zirconia particles formed according to our invention. FIG. 2a is a photomicrograph of a non-porous zirconia ceramic part formed by sintering a higher density compact of our particles.
FIG. 3 is a photomicrograph of zinc oxide particles formed according to our invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The invention will next be described in connection with the follwing non-limiting examples:
EXAMPLE 1
TiO 2 powders were prepared by the controlled hydrolysis of a dilute alcoholic solution of titanium tetraethoxide, (Ti(OC 2 H 5 ) 4 ). Since homogeneous nucleation of particulates was desired, all liquids were ultrafiltered through 0.22 micrometer pore-size filters to minimize the level of insoluble impurities (200 proof ethanol, alkoxides, and deionized water). The alkoxide was dissolved in ethanol; water was dissolved in a separated portion of the alcohol. All work was conducted under nitrogen atmosphere. The two solutions were mixed using a magnetic stirrer giving a solution with concentrations of 0.1 to 0.2M alkoxide and 0.3 to 1.0M water. The molar ratio of water to alkoxide was 3 or greater. Subsequent precipitation of amorphous, hydrated TiO 2 occurred in 2 to 90 seconds (at room temperature); the time decreased as the concentration of either reagent was increased. (The powder was repeatedly washed with deionized water and ultrasonically dispersed in slightly basic aqueous solutions (pH=9 to 10). Alternatively, powders can be washed in other solutions depending upon the desired media for later processing. Powder compacts, prepared by gravitational or centrigugal settling of the dispersions, were vacuum dried at 160° C. and sintered in air at 1050° C.).
FIG. 1 shows a dense, uniform compact formed by sedimentation of the TiO 2 powder. The successful synthesis of the uniform-size TiO 2 powder was promoted by the simultaneous satisfaction of several conditions. First, proper reagent concentrations are necessary to promote a single-nucleation regime of homogeneous nucleation. Second, insoluble impurities should be removed from reagents to prevent heterogeneous nucleation. Third, reagents should be completely mixed prior to particle nucleation, so that nucleation occurs uniformly throughout the solution. Fourth, small particles (diameter below 0.1 micrometers) are susceptible to flocculation upon collision, especially TiO 2 under neutral dispersion conditions; thus, fast growth rates of particles from the nucleus size to about 0.1 micrometer diameter are recommended to minimize the residence time of small particles. In addition, slow stirring speeds are recommended during the growth stage; high particle collision energies from more rapid stirring results in considerable flocculation.
The TiO 2 powders produced by our process were amorphous in electron and X-ray diffraction. The particles were spherical in shape and average particle size (ranging from 0.3 to 0.7 microns) decreased for increased water concentrations and fixed alkoxide concentration, but remained essentially constant for increased alkoxide concentrations and fixed water concentration. The size distribution was very narrow for these powders (sigma about 0.09). As a rule, the size ratio of the largest particles to the smallest particles was less than 3, and the ratio of the largest particles to the mean size was less than 2.
The state of aggregation of the dispersed powder and subequent packing into green bodies, both of which significantly affect the sinterability of the compact, depend on the stability of the powder dispersion. Stability against coagulation for aqueous dispersions of oxide powders requires a low electrolyte concentration (generally less than 0.01M) and a solution pH several pH units above or below the isoelectric point (IEP) of the oxide. The IEP, the pH at which no net charge exists in the particle/liquid interface region, is between 4.5 and 6.0 for crystalline TiO 2 and was assumed to have a similar value for the amorphous powders. Hence, dispersing the TiO 2 powders in distilled water at a pH above 9 or below 4 always resulted in stable dispersion--the particles remained non-agglomerated.
Sintered microstructures clearly demonstrated the effects of powder packing uniformity on the final microstructure. Sintering a porous compact consisting of agglomerated TiO 2 powder resulted in the low density structure. Conversely, dense, uniform compacts of TiO 2 powders sintered to greater than 99% of theoretical density at 1050° C., a temperature much lower than the 1300°-1400° C. reported to sinter conventional TiO 2 powders to 97% of theoretical density. The average particle size in the green compact was 0.35 microns and the average sintered grain size was approximately 0.5 microns. FIG. 1a shows a porous titania structure and FIG. 1b shows a dense titania structure formed according to our methods and then sintered.
EXAMPLE II
Doped TiO 2 powders for varistor, grain-boundary capacitor and oxygen sensor applications were formed from dilute ethanolic solutions of titanium tetraethoxide and water. The basic procedure was identical to that described above and consisted of adding a solution of water in ethanol to one of the titanium and dopant ethoxides in ethanol and mixing; precipitation was rapid (occurring in 5 to 60 seconds at 25° C.). The donor dopant (Nb 5+ or Ta 5+ ) was incorporated uniformly in the particle through cohydrolysis of the dopant ethoxide, which had been added to the initial titanium ethoxide/ethanol solution. The overall reaction is described by: ##STR2## where D=Ta or Nb and n is about 0.5. Reagent concentrations used in the experiments were 0.1M alkoxide and about 0.3-1.5M water; all precipitation reactions were conducted under dry N 2 using 200 proof anhydrous ethanol.
The counter dopant (e.g., Ba 2+ , Sr 2+ , or Cu + ) was placed onto the powder surface by two methods: inorganic salt precipitation, performed after the powder had been washed and redispersed in water; or by metal alkoxide hydrolysis, performed immediately after the powder precipitation reaction (before washing). The first method is schematically represented by the general reaction:
D'Cl.sub.2 (aq)+(NH.sub.4).sub.2 CO.sub.3 (aq)→D'CO.sub.3 (on particles) (IV)
where D'=Ba, Sr, Cu. Carbonic acid (H 2 CO 3 ) may also be used as the carbonate source. In addition to chlorides, other halides, nitrates and sulfates may be used as the soluble inorganic salts. The metal carbonate, which is deposited on the particle surface, decomposes during sintering (prior to densification) to yield the appropriate metal oxide.
The second method, the metal alkoxide hydrolysis, is schematically represented by the general reaction
D'(OR).sub.2 +H.sub.2 O→D'(OH).sub.2 (on particle) (V)
where D'=Ba or Sr. The metal hydroxide also decomposes on heating to yield either BaO or SrO.
A wide variety of doped titania powders have been prepared using the methods outlined above. Table I summarizes the dopant combination and chemical composition (dopant level desired) of powders produced. Chemical analyses by plasma emission spectroscopy and instrumental neutron activation analysis indicated that the powders were doped to the desired levels and that dopants were not lost nor were contaminants added during handling. Moreover, the spherical shape and the narrow particle size distribution observed for pure TiO 2 were maintained.
TABLE I______________________________________DOPED TITANIA COMPOSITIONS Dopants (wt. %)Sample Ba Nb Sr Ta Cu______________________________________1 0.2 0.22 0.2 0.53 0.2 0.74 0.2 0.55 0.5 0.26 0.8 1.07 1.0 0.88 0.5 0.29 0.5 0.21011 1.0 1.012 1.0 1.013 1.0 1.014 1.0 1.015 0.116 0.517 1.018 0.1______________________________________
EXAMPLE III
Zirconia (ZrO 2 ) powders were formed with analogous reactants by the controlled hydrolysis of dilute alcoholic solutions of zirconium tetra n-propoxide or zirconium tetra isopropoxide, Zr(OC 3 H 7 ) 4 according to the general reaction: ##STR3## where n is about 2.0. The alkoxide was dissolved in ethanol. Water was dissolved in a separate portion of the alcohol. The two solutions were mixed in a glove box under nitrogen using a magnetic stirrer giving precipitation of amorphorous, hydrated ZrO 2 in 3 to 40 seconds. Reagent concentrations used in the experiments were typically about 0.03M alkoxide and about 0.21-0.48M water. The time required for precipitation decreased as the reagent concentrations were increased or as the temperature was increased. The powder was repeatedly washed with deionized water and ultrasonically dispersed in slightly basic aqueous solutions (pH=9 to 11). Powder compacts, prepared by gravitational sedimentation of the dispersions were sintered in air to >98% theoretical density at 1200° C. for the n-propoxide derived ZrO 2 powder.
FIG. 2 shows a dense, uniform compact formed by sedimentation of the spheroidal ZrO 2 powder. The ZrO 2 powders produced by our process were amorphous in X-ray diffraction. The particles were spherical in shape with a very narrow size distribution. The average particle size for the n-propoxide derived zirconia was about 0.4 microns.
Chemical analyses of the as-prepared ZrO 2 powder by plasma emission spectroscopy demonstrated the high purity of the powder with very low levels of cation impurities. Electron probe microanalysis (EPMA) and proton induced X-ray emission (PIXE) analysis of sintered ZrO 2 ceramics derived from the alkoxide produced powder showed that very low hafnia (HfO 2 ) contents (<500 ppm) are present in the isopropoxide derived powder. Furthermore, the EPMA results show that the ZrO 2 powder is not contaminated during processing to a ceramic piece.
Fig. 2a shows a zirconia structure formed according to our methods and then sintered.
EXAMPLE IV
Yttria-doped zirconia was prepared by a method analogous to that of the doped titania powders described in Example II above. The general formula for the cohydrolysis reaction was as follows: ##STR4## where R is an alkyl group such as --C 3 H 7 , y is determined by valence balancing considerations, n is about 1∝2, and D is yttrium or a similar dopant. Reagent concentrations are typically about 0.1M alkoxide and about 1.0M alkoxide and about 1.0M water. A reaction procedure analogous to that described in Example II, gives yttria-doped zirconia powders with an average size of approximately 0.2 microns. EPMA results on sintered yttria-doped zirconia ceramics demonstrate that the chemical doping is homogeneous and that very little contamination is introduced during the processing operations.
Additionally, zirconia/alumina, zirconia/spinel, and zirconia/mullite two phase materials were prepared by the controlled precipitation of zirconia onto the respective oxide powders or by the mixing of alkoxide derived zirconia with size-sorted alumina powder. EPMA results on sintered ZrO 2 /alumina, ZrO 2 /spinel, and ZrO 2 /mullite ceramics demonstrate that the desired zirconia concentrations are obtained.
EXAMPLE V
Zinc oxide powders were also prepared by the controlled hydrolysis of zinc doubles alkoxides, such as Na--Zn and Li--Zn alkoxides. Typically, the double alkoxide was dissolved in 200 proof absolute ethanol (about 0.03M solution) in a nitrogen atmosphere glove box. The solution was heated at approximately 45° C. After the zinc alkoxide was dissolved, water (about 0.56M) and ammonium hydroxide (5×10 -3 M) were added to the solution with stirring. Precipitation of hydrated zinc oxide starts about 2 minutes later. Stirring is continued for 10 additional minutes to insure a reasonably complete reaction.
The precipitation reaction may be represented by the general formula: ##STR5## where M may be Li or a similar metal and n is approximately 0.2 to 0.3. The ZnO particles produced by the hydrolysis reaction are spheroidal, have an average particle size of approximately 400 angstroms and are of high purity as indicated by plasma emission spectroscopic analyses. The Li (or similar metal) remained in solution and was not incorporated in the ZnO powder.
EXAMPLE VI
Doped zinc oxide powders were prepared by methods analogous to those discussed in Example II above. Bismuth dopant was added by the hydrolysis of bismuth isopropoxide Bi(OC 3 H 7 ) 3 (reaction V) or of bismuth trichloride BiCl 3 (reaction IV). When the isopropoxide was used, it was dissolved in hot 200 proof absolute alcohol and was added to the dispersed zinc oxide powder. The excess water left in the dispersion was sufficient to hydrolyze the isopropoxide. After washing this powder, it was either processed into ceramic pieces or was further doped with manganese. The manganese dopant was added by the precipitation of manganese carbonate (reaction IV). The powder was dispersed in an aqueous solution of manganese (II) chloride and a solution containing ammonium carbonate was poured into the first solution while stirring. The manganese dopant was precipitated as manganese carbonate on the powder surface. Chemical analyses of the doubly doped powder by plasma emission spectroscopy showed that the desired bismuth and manganese dopant levels were obtained by these methods. EPMA and PIXE analyses of sintered zinc oxide ceramics also showed that the desired dopant levels could be obtained in the ceramic piece with very low levels of impurities. | Uniform-size, high-purity, spherical oxide powders are formed by hydrolysis of alkoxide precursors in dilute alcoholic solutions. Under controlled conditions (concentrations of 0.03 to 0.2 M alkoxide and 0.2 to 1.5 M water, for example) oxide particles on the order of about 0.05 to 0.7 micron can be produced. Methods of doping such powders and forming sinterable compacts are also disclosed. | 2 |
TECHNICAL FIELD
The present invention relates to power transmissions having three planetary gear sets with a single, common carrier member. More specifically, the gear sets are controlled by six torque-transmitting mechanisms to provide six forward speed ratios and two reverse speed ratios.
BACKGROUND OF THE INVENTION
Passenger vehicles include a powertrain that is comprised of an engine, multi-speed transmission, and a differential or final drive. The multi-speed transmission increases the overall operating range of the vehicle by permitting the engine to operate through its torque range a number of times. The number of forward speed ratios that are available in the transmission determines the number of times the engine torque range is repeated. Early automatic transmissions had two speed ranges. This severely limited the overall speed range of the vehicle and therefore required a relatively large engine that could produce a wide speed and torque range. This resulted in the engine operating at a specific fuel consumption point during cruising, other than the most efficient point. Therefore, manually-shifted (countershaft transmissions) were the most popular.
With the advent of three- and four-speed automatic transmissions, the automatic shifting (planetary gear) transmission increased in popularity with the motoring public. These transmissions improved the operating performance and fuel economy of the vehicle. The increased number of speed ratios reduces the step size between ratios and therefore improves the shift quality of the transmission by making the ratio interchanges substantially imperceptible to the operator under normal vehicle acceleration.
It has been suggested that the number of forward speed ratios be increased to six or more. Six-speed transmissions are disclosed in U.S. Pat. No. 4,070,927 issued to Polak on Jan. 31, 1978; and U.S. Pat. No. 6,422,969 issued to Raghavan and Usoro on Jul. 23, 2002.
Six-speed transmissions offer several advantages over four- and five-speed transmissions, including improved vehicle acceleration and improved fuel economy. While many trucks employ power transmissions having six or more forward speed ratios, passenger cars are still manufactured with three- and four-speed automatic transmissions and relatively few five or six-speed devices due to the size and complexity of these transmissions.
SUMMARY OF THE INVENTION
A multi-speed transmission is provided having a single, common carrier member functioning for each of multiple planetary gear sets. The single carrier member allows for reduction in components and a potentially lower transmission cost.
Accordingly, a multi-speed transmission includes an input shaft and an output shaft. First, second and third planetary gear sets have a common carrier member, at least two ring gear members, and each has a sun gear member. A plurality of sets of pinion gears is rotatably mounted on the common carrier member for intermeshing with the ring gear members and the sun gear members. The input shaft is not continuously connected with any member of the planetary gear sets and the output shaft is continuously connected with a member of the planetary gear sets. Six torque-transmitting mechanisms are operable for selectively interconnecting members of the planetary gear sets with the input shaft, with a stationary member, or with other members of the planetary gear sets. The six torque-transmitting mechanisms are engaged in combinations of two to establish at least six forward speed ratios and two reverse speed ratios between the input shaft and the output shaft.
In one aspect of the invention, an interconnecting member continuously interconnects the sun gear member of one of the planetary gear sets with the sun gear member of another of the planetary gear sets.
In another aspect of the invention, one of the ring gear members intermeshes with pinion gears of both the first and second planetary gear sets.
In yet another aspect of the invention, each pinion gear is characterized by a predetermined number of teeth and rotates on a respective spindle mounted on the common carrier member at a respective bearing. Each of the spindles is of the same size and each of the bearings is of the same size.
The first and second planetary gear sets may have separate ring gear members or share a common ring gear member. If separate ring gear members are used for the first and second planetary gear sets, an interconnecting member interconnects the ring gear member of the first planetary gear set with the ring gear member of the second planetary gear set.
In yet another aspect of the invention, a first of the six torque-transmitting mechanisms is operable for selectively interconnecting the sun gear member of the second planetary gear set and the sun gear member of the third planetary gear set with the input shaft.
In still another aspect of the invention, a second of the six torque-transmitting mechanisms is operable for selectively interconnecting the common carrier member with the input shaft.
In another aspect of the invention, a third of the six torque-transmitting mechanisms is operable for selectively interconnecting the input shaft with the sun gear member of the first planetary gear set. Preferably the third torque-transmitting mechanism is disposed radially inward of the first and second torque-transmitting mechanisms, as the third torque-transmitting mechanism is characterized by higher speeds than the first and second torque-transmitting mechanisms. The radially inward position of the third torque-transmitting mechanism thereby minimizes spin losses.
In still another aspect of the invention, a fourth of the six torque-transmitting mechanisms is operable for selectively interconnecting the sun gear member of the first planetary gear set with the stationary member.
In still further aspect of the invention, a fifth of the six torque-transmitting mechanisms is operable for selectively interconnecting a ring gear member of the first and second planetary gear sets with the stationary member.
In another aspect of the invention, a sixth of the six torque-transmitting mechanisms is operable for selectively interconnecting the common carrier member with the stationary member.
A method of assembling a transmission having multiple planetary gear sets includes providing a single carrier member configured to rotatably support pinion gears for each of the planetary gear sets. The method also includes radially positioning the single carrier member within the transmission on two axially spaced bushings. Thus, the use of the single carrier member enables relatively simple and accurate positioning during assembly.
The above features and advantages and other features and advantages of the present invention are readily apparent from the following detailed description of the best modes for carrying out the invention when taken in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic representation of a powertrain including an embodiment of a planetary transmission of the present invention with an alternative single ring gear member shown in phantom;
FIG. 2 is a truth table depicting some of the operating characteristics of the powertrain shown in FIG. 1 ; and
FIG. 3 is a chart depicting other operating characteristics of the powertrain shown in FIG. 1 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to the drawings, wherein like reference numerals represent the same or corresponding parts through the several views, there is shown in FIG. 1 a powertrain 10 having a conventional engine and torque converter 12 , a planetary transmission 14 and a conventional final drive mechanism 16 .
The planetary transmission 14 includes an input shaft 17 continuously connected with the engine and torque converter 12 , a planetary gear arrangement 18 , and an output shaft 19 continuously connected with the final drive mechanism 16 . The planetary gear arrangement 18 includes three planetary gear sets 20 , 30 and 40 .
The planetary gear set 20 includes a sun gear member 22 , a ring gear member 24 , and a planet carrier assembly member 26 . The planet carrier assembly member 26 includes a plurality of pinion gears 27 (a first set of pinion gears) rotatably mounted on a carrier member 29 and disposed in meshing relationship with the sun gear member 22 . A plurality of pinion gears 28 (a second set of pinion gears) is also rotatably mounted on the carrier member 29 . The pinion gears 28 are disposed in meshing relationship with the pinion gears 27 and the ring gear member 24 .
The planetary gear set 30 includes a sun gear member 32 , a ring gear member 34 , and the same planet carrier assembly member 26 . The planet carrier assembly member 26 includes a plurality of pinion gears 37 rotatably mounted on the same carrier member 29 and disposed in meshing relationship with both the sun gear member 32 and the ring gear member 34 . Pinion gears 37 are also referred to herein as a third set of pinion gears.
In an alternative embodiment, rather than separate ring gear members 24 and 34 , a single ring gear member 24 ′ is included in both the planetary gear sets 20 and 30 . The single ring gear member 24 ′ is in meshing relationship with both the pinion gears 28 and the pinion gears 37 .
The planetary gear set 40 includes a sun gear member 42 , a ring gear member 44 , and the same planet carrier assembly member 26 . The planet carrier assembly member 26 includes a plurality of pinion gears 47 (a fourth set of pinion gears) rotatably mounted on the same carrier member 29 and disposed in meshing relationship with the sun gear member 42 . A plurality of pinion gears 48 (a fifth set of pinion gears) is also rotatably mounted on the carrier member 29 and is disposed in meshing relationship with both the ring gear member 44 and the pinion gears 47 .
Each pinion gear 27 , 28 , 37 , 47 , and 48 rotates on a spindle mounted on the common carrier member 29 at a respective bearing. For instance, pinion gear 27 rotates on a spindle 25 A mounted on carrier member 29 at bearing 21 A. Pinion gear 28 rotates on a spindle 25 B mounted on carrier member 29 at bearing 21 B. Pinion gear 37 rotates on spindle 25 C mounted on carrier member 29 at bearing 21 C. Pinion gear 47 rotates on spindle 25 D mounted on carrier member 29 at bearing 21 D. Pinion gear 48 rotates on spindle 25 E mounted on common carrier member 29 at bearing 21 E.
The use of the common carrier member 29 reduces the number of required housing walls, saving axial space and reducing the number of thrust washers required. For instance, thrust washers (not shown) may be positioned adjacent end housing walls 23 A and 23 D to absorb axial thrust. However, no thrust washers are required between gear sets 20 and 30 or between gear sets 30 and 40 , as shared housing walls 23 B, 23 C, respectively, are employed.
The input shaft 17 is not continuously connected with any member of the planetary gear sets 20 , 30 and 40 . The output shaft 19 is continuously connected with the ring gear member 44 via a drum 97 . A park lock gear 80 is also disposed on the drum 97 such that it is continuously interconnected with the ring gear member 44 and the output member 19 . The sun gear member 32 is continuously connected with the sun gear member 42 via an interconnecting member 70 . The ring gear member 24 is continuously connected with the ring gear member 34 via a drum 96 . Those skilled in the art will readily understand that a consolidation of parts is realized by utilizing an alternative embodiment having a single ring gear member 24 ′ in lieu of the separate ring gear members 24 and 34 .
The input shaft 17 is selectively connectable with the sun gear member 32 via torque-transmitting mechanism 50 which may be referred to herein as the C 1 clutch. Selective engagement of the C 1 clutch connects a drum 92 which is continuously connected with the input member 17 to an inner shaft 95 which is continuously connected with the sun gear member 32 . The input shaft 17 is also selectively connectable with the common carrier member 29 via a torque-transmitting mechanism 52 , which may also be referred to herein as the C 2 clutch. The C 2 clutch 52 selectively interconnects the drum 92 with an intermediate shaft 94 that is continuously connected with the carrier member 29 . Additionally, the input shaft 17 is also selectively connectable with the sun gear member 22 via a torque-transmitting mechanism 54 , which may also be referred to herein as C 3 clutch 54 . The C 3 clutch 54 selectively interconnects the drum 92 with an outer shaft 93 that is continuously connected with the sun gear member 22 . Torque-transmitting mechanism 56 which may also be referred to herein as the C 4 clutch 56 , selectively connects the sun gear member 22 with the transmission housing 60 , which may also be referred to herein as a stationary member. An extension or wall 62 of the transmission housing 60 extends between the drum 92 and the C 4 clutch 56 . The wall 62 provides support and oil feed for the clutches 50 , 52 and 54 . A torque-transmitting mechanism 58 , which may also be referred to herein as the C 5 clutch, selectively connects the drum 96 with the transmission housing 60 , thereby grounding the ring gear members 24 and 34 with the transmission housing 60 . If the alternative single ring gear member 24 ′ is used, the C 5 clutch 58 selectively interconnects the ring gear member 24 ′ with the transmission housing 60 . A torque-transmitting mechanism 59 selectively connects the common carrier member 29 with the transmission housing 60 . The torque-transmitting mechanism 59 may also be referred to herein as the C 6 clutch.
The Reverse 1 speed ratio is established with the engagement of the C 3 clutch 54 and the C 5 clutch 58 . The C 3 clutch 54 connects the input member 17 with the sun gear member 22 , and the C 5 clutch 58 connects the ring gear member 24 and the ring gear member 34 with the transmission housing 60 . The sun gear member 22 rotates at the same speed as the input shaft 17 . The ring gear member 24 and the ring gear member 34 do not rotate. If the alternative embodiment having the single ring gear member 24 ′ is utilized, the ring gear member 24 ′ does not rotate. The common carrier member 29 rotates as a speed determined from the speed of the sun gear member 22 and the ring gear/sun gear tooth ratio of the planetary gear set 20 . The sun gear member 32 rotates at the same speed as the sun gear member 42 . The sun gear member 32 rotates at a speed determined from the speed of the common carrier member 29 and the ring gear/sun gear tooth ratio of the planetary gear set 30 . The ring gear member 44 rotates at the same speed as the output shaft 19 . The ring gear member 44 , and therefore the output shaft 19 , rotates at a speed determined from the speed of the common carrier member 29 , the speed of the sun gear member 42 , and the ring gear/sun gear tooth ratio of the planetary gear set 40 . The numerical value of the Reverse 1 speed ratio is determined utilizing the ring gear/sun gear tooth ratios of the planetary gear sets 20 , 30 and 40 .
The Reverse Low speed ratio is established with the engagement of the C 3 clutch 54 and the C 6 clutch 59 . The C 3 clutch 54 connects the input shaft 17 with the sun gear member 22 , and the C 6 clutch 59 connects the common carrier member 29 with the transmission housing 60 . The sun gear member 22 rotates at the same speed as the input shaft 17 . The common carrier member 29 does not rotate. The ring gear member 24 rotates at the same speed as the ring gear member 34 . The ring gear member 24 rotates at a speed determined from the speed of the sun gear member 22 and the ring gear/sun gear tooth ratio of the planetary gear set 20 . The sun gear member 32 rotates at the same speed as the sun gear member 42 . The sun gear member 32 rotates at a speed determined from the speed of the ring gear member 34 and the ring gear/sun gear tooth ratio of the planetary gear set 30 . If the alternative single ring gear member 24 ′ is used in lieu of ring gear members 24 and 34 , then the speed of the single ring gear member 24 ′ is determined utilizing the speed of the sun gear member 22 and the ring gear/sun gear tooth ratio of the planetary gear set 20 . Additionally, the sun gear member 32 would then rotate at a speed determined from the speed of the single ring gear member 24 ′ and the ring gear/sun gear tooth ratio of the planetary gear set 30 . The ring gear member 44 rotates at the same speed as the output shaft 19 . The ring gear member 44 rotates at a speed determined from the speed of the sun gear member 42 and the ring gear/sun gear tooth ratio of the planetary gear set 40 . The numerical value of the Reverse Low speed ratio is determined utilizing the ring gear/sun gear tooth ratios of the planetary gear sets 20 , 30 and 40 .
The first forward speed ratio is established with the engagement of the C 1 clutch 50 and the C 6 clutch 59 . The C 1 clutch 50 connects the input shaft 17 with the sun gear member 32 , and the C 6 clutch 59 connects the common carrier member 29 with the transmission housing 60 . The sun gear member 32 and the sun gear member 42 rotate at the same speed as the input shaft 17 . The common carrier member 29 does not rotate. The ring gear member 44 rotates at the same speed as the output shaft 19 . The ring gear member 44 , and therefore the output shaft 19 , rotates at a speed determined from the speed of the sun gear member 42 and the ring gear/sun gear tooth ratio of the planetary gear set 40 . The numerical value of the first forward speed ratio is determined utilizing the ring gear/sun gear tooth ratio of the planetary gear set 40 .
The second forward speed ratio is established with the engagement of the C 1 clutch 50 and the C 5 clutch 58 . The C 1 clutch 50 connects the input shaft 17 with the sun gear member 32 , and the C 5 clutch 58 connects the ring gear member 24 (or the single ring gear member 24 ′ in the event that the alternative embodiment is used) with the transmission housing 60 . The sun gear member 32 and the sun gear member 42 rotate at the same speed as the input shaft 17 . The ring gear member 24 and the ring gear member 34 (or in the case of the alternative embodiment, the single ring gear member 24 ′) do not rotate. The common carrier member 29 rotates at a speed determined from the speed of the sun gear member 32 and the ring gear/sun gear tooth ratio of the planetary gear set 30 . The ring gear member 44 rotates at the same speed as the output shaft 19 . The ring gear member 44 , and therefore the output shaft 19 , rotates at a speed determined from the speed of the common carrier member 29 , the speed of the sun gear member 42 and the ring gear/sun gear tooth ratio of the planetary gear set 40 . The numerical value of the second forward speed ratio is determined the ring gear/sun gear tooth ratios of the planetary gear sets 30 and 40 .
The third forward speed ratio is established with the engagement of the C 1 clutch 50 and the C 4 clutch 56 . The C 1 clutch 50 connects the input shaft 17 with the sun gear member 32 , and the C 4 clutch 56 connects the sun gear member 22 with the transmission housing 60 . The sun gear member 32 and the sun gear member 42 rotate at the same speed as the input shaft 17 . The sun gear member 22 does not rotate. The ring gear member 24 rotates at the same speed as the ring gear member 34 . The ring gear member 24 (or the single ring gear member 24 ′ in case the alternative embodiment is utilized) rotates at a speed determined from the speed of the common carrier member 29 and the ring gear/sun gear tooth ratio of the planetary gear set 20 . The ring gear member 34 (or, in the event that the alternative embodiment is utilized, the single ring gear member 24 ′), rotates at a speed determined from the speed of common carrier member 29 , the speed of the sun gear member 32 and the ring gear/sun gear tooth ratio of the planetary gear set 30 . The ring gear member 44 rotates at the same speed as the output shaft 19 . The ring gear member 44 , and therefore the output shaft 19 , rotates at a speed determined from the speed of the common carrier member 29 , the speed of the sun gear member 42 and the ring gear/sun gear tooth ratio of the planetary gear set 40 . The numerical value of the third forward speed ratio is determined utilizing the ring gear/sun gear tooth ratios of the planetary gear sets 20 , 30 and 40 .
The fourth forward speed ratio is established with the engagement of the C 1 clutch 50 and the C 2 clutch 52 . The C 1 clutch 50 connects the sun gear member 32 with the input shaft 17 , and the C 2 clutch 52 connects the common carrier member 29 with the input shaft 17 . In this arrangement, all the members of the gear sets 20 , 30 and 40 rotate at the same speed as the input shaft 17 . Thus the output shaft 19 rotates at the same speed as the input shaft 17 in a direct drive relationship.
The fifth forward speed ratio is established with the engagement of the C 2 clutch 52 and the C 4 clutch 56 . The C 2 clutch 52 connects the input shaft 17 with the common carrier member 29 , and the C 4 clutch 56 connects the sun gear member 22 with the transmission housing 60 . The common carrier member 29 rotates at the same speed as the input shaft 17 . The ring gear member 24 rotates at the same speed as the ring gear member 34 . The sun gear member 22 does not rotate. The ring gear member 24 (or the single ring gear member 24 ′ in the event that the alternative embodiment is utilized) rotates at a speed determined from the speed of the common carrier member 29 and the ring gear/sun gear tooth ratio of the planetary gear set 20 . The sun gear member 32 rotates at the same speed as the sun gear member 42 . The sun gear member 32 rotates at a speed determined from the speed of the ring gear member 34 , the speed of the common carrier member 29 and the ring gear/sun gear tooth ratio of the planetary gear set 30 . The ring gear member 44 rotates at the same speed as the output shaft 19 . The ring gear member 44 , and therefore the output shaft 19 , rotates at a speed determined from the speed of the common carrier member 29 , the speed of the sun gear member 42 and the ring gear/sun gear tooth ratio of the planetary gear set 40 . The numerical value of the fifth forward speed ratio is determined utilizing the ring gear/sun gear tooth ratios of the planetary gear sets 20 , 30 and 40 .
The sixth forward speed ratio is established with the engagement of the C 2 clutch 52 and the C 5 clutch 58 . The C 2 clutch 52 connects the input shaft 17 with the common carrier member 29 , and the C 5 clutch 58 connects the ring gear member 24 with the transmission housing 60 . The common carrier member 29 rotates at the same speed as the input shaft 17 . The sun gear member 32 rotates at the same speed as the sun gear member 42 . The ring gear members 24 and 34 (or the alternative single ring gear member 24 ′) do not rotate. The sun gear member 32 rotates at a speed determined from the speed of the common carrier member 29 and the ring gear/sun gear tooth ratio of the planetary gear set 30 . The ring gear member 44 rotates at the same speed as the output shaft 19 . The ring gear member, and therefore the output shaft 19 , rotates at a speed determined from the speed of the common carrier member 29 , the speed of the sun gear member 42 and the ring gear/sun gear tooth ratio of the planetary gear set 40 . The numerical value of the sixth forward speed ratio is determined utilizing the ring gear/sun gear tooth ratios of the planetary gear sets 30 and 40 .
As set forth above, the engagement schedules for the torque-transmitting mechanisms is shown in the truth table of FIG. 2 . This truth table also provides an example of speed ratios that are available utilizing the ring gear/sun gear tooth ratios given by way of example as follows N R1 /S R1 =3.86 and N R2 /S R2 =3.00 and N R3 /S R3 =3.86. N R1 /S R1 is the tooth ratio of planetary gear set 20 ; N R2 /S R2 is the tooth ratio of the planetary gear set 30 ; and N R3 /S R3 value is the tooth ratio of the planetary gear set 40 . It should be noted that single and double step ratio interchanges are of the single transmission variety.
The chart of FIG. 3 describes the speed ratios and ratio steps that are obtained by the transmission of FIG. 1 utilizing the same tooth ratios given above. For example, the step ratio between the first and second forward speed ratios is 1.714, while the step ratio between the Reverse Low and the first forward speed ratio is −1.29. A relatively wide ratio of 6.85 is obtained between the first and sixth forward speed ratios.
Shafting requirements for the transmission 14 are minimized by: (i) interconnecting the sun gear members 32 and 42 with the drum 92 and therefore the input shaft 17 via the inner shaft 95 , (ii) by selectively interconnecting the common carrier member 29 with the drum 92 and therefore the input shaft 17 via an intermediate shaft 94 when the C 2 clutch 52 is engaged, (iii) selectively interconnecting the sun gear member 22 with the input shaft 17 via the outer shaft 93 when the C 3 clutch 54 is engaged, and (iv) by creating the shafts 93 , 94 , 95 such that they are coaxially disposed. This allows for a compact arrangement. The C 3 clutch 54 is positioned radially inward of the C 1 clutch 50 and the C 2 clutch 52 . Because the C 3 clutch 54 rotates at higher speeds than the C 1 clutch 50 and the C 2 clutch 52 , spin losses are minimized by minimizing the radially displacement of the C 3 clutch 54 from a center axis of rotation (e.g., an axis defined by the input shaft 17 and the output shaft 19 ).
In the preferred embodiment, each of the pinion gears has a common number of teeth. For instance, in the transmission 14 of FIG. 1 , the pinion gears 27 , 28 , 37 , 47 and 48 may all have 27 teeth while sun gear member 22 has 21 teeth, sun gear member 32 has 27 teeth, sun gear member 42 has 21 teeth, ring gear member 24 and ring gear member 34 (or the alternative single ring gear member 24 ′) have 81 teeth and ring gear member 44 has 81 teeth. By providing pinion gears with a common number of teeth (i.e., having a predetermined size), bearings 21 A- 21 E may have a common bearing size and spindles 25 A- 25 E may be of a common size as well.
By utilizing a single common carrier member 29 , assembly time may be reduced as only one carrier member needs to be positioned within the transmission 14 rather than three separate members. The common carrier member 29 maybe located radially with precision on bushings 64 A and 64 B. The bushings 64 A and 64 B support inner radial portions of the common carrier assembly member 26 at a specifically designed radial and axial position. Accordingly, a method of assembling a transmission having multiple planetary gear sets includes providing a single carrier member 29 configured to rotatably support pinion gears 27 , 28 , 37 , 47 and 48 for each of the planetary gear sets 20 , 30 and 40 . The method further includes radially positioning the single carrier member within the transmission 14 on two axially spaced bushing 64 A, 64 B.
It is noted that the ratio coverage between the first and sixth forward speed ratios is 6.85 to 1 which provides a relatively high useable ratio coverage. The ratio of the forward and reverse speeds may be adjusted to provide nearly equal forward and reverse ratios. Other ratio coverages may be achieved with different gear tooth counts. For instance, low gear coverage may be reduced while the amount of overdrive may be increased. A low gear first forward speed ratio of 3.222 to a sixth forward speed ratio of 0.5 provides a total usable ratio coverage of 6.44 to 1. The final selection of ratio. coverage is based on cost, assembly and application guidelines.
The transmission 14 of FIG. 1 provides pinion speeds, carrier speeds and clutch slip speeds compatible with very high engine input speeds, typical of smaller displacement, variable cam engines. With the selected tooth ratios discussed above, the C 3 clutch 54 will be characterized by speeds higher than those of the C 1 clutch 50 and the C 2 clutch 52 . Speed and torque calculations which will be readily understood by those skilled in the art (and which may be calculated based on gear tooth numbers) reveal that the transmission 14 provides very good torque sharing as the ratio steps progress, which improves durability of the transmission 14 . Additionally, those skilled in the art will readily understand that the transmission 14 is void of any internal power loops which enables a very high mechanical efficiency.
While the best modes for carrying out the invention have been described in detail, those familiar with the art to which this invention relates will recognize various alternative designs and embodiments for practicing the invention within the scope of the appended claims. | A six speed transmission is provided that includes three planetary gear sets having a common carrier member and six torque-transmitting mechanisms operated in combinations of two to provide at least six forward speed ratios and two reverse speed ratios. A method of assembling a transmission is also provided. A reduction in components and component standardization is achieved. | 5 |
RELATED APPLICATIONS
[0001] This application is a continuation of U.S. patent application Ser. No. 12/582,588, filed Oct. 20, 2009, the entirety of which is incorporated herein by reference and is to be considered part of this specification.
BACKGROUND
[0002] 1. Field of the Invention
[0003] The invention relates to the systems and methods for guiding an invasive medical device within a patient for the purpose of mapping anatomical cavities.
[0004] 2. Description of the Prior Art
[0005] Existing cardiac mapping software generates surface geometry from a location data point cloud of where the catheter has been. The chamber geometry is generated from this location data point cloud. The geometric surface location is based on the limits of the point cloud and data point density at those limits. If an insufficient number of points is gathered in a particular location, those few location points may be rejected as anomalous data and the surface will not be accurately generated. Prior art systems do not generate a sufficiently consistent and repeated motion through the cardiac region to generate a sufficient cloud density throughout the chamber.
SUMMARY
[0006] The system described herein solves these and other problems by incorporating an additional motion algorithm into a catheter guidance system that rotates the catheter about the current catheter positioning vector. As the operator moves the catheter within the desired region, the catheter rotates in a controlled manner as to produce a higher density location data point cloud. This rotation is too difficult for the operator to perform manually in a consistent manner. The motion algorithm gives the operator the effective results that would be given by a catheter with more electrodes, but allows the operator to operate in smaller regions that would be inaccessible to the larger mapping catheters.
[0007] In one embodiment, the catheter is controlled by a magnetic guidance system, such as described in patent application Ser. No. 11/697,690, Shachar, et al., “METHOD AND APPARATUS FOR CONTROLLING CATHETER POSITIONING AND ORIENTATION”. The Cartesian location of each catheter electrode is continuously recorded by mapping system and these locations are sent by network data connection to the position control system for closed-loop control of catheter position. The mapping system is used to record the location data point cloud and generate the chamber geometry while the operator uses the magnetic guidance system to manipulate the catheter about the chamber. In one embodiment, the motion algorithm is manually activated by a magnetic guidance system control button, and can be turned on or off by the operator.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 is a block diagram of the placement of the motion algorithm within a catheter mapping and navigation system.
[0009] FIG. 2 is a detailed block diagram of the motion algorithm's manipulation of the catheter positioning vector.
[0010] FIG. 3 is an illustration showing the relationship between the catheter's desired position (DP) and its modified desired position (DP*).
[0011] FIG. 4 is a vector diagram depicting the time-based calculation of DP* from DP.
DETAILED DESCRIPTION
[0012] In the field of navigating surgical tools for mapping coronary chambers or other cavities and orifices, a tool is manipulated about the chamber while a mapping system records the tool's location. These tool locations are assembled to form a location point cloud which defines the operational workspace volume. A geometric manifold representing the chamber geometry is then defined at the limits of this location point cloud. This geometry is later used by the operator as a positional reference and diagnostic tool.
[0013] The tool location is detected at each of its position detection electrodes. Some mapping catheters will have twenty or more of these electrodes, which quickly produces a very high density point cloud within the chamber. These catheters can also be very large and constructed as balloons or multiple-appendage devices. When mapping the associated vasculature of the chamber, the larger catheters either have difficulty reaching into the location or will unduly distort the tissue in an attempt to fit, so smaller catheters are often used for additional detail. These catheters have as few as four position detection electrodes and therefore, do not produce as dense of a location data point cloud for the same amount of motion. Under manually-controlled manipulation, these smaller catheters will often miss details within the vasculature or give an incomplete geometric definition of the vascular ostia.
[0014] FIG. 1 is a block diagram of the placement of the motion algorithm within a catheter mapping and navigation system. The patient 1 is placed within the catheter position control system hardware 9 . The catheter position detection hardware 3 is used by the position detection and mapping system 4 to send the live actual position of the catheter 5 to the navigation and closed-loop control system 7 . The navigation and closed-loop control system 7 adjusts the magnetic field and catheter length values 8 and sends them to the position control hardware 9 . The operator inputs the user desired position (DP) 2 for the catheter through the use of a joystick or mouse (not shown). This desired position, DP, is modified by the motion algorithm 10 before it is sent to the navigation and closed-loop position control module 7 .
[0015] FIG. 2 is a detailed block diagram of the motion algorithm's manipulation of the catheter positioning vector. The user defined desired position, DP 2 , is modified by the motion control algorithm 10 to generate the modified desired position, DP* 11 . DP* is used by the navigation and closed-loop control module 7 in place of the raw user defined desired position, DP 2 .
[0016] FIG. 3 is an illustration showing the relationship between the catheter's desired position (DP) and its modified desired position (DP*). The catheter 12 emerges from within the sheath 14 and is manually manipulated through the use of magnetic forces and torques. The magnetic indicator 13 indicates the actual direction of the magnetic field. The desired position, DP 2 , is represented here as being identical to the actual location and direction of the catheter tip (AP), which is representative of a catheter that has been moved to its closed-loop rest position. The modified desired position, DP* 11 is a vector in the same direction as DP, but orbits at a relatively fixed distance.
[0017] FIG. 4 is a vector diagram depicting the time-based calculation of DP* from DP. Both DP and DP* represent the six-degree-of-freedom positions and orientations of a catheter. To locate DP* 11 with respect to DP 2 , the vector P 16 is calculated as the normalized cross product of the desired position DP 2 and the global coordinate Z axis 15 , multiplied by the orbital radius, R 20 . Where DP and Z are coincident, P 16 is set to the direction of the Y axis 19 . Equation 4.1 is the derivation of the mutually perpendicular reference vector, P 16 .
[0000] P=R*DP×Z/|DP×Z| 4.1
[0018] FIG. 4 further depicts the calculation of the current position offset of the DP* vector, PT 17 . Using standard vector equations, the perpendicular vector P 16 is rotated about the desired position DP 2 by the angle defined by the desired angular velocity multiplied by the current time, (ω.t) 18 . The result is the offset unit vector PT 17 . The modified desired position DP* is the addition of the desired position DP 2 and the offset vector PT 17 . The modified desired orientation component of DP* is substantially identical to that of DP.
[0000]
PT
=
P
rotated
about
DP
by
angle
(
ω
·
t
)
.
4.2
DP
*
=
DP
+
PT
4.3
[0019] It is to be understood that the illustrated embodiment has been set forth only for the purposes of example and that it should not be taken as limiting the invention as defined by the following claims. For example, notwithstanding the fact that the elements of a claim are set forth below in a certain combination, it must be expressly understood that the invention includes other combinations of fewer, more or different elements, which are disclosed in above even when not initially claimed in such combinations. A teaching that two elements are combined in a claimed combination is further to be understood as also allowing for a claimed combination in which the two elements are not combined with each other, but can be used alone or combined in other combinations. The excision of any disclosed element of the invention is explicitly contemplated as within the scope of the invention.
[0020] The definitions of the words or elements of the following claims are, therefore, defined in this specification to include not only the combination of elements which are literally set forth, but all equivalent structure, material or acts for performing substantially the same function in substantially the same way to obtain substantially the same result. In this sense, an equivalent substitution of two or more elements can be made for any one of the elements in the claims below or that a single element can be substituted for two or more elements in a claim. Although elements can be described above as acting in certain combinations and even initially claimed as such, it is to be expressly understood that one or more elements from a claimed combination can in some cases be excised from the combination and that the claimed combination can be directed to a sub combination or variation of a sub combination.
[0021] Insubstantial changes from the claimed subject matter as viewed by a person with ordinary skill in the art, now known or later devised, are expressly contemplated as being equivalently within the scope of the claims. Therefore, obvious substitutions now or later known to one with ordinary skill in the art are defined to be within the scope of the defined elements. Accordingly, the invention is limited only by the claims. | The invention is a method of rotating a catheter while it is manually guided in order to increase the volume of space it passes through during a geometric mapping procedure as to provide a higher and more uniform location data point cloud density in a volumetric mapping system. | 0 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a mop, and more particularly to a mop that has a sleeve for users to hold stably.
[0003] 2. Description of the Prior Arts
[0004] A mop has multiple fabric strips mounted on a handle for cleaning floors. To clean floors, the mop is soaked in a bucket of water and swept against the floor surface. Some buckets include a wringer. The wringer has multiple holes and allows users to strain excess water from the mop, to control the amount of water transferred to the floor. But a movement of rotating the mop to squeeze water costs energy. Some buckets include a dehydration device. The dehydration device has a motor and allows users to strain excess water from the mop automatically and efficiently. However, the dehydration device has a lot of power during an actuation time, which causes users can not hold the handle stably and safely.
[0005] To overcome the shortcomings, the present invention provides a mop to mitigate or obviate the aforementioned problems.
SUMMARY OF THE INVENTION
[0006] The main object of the present invention is to provide a mop.
[0007] The mop comprises a handle, a holding assembly and a head assembly. The holding assembly is mounted on the handle and has a sleeve mounted rotatably around the handle. The head assembly is mounted pivotally on the handle and has multiple fabric strips. A user can hold the sleeve during the mop squeezed water by a dehydration device. The sleeve does not be driven to move by the fabric strips or the handle. Therefore, the mop is stably and safely held and the mop can be more efficient to use.
[0008] Other objectives, advantages and novel features of the invention will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is a perspective view of a mop in accordance with the present invention;
[0010] FIG. 2 is an exploded perspective view of the mop in FIG. 1 ;
[0011] FIG. 3 is an enlarged front view in partial section of the holding assembly of the mop in FIG. 1 ;
[0012] FIG. 4 is an enlarged front view in partial section of the fixing assembly of the mop in FIG. 1 ; and
[0013] FIG. 5 is an enlarged front view in partial section of the head assembly of the mop in FIG. 1 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0014] With reference to FIGS. 1 and 2 , a mop in accordance with the present invention comprises a handle ( 10 ), a holding assembly ( 20 ), a fixing assembly ( 30 ), an adapter ( 40 ) and a head assembly ( 50 ).
[0015] The handle ( 10 ) has a top tube ( 11 ), a bottom tube ( 12 ) and a slide tube ( 13 ). The top tube ( 11 ) has a bottom end. The bottom tube ( 12 ) has a top end and a bottom end. The top end of the bottom tube ( 12 ) is connected to the bottom end of the top tube ( 11 ). The slide tube ( 13 ) is mounted movably through the bottom tube ( 12 ) and has a top end, a bottom end and a top end surface.
[0016] With further reference to FIG. 3 , the holding assembly ( 20 ) is mounted around the handle ( 10 ) and has a tubular connector ( 21 ), a sleeve ( 22 ) and a connecting ring ( 23 ). The tubular connector ( 21 ) is mounted around the top tube ( 11 ) and the bottom tube ( 12 ) to connect the top tube ( 11 ) and the bottom tube ( 12 ) securely, has an outside, an inside, a top end, a bottom end, a middle section, a flange ( 211 ), a convex part ( 212 ) and a positioning ring ( 213 ). The flange ( 211 ) is formed around and protrudes from the outside and the bottom end of the tubular connector ( 21 ). The convex part ( 212 ) is formed around and protrudes from the outside and the top end of the tubular connector ( 21 ). The positioning ring ( 213 ) is formed around and protrudes from the inside and the middle section of the tubular connector ( 21 ) and is clamped between the top tube ( 11 ) and the bottom tube ( 12 ).
[0017] The sleeve ( 22 ) is mounted rotatably around the tubular connector ( 21 ). The connecting ring ( 23 ) is connected to the top end of the tubular connector ( 21 ) and has an outside, an inside, a top end, a bottom end, a flange ( 231 ) and an annular groove ( 232 ). The flange ( 231 ) is formed around and protrudes from the outside and the top end of the connecting ring ( 23 ). The annular groove ( 232 ) is formed in the inside of the connecting ring ( 23 ) and engages the convex part ( 212 ) of the tubular connector ( 21 ). The sleeve ( 22 ) is limited between the flanges ( 211 , 231 ) of the tubular connector ( 21 ) and the connecting ring ( 23 ).
[0018] With further reference to FIG. 4 , the fixing assembly ( 30 ) is mounted around the handle ( 10 ) and has a threaded tube ( 31 ), a nut ( 32 ), a liner tube ( 33 ) and a positioning sleeve ( 34 ). The threaded tube ( 31 ) is mounted around the bottom tube ( 12 ) and the slide tube ( 13 ) and connected securely to the bottom end of the bottom tube ( 12 ) and has an outside, an inside, a lower section, a thread part ( 311 ), a pressing surface ( 313 ) and an abutting surface ( 314 ). The thread part ( 311 ) is formed around the outside and the lower section of the threaded tube ( 31 ). The pressing surface ( 313 ) is formed on the lower section of the threaded tube ( 31 ). The abutting surface ( 314 ) is formed around the inside of the threaded tube ( 31 ).
[0019] The nut ( 32 ) is mounted around the slide tube ( 13 ) and is screwed onto the thread part ( 311 ) and has an inside, a lower section and a pushing surface ( 322 ). The pushing surface ( 322 ) is formed on the inside and lower section of the nut ( 32 ) and abuts the pressing surface ( 313 ) of the threaded tube ( 31 ). The liner tube ( 33 ) is mounted securely through the top end of the slide tube ( 13 ) and has an outside, a top end and an abutting ring ( 331 ). The abutting ring ( 331 ) is formed around and protrudes from the outside and the top end of the liner tube ( 33 ) and abuts the top end surface of the slide tube ( 13 ). The positioning sleeve ( 34 ) is mounted around the top end of the slide tube ( 13 ) and has a bottom end surface.
[0020] The nut ( 32 ) is rotated to be distant from the threaded tube ( 31 ) and the slide tube ( 13 ) can be moved along the bottom tube ( 12 ) up and down to adjust an appropriate position for different users or different use conditions. When the slide tube ( 13 ) is moved to a suitable height, screwing the nut ( 32 ) onto the threaded tube ( 31 ) causes the pushing surface ( 322 ) of the nut ( 32 ) to push the pressing surface ( 313 ) of the threaded tube ( 31 ) inward to abut the slide tube ( 13 ) and fix the bottom tube ( 12 ) and the slide tube ( 13 ). Besides, the bottom end surface of the positioning sleeve ( 34 ) abuts the abutting surface ( 314 ) of the threaded tube ( 31 ) to avoid detaching from the bottom tube ( 12 ).
[0021] The adapter ( 40 ) is connected securely to the bottom end of the slide tube ( 13 ) and has a bottom end, a bottom end surface, a protrusion ( 42 ) and a positioning tube ( 41 ). The protrusion ( 42 ) protrudes from the bottom end surface of the adapter ( 40 ). The positioning tube ( 41 ) is mounted radially on the bottom end of the adapter ( 40 ).
[0022] With further reference to FIG. 5 , the head assembly ( 50 ) is mounted pivotally on the handle ( 10 ) and has a cover board ( 51 ), a joint seat ( 52 ), a rotating disk ( 53 ), a mounting board ( 54 ) and multiple fiber strips ( 55 ). The cover broad ( 51 ) is circular and has a center, a bottom surface, a mounting hole ( 511 ), an inner annular recess ( 512 ) and an outer annual recess ( 513 ). The mounting hole ( 511 ) is formed through the center of the cover broad ( 51 ). The inner annular recess ( 512 ) and the outer annual recess ( 513 ) are respectively formed in the bottom surface of the cover broad ( 51 ). The inner annular recess ( 512 ), the outer annual recess ( 513 ) and the cover broad ( 51 ) are concentrically.
[0023] The joint seat ( 52 ) is circular and has a center, a top surface, a positioning hole ( 521 ), two connecting blocks ( 522 ) and an annular sidewall ( 524 ). The positioning hole ( 521 ) is formed through the center of the joint seat ( 52 ). The connecting blocks ( 522 ) protrude separately and symmetrically from the top surface of the joint seat ( 52 ) and are respectively positioned in two corresponding sides of the positioning hole ( 521 ). Each connecting block ( 522 ) has a pivot hole ( 523 ) formed radially in the connecting block ( 522 ) and the pivot holes ( 523 ) align with each other.
[0024] The rotating disk ( 53 ) is circular and has a center, a top surface, a column ( 531 ) and an annular sidewall ( 532 ). The column ( 531 ) protrudes from the center and the top surface of the rotating disk ( 53 ). The mounting board ( 54 ) is circular and is connected securely to the bottom surface of the cover board ( 51 ) and has a bottom surface. The fiber strips ( 55 ) is connected to the bottom surface of the mounting board ( 54 ).
[0025] The joint seat ( 52 ), the rotating disk ( 53 ) and the mounting board ( 54 ) are mounted sequentially on the bottom surface of the cover broad ( 51 ). The connecting blocks ( 522 ) of the joint seat ( 52 ) protrude from the mounting hole ( 511 ) of the cover broad ( 51 ). The annular sidewall ( 524 ) of the joint seat ( 52 ) is mounted in the inner annular recess ( 512 ) of the cover board ( 51 ). The column ( 531 ) of the rotating disk ( 53 ) protrudes from the positioning hole ( 521 ) of the joint seat ( 52 ). The annular sidewall ( 532 ) of the rotating disk ( 53 ) is mounted in the outer annual recess ( 513 ) of the cover board ( 51 ). The pivot holes ( 523 ) of the joint seat ( 52 ) of the head assembly ( 50 ) align with the positioning tube ( 41 ) of the adapter ( 40 ). Two pins ( 60 ) are mounted respectively through the pivot holes ( 523 ) and positioning tube ( 41 ) to connect the handle ( 10 ) and the head assembly ( 50 ) pivotally.
[0026] When the mop in accordance with the present invention is dehydrated by a dehydration device, users can hold the sleeve ( 22 ) of the holding assembly ( 20 ). Because of the sleeve ( 22 ) does not be driven to move by the fiber strips ( 55 ) or the handle ( 10 ), the mop can be stable to dehydrate. Besides, when the handle ( 10 ) is in a vertical state, the protrusion ( 42 ) of the adapter ( 40 ) abuts the column ( 531 ) of the rotating disk ( 53 ) to allow the mop to be used stably and safely.
[0027] Even though numerous characteristics and advantages of the present invention have been set forth in the foregoing description, together with details of the structure and features of the invention, the disclosure is illustrative only. Changes may be made in the details, 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. | The mop has a handle, a holding assembly and a head assembly. The holding assembly is mounted on the handle and has a sleeve mounted rotatably around the handle. The head assembly is mounted pivotally on the handle and has a fiber strips. A user can hold the sleeve during the mop squeezed water by a dehydration device. The sleeve does not be driven to move by the fiber strips or the handle. Therefore, the mop is stably and safely held and the mop can be more efficient to use. | 0 |
CLAIM OF BENEFIT OF PROVISIONAL APPLICATION
Pursuant to 35 U.S.C. Section 119, the benefit of priority from provisional application No. 60/250,255, with a filing date of Nov. 28, 2000, is claimed for this non-provisional application.
ORIGIN OF THE INVENTION
This invention was jointly made by employees of the United States Government, a contract employee during the performance of work under NASA Contract NAS1-97046, and an employee of the National Research Council and may be manufactured and used by or for the government for governmental purposes without the payment of royalties thereon or therefor. In accordance with 35 USC 202, the contractor elected not to retain title.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to electroactive polymeric materials. More particularly, it relates to a new class of polymeric blends for sensor and actuation dual functionality.
2. Description of the Related Art
Sensors and actuators are widely demanded in many technologies to realize precise control of mechanical motion in mechanical, electronic and optical, as well as electro-optical and electromechanical devices. Miniaturization and intellectualization of these devices requires multifunctional materials for simple processing and low cost. Intelligent structures and systems are very important in flight safety and efficiency of aerospace crafts. As a core technology in the intelligent structure and systems, microelectromechanical systems (MEMS) are composed of micro-scale mechanical sensors and actuators. Presently, sensor materials and actuator materials are chosen as separate individual materials for the processing of MEMS.
U.S. Pat. No. 6,239,534 describes a piezoelectric/electrostrictive device. This device, however, requires extensive mechanical manipulation. Specifically, it requires a substrate having two pairs of concave recesses, a connection plate, fixing plate and piezoelectric/electrostrictive elements.
U.S. Pat. No. 6,232,702 describes an electroactive device. This device also has burdensome mechanical requirements. This device requires a ceramic annular substrate having a pair of opposed planar annular surfaces, a hollowed interior region and a thickness aspect.
The new sensor-actuation dual functional polymeric blends described herein provide an enabling electroactive polymer for simplification of processing for MEMS and other electromechanical and electro-optical devices; therefore, the cost of the devices can be significantly reduced.
SUMMARY OF THE INVENTION
It is a primary object of the present invention to provide what is not available in the art, viz., an electroactive polymeric material which provides both sensing and actuation functionality.
It is another object of the present invention to provide a material having temperature invariant piezoelectric response over a range of temperatures.
It is another object of the present invention to provide a material having excellent piezoelectric properties and sensing capability.
It is yet another object of the present invention to provide a material having a large electric field induced strain that significantly increases the range of the electrically-controlled mechanical motion.
Another object of the present invention is to provide a material having excellent processability that makes the material properties tailorable for specific requirements in applications.
Yet another object of the present invention is to provide a lightweight dual-functionality material.
Still another object of the present invention is to provide a material with high power density resulting in reduced energy consumption.
Another object of the present invention is to provide conformable, flexible actuation material that will enable the design for new types of actuators.
Yet another object of the present invention is to provide a two-phase system with adjustable-composition and morphology to optimize mechanical, electrical, and electromechanical properties.
These primary objects, and other attending benefits, are achieved by the present invention. The invention described herein supplies a new class of electroactive polymeric blend materials which offer both sensing and actuation dual functionality. The blend comprises two components, one component having a sensing capability and the other component having an actuating capability. These components should be co-processable and coexisting in a phase separated blend system. Specifically, the materials are blends of a sensing component selected from the group consisting of ferroelectric, piezoelectric, pyroelectric and photoelectric polymers and an actuating component that responds to an electric field in terms of dimensional change. Said actuating component includes, but is not limited to, electrostrictive graft elastomers, dielectric electroactive elastomers, liquid crystal electroactive elastomers and field responsive polymeric gels. The sensor functionality and actuation functionality are designed by tailoring the relative fraction of the two components. The temperature dependence of the piezoelectric response and the mechanical toughness of the dual functional blends are also tailored by the composition adjustment. Since the dual functional blends contain two components, the electric, mechanical, and electromechanical properties of the blends are controlled by the following design parameters: molecular synthesis of sensing polymers and actuating polymers for the blends; selection of the sensing component and actuating components for blends; variation of the fraction of the two component polymers; morphology control of the two components by designed processing routes.
Commercial applications for self-sensing actuation materials include electromechanical transdusors/actuators that can be used in surface flow dynamics control, precise position control, vortex generators in flow control, optical switching, optical filtering, and vibration suppression. These and other actuation applications could benefit from these materials as they will allow simultaneous sensing and actuation capability.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the present invention, including the primary objects and attending benefits, reference should be made to the Detailed Description of the Invention, which is set forth below. This Detailed Description should be read with reference to the accompanying Drawings, wherein:
FIG. 1 is a graph showing the relationship between the copolymer content and the crystallinity in the blends;
FIG. 2 is a graph showing the relationship between the copolymer content and the remanent polarization;
FIG. 3 is a graph comparing the mechanical modulus, E 11 , of the blend films and pure polymer films;
FIG. 4 is a graph showing the temperature dependence of the piezoelectric strain coefficient, d 31 , of the blend films (1 HZ) as a function of various compositions;
FIG. 5 is a graph showing the relative composition dependence of the piezoelectric strain coefficient, d 31 , at 30° C. and 65° C.;
FIG. 6A is a graph showing the temperature dependence of the dielectric constant;
FIG. 6B is a graph showing the composition dependence of the dielectric constant;
FIG. 7A is a graph showing the field-induced strain response of the blends calculated according to equation (3);
FIG. 7B is a graph showing the measured field-induced strain response of the blends;
FIG. 8 is a graph comparing the experimental strain response of the 75 wt % copolymer blend with the prediction based on the calculation using equation (3);
FIG. 9 is a graph showing the electric field-induced strain of the blends as a function of the copolymer content at an electric field strength of 3 MV/m;
FIG. 10A is a bending actuator incorporating a copolymer-elastomer blend when no electric field is applied;
FIG. 10B is a bending actuator incorporating a copolymer-elastomer blend when an electric field of 90 MV/m is applied.
DETAILED DESCRIPTION OF THE INVENTION
In a preferred embodiment, the polymer blend combines an electrostrictive graft-elastomer with a piezoelectric poly (vinylidene fluoride-trifluoroethylene) polymer. Mechanical properties, piezoelectric properties and electric field induced strain response of the blends are a function of temperature, frequency and relative composition of the two constituents in the blends. A bending actuator device was developed incorporating the use of the polymer blend materials.
The electrostrictive graft polymer is described fully in U.S. patent application Ser. No. 09/696,528, now U.S. Pat. No. 6,515,077, entitled “Electrostrictive Graft Elastomers” and incorporated by reference herein. The graft-elastomer polymer exhibits a large electric field induced strain due to electrostriction and consists of two components, a flexible backbone elastomer and grafted crystalline groups. The graft crystalline phase provides the polarizable moieties and serves as cross-linking sites for the elastomer system.
Specifically, the electrostrictive graft elastomer comprises a backbone molecule which is a non-crystallizable, flexible macromolecular chain, and a grated polymer forming polar graft moieties with backbone molecules, the polar graft moieties having been rotated by an applied electric field, advantageously into substantial polar alignment. The backbone molecule is advantageously a member selected from the group consisting of silicones, ployurethanes, polysulfides, nitrile rubbers, polybutenes, and flourinated elastomers, e.g., a chlorotrifluoroethylene-vinylidene fluoride copolymer. The grafted polymer is a homopolymer or a copolymer, and the polar graft moieties are polar crystal phases and physical entanglement sites with backbone molecules. The grafted polymer is preferably a member selected from the group consisting of poly(vinylidene fluoride) and poly(vinylidene fluoride-trifluoroethylene) copolymers. In a particularly preferred embodiment, the backbone molecule is a chlorotrifluoroethylene-vinylidene fluoride copolymer, and the grafted polymer is a poly(vinylidene fluoride) or a poly(vinylidene fluoride-trifluoroethylene) copolymer. The polar graft moieties, which are polar crystal phases and physical entanglement sites with backbone molecules, have been rotated by an applied electric field, advantageously into substantial polar alignment.
In the preferred embodiment, the current invention combines this graft-elastomer with a poly(vinylidene fluoride-trifluoroethylene) copolymer to yield a peizoelectric-electrostrictive blend. This blend results in an enhancement of the toughness of the copolymer since the pure copolymer is somewhat brittle after annealing. Likewise it has a higher force output than the pure graft-elastomer when used as an actuator. Additionally, by careful selection of the composition, the potential exists to create a blend system with electromechanical properties that can be tailored for various conditions and applications.
EXAMPLES
Experimental Set-Up
Film Preparation: The blend films were prepared by solution casting. The piezoelectric poly(vinylidene fluoride-trifluoroethylene) copolymer (50/50 mol. %) and graft elastomer powders were added to N,N-dimethylformamide. Although N,N-dimethylformamide was used in this particular example, any solvent capable of dissolving the polymeric functional components for processing may be used. The mixture was heated to 60° C. while stirring to make a 5 wt. % polymer solution containing the desired fraction of the two components. The solution was then cooled to room temperature, cast on glass substrates, and placed in a vacuum chamber. After drying overnight under vacuum, tack-free films were obtained. In order to increase their crystallinity, and possibly their remanent polarization, the blend films were thermally annealed at 140° C. for 10 hours. The thickness of the films was approximately 20 micrometers. The composition and crystallinity of the annealed blend films were determined using an x-ray diffractometer (XRG 3100, Philips) and differential scanning calorimetry.
Poling Treatment: Gold electrodes were sputtered on the opposing surfaces of the films using a plasma deposition set-up (Technics, Inc.) to establish electrical contact. The films were poled using a triangular waveform with a peak value of 100 MV/m at 30 mHz. The blend films were immersed into silicone oil to minimize arcing during the poling treatment.
Mechanical and Piezoelectric Measurements: The modulus, E 11 , and the piezoelectric strain coefficient, d 31 , of the copolymer-elastomer blend films were measured using a modified Rheovibron DDV-II-C (Imass Inc.). The measurements were performed as a function of the relative composition of the blends (wt. % copolymer content), temperature, and frequency.
Electric Field Induced Strain Measurement: The measurement of the electric field induced strain response of the blend films in the longitudinal direction was accomplished using a fiber optic sensor (FOS)-based Dual Channel Angstrom Resolver (OPTO Acoustic Sensors) combined with a waveform generator (Hewlett Packard 33120A), a voltage amplifier (Trek 50/750), and an oscilloscope (Hewlett Packard 54601B). The measurement set-up was computer controlled. The FOS was positioned to measure the out-of-plane displacement through the thickness of the sample. The peak-to-peak displacement was recorded as voltage and converted into meters using the proper gains (filter gain, sensor gain and sensor sensitivity). The frequency of measurement was 1 Hz.
Capacitance Measurement: The capacitance of the blend films was measured using a Hewlett Packard Analyzer 4192A, and the dielectric constant, Ε, was calculated from the value of the capacitance. These measurements were performed by a function of the relative composition of the blends (wt. % polymer content), temperature, and frequency.
Results
FIG. 1 shows the crystallinity as a function of copolymer content in the blend. The calculated crystallinity of the blend system is found from:
X total =f copolymer X copolymer +f elastomer X elastomer (1)
where f is the relative fraction of the components and X is the crystallinity. Both the measured and calculated crystallinities increase with increasing copolymer content in the blend; however, the measured crystallinity is lower than the calculated one. This indicates that the presence of both components in the blend may reduce their crystallization as compared to each individual one.
FIG. 2 shows the measured remanent polarization, P r , as a function of the copolymer content in the blends compared with the remanent polarization calculated using the following equation:
P r(total) =f copolymer P r(copolymer) +f elastomer P r(elastomer) (2)
where f is the relative fraction of the components, P r(copolymer) is the remanent polarization in the pure copolymer, P r(elastomer) is the remanent polarization in the elastomer, and P r(total) is the resulting remanent polarization of the blend film. To determine the remanent polarization, the measurement of the polarization, P, versus the electric field, E, was carried out. Corrections were made to eliminate the effects of conductivity on the ferroelectric hysteresis loops. Both the measured and the calculated remanent polarization increase with increasing copolymer content in the blends. The value of the measured remanent polarization is very close to the calculated one. This is an indication of the linear relationship between P r and the polar crystallinity in the blends.
FIG. 3 shows the mechanical modulus, E 11 , for all the blends as a function of temperature at 1 Hz. The mechanical modulus of the blends increases with increasing copolymer content and the copolymer has the highest modulus. Due to the brittleness of the copolymer film, it tended to fail at about 65° C., while the copolymer-elastomer blends show improved toughness compared to the pure copolymer.
FIG. 4 shows the temperature dependence of the piezoelectric strain coefficient, d 31 , for blend films with various compositions. The piezoelectric strain coefficient, d 31 , increases with increasing copolymer content. However, the blend film with 75 wt. % copolymer exhibits the highest d 31 from room temperature to about 45° C. Additionally, the blend film with 50 wt. % shows an almost constant piezoelectric response from room temperature to 70° C. These results reflect the influence of both the electrical polarization and mechanical modulus of the films on the piezoelectric strain response. As observed in the case of the 75 wt. % copolymer blend, even though it had a lower remanent polarization than the copolymer, it showed a higher piezoelectric strain response due to its lower modulus. For the experimental conditions, the copolymer film breaks at a temperature close to 65° C., while the rest of the blend films maintain their piezoelectric response up to 75° C. without mechanical failure. In particular, the piezoelectric strain response of the 75 wt. % copolymer and 50 wt. % copolymer blend films is still significantly high up to 75° C.
FIG. 5 demonstrates the different trends observed at 30° C. and 65° C. when the dependence of the piezoelectric strain coefficient, d 31 , on the relative composition of the two components in the blend is examined. The reason for the non-linear dependence may be attributed to the nature of the piezoelectric strain response of the material. The intrinsic contributions of both the mechanical properties (through the modulus) and the electrical properties (through the polarization) may yield this non-linear behavior.
FIGS. 6A and 6B show the temperature dependence and composition dependence of the dielectric constant at 10 Hz for the copolymer-elastomer blend films. The temperature dependence of the dielectric constant shown in FIG. 6A gives a reasonable trend for a blend system. The elastomer shows a transitional change in the temperature range from 40° C. to 50° C. and less temperature dependence than the copolymer in the measured temperature range. The transitional change is the second glass transition of the elastomer due to the molecular motion of the graft crystal cross-linking sites. The addition of the copolymer in the blend decreases the second glass transition of the graft elastomer significantly. This might be attributed to the molecular interaction between the added copolymer and graft unit in the elastomer. This interaction may also be the reason that the measured crystallinity of the blend is lower than the calculated one. The dielectric constant of the copolymer shows an obvious increase above 50° C. due to the ferroelectric-paraelectric phase transition. For the blend system, as the copolymer content increases, the transition behavior in the dielectric constant becomes more apparent. FIG. 6B shows the inter-relationship between the dielectric constant and the relative composition of the two components in the blend. Unlike the piezoelectric strain response, the dielectric constant shows a linear dependence to the relative composition at both 25° C. and 65° C.
FIG. 7A shows the results of a comparison to a field-induced strain response in the copolymer and the graft-elastomer. Assuming the two constituents of the blend system contribute independently to the total field-induced strain response in the blends, the total response in the longitudinal direction can be predicted as
S=f cop. S cop. +f elast. S elast. =f cop. d cop. E+f elast. R elast. E 2 (3)
where S is the total strain, E is the applied electric field, f cop. is the fraction of the piezoelectric copolymer in the blend, d cop. is the piezoelectric coefficient of the piezoelectric copolymer, while f elast. is the fraction of the electrostrictive graft-elastomer, R elast. is the field-induced strain coefficient of the electrostrictive graft-elastomer. Using the piezoelectric coefficient of the copolymer and the field-induced strain coefficient of the graft-elastomer, the field-induced strain for the blends is calculated. The predicted strain response of the copolymer is linear (piezoelectric) while the strain response of the graft-elastomer is quadratic (electrostrictive). As evident in FIG. 7A, the strain response of the blends is intermediate to that of the constituents. There is a critical electric field strength at about 12 MV/m. For field strengths below the critical field, the piezoelectric constituent of the blend is dominant, therefore the strain increases with increasing copolymer content in the blends. Above the critical field strength, the electrostrictive constituent becomes a dominant contributor to the total strain, hence the strain in the blends increases with increasing graft-elastomer content. In FIG. 7B, the experimental results of the field-induced strain of the blend, in the longitudinal direction, is shown as a function of field strength. The blend compositions measured are identical to the blend compositions used in the prediction in FIG. 7 A. Although there is a composition dependence for the measured strains, there are several key differences from the predicted strain. First, the measured strain response is significantly smaller than the predicted one. Secondly, the critical field strength for the transition from piezoelectric to electrostrictive dominance occurs at a higher field. Lastly, the electrostrictive (quadratic) contribution becomes evident at a higher field strength in the measured strains. These differences strongly suggest that the electromechanical contributions of the constituents to the total strain response of the blends are not independent. The interactions between the copolymer and graft-elastomer may affect their contributions to the strain response, especially the contribution from the electrostrictive graft-elastomer.
The piezoelectric contribution to the total strain is attributed to the remanent polarization of the crystals within the copolymer, and is expected to be proportional to the relative composition of the copolymer in the blend. The elctrostrictive contribution to the total strain is controlled by the ability of the polar graft moieties in the elastomer to rotate with the applied electric field. Hence the electrostrictive contribution is dependent on the overall morphology of the blend. The effect of the blend morphology on the electrostriction is key since free volume is essential for the rotation of the graft polar moieties in the electrostrictive graft-elastomer. Presence of the copolymer in the blends occupies volume and offers more resistance to the rotation of the polar graft units than in the pure elastomer. This resistance increases the barrier energy for the polar moieties to overcome for their rotation, resulting in the onset of the electrostriction at higher field strengths. This is possibly the key intrinsic mechanism for the differences observed in the experimental and predicted results.
In FIG. 8, the measured strain response of 75 wt. % copolymer blend is compared with the prediction calculated using equation (3). According to calculated results, the critical electric field strength is 12 MV/m, (marked as 1). Theoretically, at this critical field strength, the copolymer and the elastomer contribute equally to the overall strain response. However, experimental results indicate that the strain is linear prior to a field strength of about 22 MV/m (marked as 2). As the electric field is increased, the contribution of the electrostrictive elastomer becomes significant as seen by the deviation from linearity above a field strength of 22 MV/m. For field strengths higher than 39 MV/m, the strain of the blend is larger than that of the pure copolymer. This is an indication that the electrostrictive contribution becomes dominant and the field of 39 MV/m (marked 3) is believed to be the critical electric field for the transition from piezoelectric to electrostrictive dominance for the 75 wt. % copolymer blend. This is significantly higher than the calculated one.
According to these observations, the strain response of the blend can be divided into three regions: piezoelectric dominant region, intermediate region, and electrostrictive dominant region. In the piezoelectric dominant region (E<22 MV/m), the contribution of the electrostrictive constituent is not significant since the rotation of the polar component of the elastomer is confined due to the presence of the copolymer constituent, which increases the barrier energy for rotation. In the intermediate region (22 MV/m<E<39 MV/m), the field strength is high enough to overcome the increased barrier energy, therefore, the electrostrictive contribution becomes obvious. In the electrostrictive dominant region (E>39 MV/m), the blend exhibits a field-induced strain higher than that of the copolymer. The increase in the barrier energy for the electrostrictive contribution in the blend should be dependent on the relative copolymer content in the blends, the overall blend morphology, and the crystal size of the constituents as well as the distribution of the crystal size.
FIG. 9 illustrates the variation in field-induced strain with copolymer content in the blend for a field strength of 3 MV/m. For this relatively low field strength, the piezoelectric response is dominant; therefore, the strain increases as the amount of the piezoelectric constituent increases. For the 75 wt. % copolymer blend, the strain is almost three times of that of the graft-elastomer and it is only about 8% lower than that of the copolymer. Considering the improved toughness of the blend as compared to the copolymer, and the enhanced strain and the mechanical modulus as compared to the graft-elastomer, the piezoelectric-electrostrictive polymer blend systems offer a way to optimize electromechanical properties for applications at lower field strength.
FIG. 10 depicts a prototype bending actuator fabricated using a film of the 50 wt. % composition of the copolymer-elastomer blend. The deflection of the bending actuator is determined by the applied electric field and the electric field induced strain of the blend. A deflection of approximately 4.5 mm was achieved with this actuator with the length of 22 mm. Larger deflections are achievable if the actuator is fabricated using the pure graft-elastomer; however, there is a trade-off between actuation force and deflection due to the relative moduli of the materials.
The copolymer-graft-elastomer blend system exhibited a marked improvement in toughness as compared to the copolymer. The blends also offer the potential of varying the composition of the materials constituents to tailor the properties for the desired applications. Due to the synergistic effect of the contributions of the remanent polarization and the mechanical stiffness, blends can be made to exhibit a higher piezoelectric strain and field-induced strain than the copolymer. As an example, the blend containing 75 wt. % copolymer exhibited a higher piezoelectric strain coefficient (d 31 ) and field induced strain (%) than the pure copolymer for some conditions. Furthermore, by adjusting the relative fraction of the two components in the blend, a temperature-independent piezoelectric strain response was achieved such as in the case of the 50 wt. % copolymer blend. The electric field induced strain in the copolymer-elastomer blend results from both piezoelectric and electrostrictive constituents. The piezoelectric contribution dominates when the electric field is low while the electrostrictive contribution becomes dominant at higher field strengths. The contributions of the two constituents are not independent. The presence of the copolymer in the blend appears to increase the barrier energy for the polar graft moieties to overcome in order to rotate (the mechanism for the electrostriction in the graft-elastomer).
It should be understood that the foregoing description and examples are only illustrative of the invention. Various alternatives and modifications can be devised by those skilled in the art without departing from the invention. Accordingly, the present invention is intended to embrace all such alternatives, modifications and variances that fall within the scope of the appended claims. | The invention described herein supplies a new class of electroactive polymeric blend materials which offer both sensing and actuation dual functionality. The blend comprises two components, one component having a sensing capability and the other component having an actuating capability. These components should be co-processable and coexisting in a phase separated blend system. Specifically, the materials are blends of a sensing component selected from the group consisting of ferroelectric, piezoelectric, pyroelectric and photoelectric polymers and an actuating component that responds to an electric field in terms of dimensional change. Said actuating component includes, but is not limited to, electrostrictive graft elastomers, dielectric electroactive elastomers, liquid crystal electroactive elastomers and field responsive polymeric gels. The sensor functionality and actuation functionality are designed by tailoring the relative fraction of the two components. The temperature dependence of the piezoelectric response and the mechanical toughness of the dual functional blends are also tailored by the composition adjustment. | 2 |
BACKGROUND OF THE INVENTION
The invention relates to a sounding apparatus for pressing a sounding rod into a piece of ground in order to determine the soil properties at various depths, comprising:
a sounding rod which is intended to be pressed into a piece of ground;
first and second clamping members for alternately clamping the sounding rod in place;
first drive means for moving the first clamping member up and down in the longitudinal direction of the sounding rod.
A sounding apparatus of this nature is known from SU-A-476 367. The sounding apparatus described herein comprises a sounding rod with a conical measurement head which is intended to determine soil properties at various depths. In this case, the sounding rod is pressed into a piece of ground in steps (discontinuously). The apparatus comprises a first clamping member which is directly connected to two pistons of a hydraulic system. The pistons are indirectly actuated by means of a gear-rack transmission for each downwards movement. The first clamping member is designed with two tilting bodies which clamp the sounding rod in place during a downwards movement of the first clamping member and release it during an upwards movement. The apparatus furthermore comprises a second clamping member which is designed with two tilting bodies which automatically release the sounding rod during a downwards movement of the sounding rod and clamp it in place in the event of any upwards movement of the sounding rod. The second clamping member is fixedly connected to a frame. The gear wheel comprises a section of approximately a quarter of a circle which is cut out. The hydraulic system is under spring load. Shortly before the end of the downwards movement of the pistons, the cut-out section in the gearwheel comes to lie opposite the rack. This provides the pistons with the freedom to execute an upwards movement under spring load, during which movement the first clamping member automatically moves into an open position. At the same time, the fixedly arranged second clamping member prevents the sounding rod from being able to carry out an undesired movement back upwards. The sounding apparatus is then ready for the next penetration movement.
A drawback of this known sounding apparatus is that it is only able to carry out discontinuous sounding measurements. The penetration movement of the sounding rod into the soil is always interrupted as soon as the pistons have reached their lowest point and have to carry out an upwards movement before the penetration movement can be continued. Waiting each time for the pistons to return to their uppermost point wastes valuable working time. Even more importantly, during each interruption of the sounding measurement, the soil in the area of the sounding rod is given time to settle. Owing to dissipation effects and the build-up of skin friction, the measurement data from a thin layer of soil are lost each time. Furthermore, the structure of the known sounding apparatus is complex
It should be noted that over the course of the years, a number of structures have been designed for carrying out a continuous downwards penetration movement of a sounding rod, using a sounding apparatus. Hitherto, however, no satisfactory solution has been found.
SUMMARY OF THE INVENTION
The object of the invention is to overcome the abovementioned drawbacks, and in particular to provide a sounding apparatus which is simple to operate and which can be used to carry out both continuous and discontinuous sounding measurements.
This object is achieved according to the invention by means of a sounding apparatus according to claim 1 . According to the invention, the sounding apparatus comprises first and second clamping members which can be separately actuated between a closed position, in which a sounding rod is clamped in place, and an open position, in which a sounding rod is released. First drive means are provided for the first clamping member, while second drive means are provided for the second clamping member. Both the first and the second drive means are able to cause the associated clamping members to carry out upwards and downwards movements. The clamping members and the drive means are connected to control means. The control means are able to cause the clamping members to alternately clamp in place and release, and, by means of activation of the associated drive means, to carry out upwards and downwards movements. Since both clamping members can move up and down in a separately controllable manner and can be activated separately with regard to the clamping function, the sounding apparatus can advantageously be employed in multifunctional mode. In particular, it is possible, according to the invention, to carry out reliable continuous sounding measurements. This will be explained in more detail below. The sounding apparatus according to the invention is suitable to be supported on the ground via a frame, but may advantageously also be mounted on any sounding vehicle, for example a caterpillar vehicle. In addition to continuous sounding, the apparatus may furthermore be used for carrying out discontinuous sounding measurements, for taking soil samples and for drilling. The sounding apparatus is also suitable for carrying out sounding measurements underwater, for example on the sea bed, provided that it is equipped with a special underwater drive unit.
Preferred embodiments of the sounding apparatus are defined in claims 2 - 9 .
A method for carrying out a continuous sounding measurement according to the invention is defined in claim 10 . In this case, the invention is based on a transfer principle. When the first clamping member, in the clamped position, ends a downwards movement, during which movement a sounding rod which is clamped in place by the first clamping members is pressed into a piece of ground, the second clamping members take over the penetration movement of the sounding rod, by likewise carrying out a downwards movement in the clamped position. At the same time as this latter step, the first clamping members, in the unclamped state, carry out an upwards movement. This results in a continuous penetration rate of the sounding rod. The continuous sounding measurement provides considerable advantages with regard to the quality and quantity of sounding measurements. Since the sounding can now be carried out on a continuous basis, considerable time can be saved. At a continuous penetration rate of 2 cm per second, a daily penetration depth to be measured of 200-250 m, and 50 working weeks per year, it is possible to save 100 hours per year. This provides a considerable cost saving. With regard to the quality of measurement, in practice it has been found that significantly better results are obtained. Advantageously, the measurement results show no trace of dissipation effects or of a build-up of skin friction. This allows measurements to be made more accurately and allows the soil properties to be determined over the entire penetration depth without interruption.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be explained in more detail with reference to the appended drawing, in which:
FIG. 1 shows a diagrammatic front view of an embodiment of a sounding apparatus according to the invention;
FIG. 2 shows a view in cross section on line II—II in FIG. 1;
FIGS. 3 a, b, c and d show four respective steps of a continuous sounding measurement using a sounding apparatus as shown in FIG. 1;
FIG. 4 is a rear view of a sounding apparatus for a continuous sounding process, with an electrical cone; and
FIG. 5 shows a front view of a sounding apparatus for a discontinuous sounding process, with a mechanical cone.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The sounding apparatus which is shown in FIG. 1 comprises two hard chromium plated piston rods I which are disposed next to one another. The piston rods 1 are vertical and are attached to a lower bridge piece 2 on their underside. The lower bridge piece 2 is connected to a fixture, as diagrammatically indicated. The fixture may, for example, be the subframe of a caterpillar vehicle. The device furthermore comprises two cylinder heads 3 which are able to move up and down along the ends of the piston rods 1 . At their bottom ends, the cylinder heads 3 are connected to one another by means of an upper bridge piece 4 . This results, as it were, in the shape of a rugby goal, with two upwardly projecting posts. The cylinder heads 3 are able to execute an upwards and downwards movement along the piston rods 1 and form first drive means. The two piston rods 1 are longer than is necessary for this movement. On the extended part of the piston rods 1 , there are two cylinder sleeves 5 . The piston rods 1 extend through the whole of the cylinder sleeves 5 . The two cylinder sleeves 5 are connected to one another by means of a central bridge piece 6 which is designed in the same way as the upper bridge piece 4 . The cylinder sleeves 5 are able to execute an upwards and downwards movement along the piston rods 1 and form second drive means. For their upwards and downwards movements, the cylinder heads 3 and the cylinder sleeves 5 are hydraulically activated via control means. Advantageously, four limit switches are fitted, which limit the upwards and downwards movements of the cylinder heads 3 and the cylinder sleeves 5 along the piston rods 1 . The design with the two piston rods 1 disposed next to one another is robust, stable and reliable.
It can be seen from FIG. 2 that the central bridge piece 6 is provided in the centre with a continuous hole. In this hole, there is a block 7 with a recess which is V-shaped, for example, therein. A hydraulic cylinder 8 is attached to the rear side of the central bridge piece 6 . A clamping block 9 with a knurled, shell-shaped recess is mounted on the end of a piston rod of this hydraulic cylinder 8 . The blocks 7 and 9 together form a hydraulically actuable clamping member. The clamping member is suitable for clamping rods or tubes of different diameters, for example 36 and 56 mm. To switch over from 36 mm to 56 mm, a filler plate 12 has to be removed. This can be done easily, for example by unscrewing a bolt (not shown), allowing the filler plate 12 to be pulled upwards behind the clamping block 7 . The upper bridge piece 4 likewise comprises a hydraulically actuable clamping member which corresponds to the central bridge piece 6 .
Since both drive means and both clamping members are hydraulically actuable, the control means may advantageously be of simple design.
The sounding apparatus in FIG. 1 is intended to press a sounding rod, which is denoted by 10 in the figure, into a piece of ground, in order to determine soil properties at various depths. For this purpose, the sounding rod 10 is designed, in a known way, with a measuring probe. The measurement data may be recorded electronically or mechanically and fed to a processing unit. The sounding rod 10 is composed in particular of a plurality of pipe parts which can be connected to one another. In this case, the pipe parts should be connected to one another during an ongoing penetration process, for example by means of a screw connection. A substantial advantage in this case is the open structure between the two cylinder heads 3 located at the top. This provides easier access for an operator.
The sounding apparatus as shown in FIG. 1 furthermore comprises a scraper clamp 15 , which is composed of two hydraulic cylinders with shell-shaped blocks on piston rods of the cylinders. The blocks are pressed against the sounding rod 10 and are made in particular from a very wear-resistant plastic. During a sounding measurement, the blocks support the sounding rod 10 . While the sounding rod 10 is being pulled back out of the ground, the rod is scraped clean by the blocks of the scraper clamp 15 .
Highly advantageously, the sounding apparatus described above is used to carry out a continuous sounding measurement. To this end, the drive means and the clamping members have to be actuated according to a set pattern. This advantageous continuous sounding process will be explained in more detail with reference to FIGS. 3 a, b, c and d.
In FIG. 3 a , the upper bridge piece 4 , with the first clamping member in the clamped position, as a result of suitable driving of the cylinder heads 3 , makes a downwards movement, indicated by arrow 20 . As a result, the sounding rod 10 is pressed downwards. At the same time, the centre bridge piece 6 , with the second clamping member in the unclamped position, as a result of suitable driving of the cylinder sleeves 5 , makes an upwards movement, indicated by arrow 21 . Just before the downwards movement of the upper bridge piece 4 reaches its deepest point, the centre bridge piece 7 is also moved downwards. Then, the clamping force is gradually transferred from the first clamping member to the second clamping member. After this has been completed, the second clamping member clamps the sounding rod 10 in place and continues the penetration movement which has been initiated by the first clamping member. This is indicated by arrow 22 in FIGS. 3 b and 3 c . The first clamping member in the upper bridge piece 4 is in an unclamped position, and the upper bridge piece 4 , in this unclamped position, carries out an upwards movement. This is indicated by arrow 23 in FIGS. 3 b and 3 c . Just before the downwards movement of the centre bridge piece 6 reaches its deepest point, the upper bridge piece 4 , as a result of corresponding actuation of the cylinder heads 3 , is moved back downwards. The clamping force is gradually transferred from the second clamping member to the first clamping member. After this transfer has been completed, the first clamping member clamps the sounding rod 10 in place and continues the penetration movement. This is indicated by arrow 24 in FIG. 3 d . The cycle is then repeated from the beginning. Suitable activation of the clamping members and drive means, as described above with reference to FIG. 3, results in a kind of transfer principle, making it possible to press the sounding rod into a piece of ground at a substantially continuous rate.
The penetration depth of the sounding rod can be recorded in various ways. One option is a wheel which is coupled to a pulse generator, which wheel is pressed against the sounding rod, for example by means of a spring or a pneumatic cylinder. The number of revolutions of the pulse-generator wheel defines the penetration depth of the sounding rod.
While the sounding rod which is composed of a plurality of pipe parts may be pressed continuously into a piece of ground, the sounding rod is in principle pulled out of the ground in a discontinuous manner. The sounding rod is pulled out at a greater speed, for example 16 cm per second, compared to 2 cm per second for penetration. With such a high withdrawal rate, a continuous upwards movement of the sounding rod would not leave sufficient time for the various pipe parts to be unscrewed. The sounding rod parts can be pulled out of the ground as follows:
the centre bridge piece 6 remains in the upper position during withdrawal;
the first clamping member in the upper bridge piece 4 is closed;
the second clamping member in the centre bridge piece 6 is opened;
the upper bridge piece 4 moves upwards in the clamped position and pulls the sounding rod 10 out of the ground;
the upper bridge piece 4 stops at the end of its travel;
the second clamping member in the centre bridge piece 6 closes;
the first clamping member in the upper bridge piece 4 opens;
the upper bridge piece 4 moves downwards in the unclamped position;
the cycle is repeated from the beginning.
According to a significant feature of the invention, the drive means of the cylinder heads 40 and the cylinder sleeves 41 , as well as the dimensions thereof, are designed in such a way, or else limiting means are arranged at such positions, that the first clamping member 42 in the upper bridge piece 43 is able to make a movement which is many times greater than the movement which the second clamping member 44 in the centre bridge piece 45 is able to make. This is illustrated in FIG. 4, in which the upper movement arrow 46 is more than four times longer than the lower movement arrow 47 , for example amounting to 800 and 200 mm respectively. As a result, the accessibility of the sounding rod 48 during a sounding measurement is high, and new pipe parts are advantageously simple to screw on.
It can be further seen from FIG. 4 that a measurement cable 49 extends through a recess in the sounding rod 48 . This makes the sounding apparatus shown in FIG. 4 suitable for electrical sounding. For this purpose, the sounding rod 48 is designed with an electrical measurement cone 49 ′. The pipe parts which are to be screwed onto the sounding rod 48 which has already been shown have, as a preparatory measure, already been pushed over the measurement cable 49 and can be stored at the side of the sounding apparatus.
By dint of its design, the sounding apparatus according to the invention is multifunctional. In addition to the advantageous method described above for carrying out continuous sounding measurements, it is also possible to carry out a discontinuous sounding measurement. During a discontinuous sounding measurement, by way of example, the cylinder sleeves are not actuated and the second clamping member remains in a constant position. By driving the cylinder heads in combination with a suitable alternating actuation of the first and second clamping members, a sounding rod can be pressed into a piece of ground in steps. This is shown in FIG. 5 . In this case, the centre bridge piece 50 is fixed in its lowermost position. A sounding rod with a mechanical cone 52 at its bottom end and a hydraulic or electrical measurement appliance 53 at its top end, is clamped in place in the first clamping member of the upper bridge piece 51 . Only the upper bridge piece 51 executes upwards and downwards movements of, for example, 1 m, indicated by arrow 55 , as a result of the cylinder heads 54 being actuated. After each downwards movement, the upper bridge piece 51 is firstly placed in its uppermost position, after which a new pipe section can be screwed on. Then, a sounding measurement over a limited penetration depth can again be carried out.
Thus, the invention provides a multifunctional sounding apparatus, by means of which it is possible, in particular, to carry out continuous sounding measurements on the basis of a transfer system with two clamping members which can move up and down and can be actuated with regard to clamping. | Sounding apparatus for pressing a sounding rod into a piece of ground in order to determine the soil properties at various depths, comprising a sounding rod which is intended to be pressed into a piece of ground; first and second clamping members for alternately clamping the sounding rod in place; first drive means for moving the first clamping member up and down in the longitudinal direction of the sounding rod; in which apparatus the first and second clamping members can be separately actuated between an open position and a closed position; second drive means are provided for moving the second clamping member up and down in the longitudinal direction of the sounding rod; and control means are provided, which are connected to the clamping members and drive means for alternately clamping in place, releasing and moving the respective clamping members up and down. | 4 |
This is a continuation, of application Ser. No. 933,420 filed Aug. 14, 1978, now abandoned.
FIELD OF INVENTION
This invention relates to a system for magnetically uncoupling and coupling model railroad cars.
BACKGROUND OF INVENTION
The model railroader has had various couplers available for use in coupling and uncoupling of model rail or freight cars. Of these, the most popular coupler has been a hook type coupler or a variation thereof. These couplers have been used with all types of railroad systems, the most popular models adapted for "HO" gauge or "N" gauge track.
In an attempt to provide remote control and authenticity, magnetic coupling and uncoupling systems were developed, as exemplified in U.S. Pat. No. 3,111,229 and U.S. Pat. No. 3,115,255. Delayed action magnetic couplers were introduced to overcome inadequateness of these prototypes, as shown in U.S. Pat. Nos. 3,117,676 and 3,469,713. In these later attempts, alterations of the housing pivot, shank and knuckle were made.
A difficulty with conventional magnetic couplers exists with the uncoupling pin which extends downward from the coupler, perpendicular to the track rail surface and the "between-the-track" arrangement of the magnetic field. If the downward extended pin comes too close to the surface of the rail, it oftentimes hits the side of the track, snags at switch points, frogs on rerailing ramps or even within its own uncoupling ramp, causing inadvertent uncoupling and derailments of the rolling stock. As a result of this basic problem, some model railroaders simply cut the pin from the coupler and then use hand uncoupling to effect separation or uncoupling of rolling stock when it is desired, which is far from being prototypical.
Another unsolved problem resides in the incompatibility of a magnetic coupler system with conventional hook-horn coupler design which is available on rolling stock, such as "HO" gauge in ready-to-run or kit form. These conventional couplers do not operate by delayed uncoupling, which is defined as the means whereby rolling stock can be uncoupled, spotted and released at any desired location on a model railroad layout from a single remote uncoupling site. If the model railroader wishes to convert a conventional hook-horn type coupler to a delayed uncoupling system, he must also replace the conventional couplers, possibly the coupler pocket housings, and in some cases the entire truck frame, which may include ferromagnetic wheels and/or axles. This is a time consuming disadvantage that also adds to the cost of rolling stock.
SUMMARY OF THE INVENTION
This invention is directed to an improved magnetically-automated delayed uncoupling system which comprises a knuckle positioned magnet and an outside-the-rail positioned magnetic field for a full opening activation of the uncoupling procedure.
An advantage of the instant invention is an economically simple means to produce an improved magnetically-automated delayed uncoupling system for model railroads. The uncoupling system of the instant invention provides also for simple conversion of the conventional hook type coupler to a magnet-actuated coupler. According to the instant invention, the magnetic coupler may be preferably activated by a magnetic force field from magnets positioned outside the rail track to facilitate said coupler to uncouple: (1) from a conventional coupler, and (2) from a companion magnet-actuated coupler by a delayed mechanism. A method is provided whereby rolling stock can be uncoupled, spotted and released at any desired uncoupling site. The improved coupler system of the instant invention will reliably recouple with various conventional couplers and allow recoupling with the heavier springs associated with conventional hook type couplers.
This versatility of recoupling is accomplished with a specifically designed magnetic force field, without replacement of ferromagnetic wheels, axles and/or truck frames on rolling stock with costly non-ferromagnetic substitutes. One unique feature of the magnetic coupler system of this invention is the magnetic force field which is specific for the knuckle positioned magnet-actuated coupler and will not activate delayed uncoupling of other currently available magnet-actuated couplers. Another distinctive feature of the instant system is that no other magnetic force field design, except the outside-the-track force field described in this invention, will facilitate the magnet-actuated coupler of this invention to respond to delayed uncoupling. The combination of the magnet-actuated coupler with the outside-the-track magnetic force field, therefore, provides a unique magnetic coupler system.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be more readily understood by referring to the accompanying specifications, consisting of drawn figures and the detailed description, which are intended as illustrative of the invention rather than as limiting the invention to the specific details herein set forth.
FIGS. 1, 3 and 5 are the overall, side and front views, respectively, of a conventional hook type coupler.
FIGS. 2, 4 and 5 are the overall, side and front views, respectively, of the knuckle positioned magnetic-actuated coupler according to this invention.
FIGS. 7 and 9 are the front and top views, respectively, of a conventional coupler pocket housing.
FIGS. 8 and 10 are the front and top views, respectively, of suitable coupler pocket housing for this invention.
FIGS. 11 and 13 are the top and front views section, respectively, of the rail track.
FIGS. 12 and 14 are the top and front views, respectively, of the rail track containing the preferred parallel separate bar magnets in place, constituting the magnetic force field.
FIGS. 15-A, 15B, 15C and 15D is a top view illustration of the delayed uncoupling mechanism in action according to the features of this invention.
DETAILED DESCRIPTION OF THE INVENTION
To make the instant invention readily understandable and distinguishable, a comparison to a conventional coupler is provided. A conventional coupler, commonly used on "HO" gauge rolling stock is illustrated in FIGS. 1, 3 and 5. As depicted in FIGS. 2, 4 and 6, the instant invention closely resembles the prototype in its physical appearance. This is shown wherein the length of the horn 1 is reduced to achieve the apearance of tip 2. Preferably gap 3 is filled with a plastic molding material and shaped to a knuckle-like appearance 4 being defined by the outer end of the draw bar. The uncoupling pin 5, located on the conventional coupler may be completely removed for operational purposes of this invention. A curved ferromagnetic component 6, best viewed in FIGS. 4 and 6, may be inserted into a predrilled hole in the underside portion of knuckle 4, adjacent to post 7, attached to bypass 8. The curved ferromagnetic component 6 may be angled toward the tip 2, best viewed in FIG. 6. Preferably the shape and position of the ferromagnetic component 6, attached to knuckle 4 of the coupler, adds to the prototypical appearance of the coupler with the preferred curve for ferromagnetic component 6 closely resembling the air hose on life size rolling stock. For the most effective magnetic pull on the coupler, the distance between the bottom of the ferromagnetic component 6 and the surface of the track is preferably slightly less than about 1/32 inch. The position and angle of the curved ferromagnetic component 6 accomplishes cooperation with the bar magnet 22, best viewed in FIGS. 12 and 14, positioned on the outside face of the rail, such that the tip of the curved ferromagnetic component 6 operates in a manner that facilitates delayed uncoupling, as further illustrated in FIG. 15-A.
The off-centered position and angle of the ferromagnetic component 6 of the knuckle positioned magnet-actuated coupler of this invention does not interfere with pin 5 of a conventional coupler when the two couplers are used together in a recoupling operation. Interference between the ferromagnetic component 6 with the pin 5 of a conventional coupler is prevented since face 9 of the instant coupler engages with the opposite face of the conventional coupler allowing component 6 to slide past pin 5 as the couplers engage in recoupling.
In order for the bar magnets 22, shown in FIGS. 12 and 14, to active and attract the knuckle positioned magnet-actuated coupler to a full open position, according to this invention, the tension of the attached spring 10 of FIG. 2 may be reduced, preferably by reduction in the thickness of the spring as shown at position 11. The tension of the instant spring must be such that bar magnet 22 moves the coupler to a point where bypass 8 on one coupler clears the bypass of its companion coupler, illustrated in FIG. 15-B and C, to facilitate delayed uncoupling. Moreover, the tension of spring 10 is at the same time sufficient to allow recoupling with conventional stiff sprung couplers.
In comparison to conventional couplers, the forward portion of the draw bar immediately behind knuckle 12 may have cut out sections as shown at position 13 and position 15. Therefore, the knuckle positioned magnetic coupler can open to its maximum in the coupler pocket housing so that delayed uncoupling is achieved, as shown in the operational sequence A, B and C, depicted in FIG. 15. Conventional couplers may vary for individual manufacturing design of the draw bar, leaf spring and respective coupler pocket housing. As shown in FIGS. 2 and 4, the bypass 8 on one coupler does not interfere with the bypass on the opposite companion coupler. In this invention a thin shim 16, FIGS. 8 and 10 may be inserted into the coupler pocket housing at point 17 to arrest the coupler in a more centered position within the coupler pocket housing when in a ready to couple position outside of the magnetic force field, as illustrated in FIG. 15-D.
When the knuckle-positioned magnetic coupler re-enters the magnetic force field, magnetic lines of force actively engage the ferromagnetic component 6, drawing the coupler laterally outward from the over the outside edge of the rail to a maximum open position to facilitate uncoupling by a delayed mechanism. Neither a magnetic field placed between the track rails or a wider magnetic field placed directly beneath the track ties will activate the thus arranged knuckle-positioned magnetic coupler to uncouple by delayed action. An outwardly aligned magnetic force field 26 of this invention will, however, accomplish the uncoupling.
The unique design of the magnetic force field 26, arranged specifically to actuate the herein described knuckle positioned magnetic coupler for delayed uncoupling, is further illustrated in the embodiments of FIGS. 12 and 14. In a preferred embodiment of the instant invention, bar magnets are positioned flat against the track in an outside position. It is an essential feature of this invention that an outside track position is held for proper concentration of the magnetic force. For descriptive purposes, several tie ends 18, may be viewed in FIG. 11, as cut away from the track shown in FIG. 12, with cut-out at position 19 to 20 of the track rail and parallel magnets 22 affixed flush to the rail 21, as shown in FIGS. 13, and 14. Preferably, a 3/16 inch bar magnet 22 is fitted on the outside of the track with the surface of the bar magnet even with the surface of the rail. The strength of the bar magnets and positioning on the track work is closely controlled so that the magnetic force field 26 will (1) allow the use of rolling stock equipped with ferromagnetic axles, wheels and/or truck frames and (2) retain a normal track appearance. The uncoupling site is not easily noticed on a railroad layout when the preferred bar magnets are inserted into the track system "as is" or are concealed in rerailing, crossover and/or switch track assemblies. If too powerful magnets are used, the first advantage no longer applies, since rolling stock equipped with ferromagnetic wheels will "wobble" in a magnetic force field and cause problems in delayed uncoupling. If physically larger magnets are used, the second advantage is lost since these would be easily noticed on the railroad track layout and would be difficult to conceal in rerailing, crossover or switch track assemblies.
In a preferred arrangement of this invention, a 1/32 inch thick steel plate 23, is placed under two bar magnets 22 to cover an area that extends from the outer edge of one bar magnet across and under the ties, over to the outer edge of the opposite bar magnet, as depicted in FIGS. 12 and 14. Positioning of the steel plate 23, directionally orients and concentrates the magnetic force lines to be outwardly displaced over each rail to facilitate full opening of the wide pivot radius of the knuckle positioned magnetic coupler for delayed uncoupling. The bar magnet 22, can be metal, ceramic and/or a plastic material and the magnetic field 26, may be either a permanent one or an electro-magnetic type, preferably activated by means of an automatic push button or switch device. If bar magnets 22, are in direct contact with the track rail at the tee stem positions 21 of FIG. 14, and a steel plate 23 connects both bar magnets 22, it is necessary to insert an insulator, such as a micro-thin strip of plastic (polyethylene) non-conductor between the bottom of each bar magnet 22 and the steel plate 23 to avoid a short circuit between the plus and minus track rails and, particularly if electrically conducting bar magnets other than the plastic types are used in the system. The unique design features of the magnetic force field 26, is specific for the knuckle-positioned magnetic coupler and will not activate delayed uncoupling of available commercial magnet-actuated couplers.
The overall mechanism for delayed uncoupling employing this system is best viewed sequentially in A, B, C, and D of FIG. 15. When rolling stock is pulled across the magnet force field, the couplers remain engaged. However, when the rolling stock is stopped over the magnetic force field and slack is allowed between the couplers, as shown in FIG. 15-A, the couplers disengage and withdraw to their outer respective rail tracks as shown in FIG. 15-A. When the rolling stock is reversed, FIG. 15-B, the bypass 8 on one coupler passes its companion bypass on the other coupler to a point where both coupler faces 9 engage with the stopping block 24 extending outward from the side of the coupler pocket housing of FIG. 8, and/or the bypass 8 on each coupler engages with the stopping block 25 extending downward from the front of the coupler pocket housing f FIG. 8, thus preventing the couplers from moving too far below each other car's underframe. In this position, the locomotive can now move the rolling stock outside of the magnetic force field and drop the uncoupled car at any desired point on a model railroad layout. When the locomotive moves away from the uncoupled car as shown in FIG. 15-C, the couplers slide over each other at the bypass position 8, such that the couplers will not re-engage in coupling but, in fact, allow the uncoupled car to be left at its desired location. Since the geometrical configuration of the bypass 8 varies from one conventional coupler to another, it is essential to compatibility that the shape be adjusted, such that recoupling does not occur when the rolling stock is being moved away by the locomotive from the uncoupled car. Once the cars have been uncoupled by the delayed mechanism, the couplers return to their normal centered position within their coupler pocket housing and are ready to recouple, as shown in FIG. 15-D. In essence, this illustrates the mechanism for delayed uncoupling of the knuckle positioned magnet-actuated coupler over the specially designed double bar magnet force field.
Rolling stock derailments and inadvertent uncoupling, attributed to the uncoupling pin of the conventional coupler, is eliminated by this invention wherein neither the magnet-actuated coupler nor the conventional couplers used in the system require a pin for any operational purpose. This is accomplished by positioning a ferromagnetic element on the knuckle portion of the magnet-actuated coupler and applying a specially directed magnetic force field for full opening of the coupler to allow for delayed uncoupling. The knuckle positioned magnet-actuated coupler of this invention does not respond to a magnetic force field placed either between the rail track or to a wider magnetic force field placed directly beneath the track ties. To operate the knuckle positioned magnetic coupler, the force field is constructed with two separate bar magnets in parallel position on the outside face of each rail opposite the other to effect a wider pivot radius for opening in delayed uncoupling.
Moreover, the double bar magnet force field does not facilitate activation of any other magnet-actuated coupler for delayed uncoupling and is specific for the knuckle-positioned magnet-actuated coupler of this invention. The knuckle-positioned coupler will disengage or uncouple from conventional couplers over the outside-the-track magnetic field. Since the preferred bar magnets of this invention are sufficiently far apart on the track, and the magnetic field pull between the rails is reduced, such that rolling stock equipped with ferromagnetic wheels, axles and/or truck frames do not "wobble" in the magnetic field to the degree evidenced with prior art magnetic fields that have a bar magnet positioned either in between the rails or directly under the rail ties.
Since a large variety of "HO" gauge rolling stock is equipped with conventional hook horn type couplers, the new magnetically-automated delayed uncoupling system is desirable for combined functional compatibility in coupling, uncoupling and delayed uncoupling operations. Rolling stock currently limited to a coupler pocket housing that is designed to accept only a conventional hook type coupler, may be now easily adapted to accept the magnetic coupler of this invention. The model railroader is thus provided with more economical rolling stock since it would no longer be necessary to replace couplers to ferromagnetic axles, wheels and/or truck frames with costly substitutes. Major manufacturers of "HO" gauge rolling stock can now easily adapt their process with a minimum of investment in production setup to produce a magnetically-automated delayed uncoupling system. The knuckle-positioned magnetic coupler may be one molded piece comprising knuckle, draw bar, and leaf spring with the magnet attached later to the knuckle.
While the invention has been described with specific embodiments thereof, it will be understood that it is capable of further modification and adaptions or variations as apparent to those skilled in the model railroading art. | A magnetically automated delayed uncoupling system consisting of a knuckle positioned magnet actuated coupler and a parallel outside-the-track magnetic force field which permits use of ferromagnetic train wheels without wobble and provides delayed uncoupling and coupling. The improved system is compatible with hook type couplers when used in combination therewith. | 0 |
BACKGROUND
1. The Field of the Invention
This invention relates to equipment for maintaining and repairing heat exchangers and, more particularly, to novel systems and methods for use in pulling tubes from heat exchangers for replacement.
2. The Background Art
A heat exchanger is any apparatus constructed for transferring heat from one object or medium to another. One type of common heat exchanger passes one fluid through tubes, and a second fluid flows over the outside of the tubes. Heat is exchanged between the fluid inside the tube and the fluid outside the tube. Heat will flow from the hotter fluid to the cooler fluid. Tubes may be provided with fins on an inside surface or on an outside surface to improve performance. Either fluid (inside or outside the tube) may be a liquid or a gas. A most common example of a heat exchanger is an automobile radiator. Another is a cooling coil on the back of a household refrigerator. Less visible, but equally common, heat exchangers include water heater cores, home furnace boilers, industrial boilers, and expansion coils in an air conditioner.
Industrial heat exchangers are often of the "shell-and-tube" type. A long shell or tank is provided with a bulkhead near each end. The bulkheads are provided with a latticework of closely spaced circular perforations. The perforations are sized to receive long tubes. Tubes fitted into the perforations extend from one bulkhead to the other. Tubes may be welded or swaged into place in the bulkheads, each forming a fluid-tight seal.
A shell-and-tube heat exchanger is typically assembled with one end of the tank and one bulkhead forming a first chamber or plenum. This end of the tank is provided with an inlet line (inlet pipe) for receiving fluid. The opposite end of the tank and the other bulkhead form a second plenum having an exit line (outlet pipe) for discharging fluid from the heat exchanger. Fluid can pass through the inlet line to the first plenum, into the tubes passing through the perforations in the first bulkhead, through the length of the tubes, out of the tubes at their ends passing through the second bulkhead, into the second plenum, and out of the second plenum through the exit line.
The bulkheads form another chamber or plenum. The walls of this plenum are formed by the bulkheads, the shell or tank wall extending between the bulkheads, and the outer surface of the tubes. An inlet line and outlet line pass fluid into and out of this plenum. Within the plenum, the fluid passes over the outside surfaces of the tubes "bundled" close to one another by the bulkheads. Thus, heat is transferred between the fluid inside the tubes and the fluid outside the tubes.
When tubes have been used for their useful life, they may be corroded (rust for example) or fouled (covered or plugged up by deposits). Corrosion may thin the walls of the tubes or pit them. Fouling typically occurs as stone-like deposits of various compounds precipitate out of the fluids passing through the tubes. Fouling deposits may accumulate on the inside surface, outside surface, or both, of a tube. Deposits inside a tube may completely block the tube, creating a rock-like "plug" in the tube.
Some heat exchangers have tubes that can be replaced. The shell is opened, exposing the bulkheads with their banks of tubes. Each tube is first broken free from the bulkhead (the "breaking" operation). Breaking often employs a combination of cutting or pressing, followed by a pull of a few inches. A hydraulic press of the collet type or the screw type may typically be used. The press engages one end of the tube and draws the tube through the bulkhead a distance of several inches.
After the tube is broken free, it must be removed. The hydraulic press cannot remove the tube. A longer stroke than that of the hydraulic press is required. Therefore, a mechanism is required to grasp a tube and draw it out quickly and completely from the bulkhead.
The hydraulic press has a very high force (tens of tons) over a very short stroke (distance of several inches). Compared to the hydraulic press, a lesser force (less than a ton, often less than 100 pounds) is adequate for removal of a tube. However the tube must be moved its entire length. The length of a tube may be from several feet to several dozen feet.
Numerous patents and other technical articles disclose methods for removing long tubes. The pullers for long tubes are sometimes referred to as travelers. The term "traveler" emphasizes the nature of the longer pulling operation at reduced force (the "traveling" operation) as compared to the short, powerful stroke of the hydraulic press in the "breaking" operation.
A traveler typically includes multiple, powered, synchronized wheels rotating opposite one another in close proximity. These "drive wheels" grasp and crush a tube between them. Helical springs provide the crushing force to keep the drive wheels close together. As a tube is crushed, it passes between the powered rollers.
The machinery for traveling is usually large and heavy. The operators must move the heavy traveler into position. Because the traveler is large, operators may not be able to see around it. Operators may have difficulty guiding the traveler toward the end of the tube if they cannot see it.
Also, the tube is ejected out the back of the traveler very rapidly. Moreover, the tube may be free to warp in any direction, because it is crushed, sometimes to a very thin, ribbon-like appearance. Unless one operator holds onto the tube to guide it, the tube may injure people, damage machinery, or clutter the work area.
The size also interferes with the breaking operation. If more than one tube extends away from the bulkhead (also called a tube sheet) within an area the size of the front face of the traveler, the traveler cannot reach the tubes. Each tube interferes with the traveler's approach to the other tubes. Thus, only one tube within a large area can be broken free in the breaking operation before the traveling operation must occur. That is, one tube is typically broken free, after which that tube must be traveled before the next tube can be broken free.
The hydraulic press is operated by a "breaking" operator, and the traveler is operated by a "traveling" operator. The breaking operator and the traveling operator must wait for each other, effectively operating in series. Only one operator and one machine are active at any time. Thus, one operator and one machine are idled (wasted) at all times.
The frequent exchanging of positions between the breaking and traveling operators adds additional wasted time. Moreover, the traveler must be moved large distances to accommodate the frequent exchange of positions. Safety is a concern in this circumstance where large pieces of heavy, powered equipment are moved rapidly about a constricted working area by a team of at least three workers (for breaking, traveling, and tube guiding at the exit of the traveler, respectively).
The great weight of the traveler makes large hoists necessary to move the traveler between tubes in a single bundle. A hoist requires additional controls to move the traveler up, down, right, left, forward and backward to the tube. These controls must be operated in series with the traveling operation, distracting the operator. Of course, the positioning of the traveler with the hoist is idle time in which tubes are not being traveled.
The size of the traveler is largely due to the complex machinery, multiple hoses, multiple hydraulic motors, and mounting hardware required to support the hydraulic loads.
In addition, the reliability of a machine is dependent on the number of parts, particularly moving parts. The travelers typically used have numerous, powered, moving parts.
Another difficulty with current travelers is their reliance on multiple drive wheels for engaging the tube. Making one drive wheel movable with respect to another adds parts, cost, complexity, weight and size. However relative translation is necessary for accommodating "plugs," large blockages of fouling deposits inside a tube.
If a plug is encountered in the tube, the traveler may be damaged. Some travelers release the drive wheels drawing the tube. However, the wheels typically can move only a very short distance apart. Moreover, the helical spring forces are not balanced or proportional with respect to the driving forces exerted by the drive wheels. Thus, the tube may stall or not engage properly when the drive wheels spin against the tube. If springs holding the drive wheels together are too strong, the drive wheels may not open properly at their nip point to grasp a larger tube and crush it initially. Yet, if springs are not strong enough, crushing may be hampered.
The size of the nip between drive wheels must be large enough to feed a tube, yet small enough to permit grasping the tube after crushing. Too high a spring load makes engagement of the tube difficult in the nip. Too low a spring load hampers crushing and may allow slipping when a plug is encountered. The crushing forces are not typically balanced with the driving forces of the drive motors.
Travelers are not typically guarded. A crushed tube is simply ejected from the back side of the traveler. The tube may bend in any direction, striking workers. A second person, in addition to the traveling operator is typically required to grasp a long, exiting tube and direct it.
BRIEF SUMMARY AND OBJECTS OF THE INVENTION
In view of the foregoing, it is one object of the present invention to increase the reliability of tube travelers.
Another object of the invention is to reduce the weight, size and the profile of a tube traveler.
It is an object of the invention to provide easier access to tubes to be traveled, and to allow breaking free more tubes before requiring traveling.
One object of the invention is to improve the speed at which the operations of breaking and traveling may be conducted.
It is an object of the invention to reduce the number of times that a breaking operator and a traveling operator must exchange places to obtain access to the workpiece (tube bundle).
It is an object of the invention to provide single-handed operation of the controls for a tube traveler.
One object of the invention is to provide safe handling of plugged tubes without damage to the traveler.
Another object of the invention is to provide for rapid opening, clamping and loading of a traveler on tubes.
Another object of the invention is to provide a more nearly constant load on the tubes being traveled.
Another object of the invention is to apply proportionally the clamping forces acting on a tube and the force of the drive wheel acting to travel the tube.
Another object of the invention is to guard workers against ejection of tubes in a random direction.
Another object of the invention is to travel tubes with an apparatus having fewer parts, fewer moving parts, fewer powered parts, fewer hydraulic motors, and fewer drive wheels than are currently required.
Consistent with the foregoing objects, and in accordance with the invention as embodied and broadly described herein, an apparatus is disclosed in one embodiment of the present invention as a traveler for removing tubes from a tube sheet. The apparatus includes a frame holding a motor having a housing secured to the frame. A rotatable shaft extends away from the housing.
A driver connects to the shaft to rotate with the shaft. The driver is positioned to contact a tube to be pulled. The driver contacts the tube at the outer diameter of the tube. Upon rotation, the driver urges the tube to move in a longitudinal direction. The driver may include an axle, a bearing and a wheel. The shaft of the motor may serve as the axle. The wheel may have teeth for increasing the stress applied to the tube. A controller connects to the motor for controlling the rotational speed of the driver.
An idler rotatably connects to the frame. The idler is free to rotate in at least one direction without appreciable resistance. The idler may urge the tube in a lateral direction against the driver. The idler and driver tend to collapse one portion of a wall of the tube toward another portion of the wall.
A carriage is connected to the frame to rotatably carry the idler. The carriage may slide, pivot, or the like with respect to the frame. The carriage may selectively position the idler with respect to the driver. An actuator is connected between the frame and the carriage holding the idler. The actuator selectively moves the idler between a first position away from the driver and a second position proximate the driver.
A fluid (working fluid) is selectively moveable into and out of the actuator for urging the actuator between the first position and the second position. The fluid may be oil, air, or an equivalent. The fluid may be incompressible or compressible.
A buffer may be in fluid communication with the actuator for absorbing impacts received by the actuator. A buffer is preferred when the working fluid is an incompressible liquid.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing and other objects and features of the present invention will become more fully apparent from the following description and appended claims, taken in conjunction with the accompanying drawings. Understanding 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 with additional specificity and detail through use of the accompanying drawings in which:
FIG. 1 is a partially cutaway isometric view of one embodiment of an apparatus in accordance with the invention;
FIG. 2 is a side elevation view of the apparatus of FIG. 1;
FIG. 3 is a front elevation view of the apparatus of FIG. 1;
FIG. 4 is a front quarter isometric view of the apparatus of FIG. 1;
FIG. 5 is an isometric view of one embodiment of a driver of the apparatus of FIG. 1;
FIG. 6 is an isometric view of an alternate embodiment of an idler of the apparatus of FIG. 1;
FIG. 7 is an isometric view of an alternate embodiment of an idler of the apparatus of FIG. 1 connected to a unidirectional clutch;
FIGS. 8-10 are top plan views of alternate embodiments of the carriage and idler of the apparatus of FIG. 1;
FIGS. 11-13 are side elevation views of alternative embodiments of carriages in the apparatus of FIG. 1;
FIGS. 14-15 are side elevation views of alternative embodiments of actuators for the apparatus of FIG. 1; and
FIGS. 16-18 are schematics of alternative embodiments of controls for controlling the apparatus of FIG. 1.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
It will be readily understood that the components of the present invention, as generally described and illustrated in the Figures herein, could be arranged and designed in a wide variety of different configurations. Thus, the following more detailed description of the embodiments of the system and method of the present invention, as represented in FIGS. 1 through 18, is not intended to limit the scope of the invention, as claimed, but it is merely representative of the presently preferred embodiments of the invention.
The presently preferred embodiments of the invention will be best understood by reference to the drawings.
Structure of the Apparatus
The apparatus is best understood by reference to FIGS. 1-18 wherein like parts are designated by like numerals throughout. Referring particularly to FIGS. 1-4, an apparatus 10, for traveling tubes 11 that have been broken free from a tube sheet includes a frame 12. The frame carries a driver 14 rotating under the power of a power supply 16. An idler assembly 18 provides an opposing, rotatable member opposite the driver 14. The idler assembly 18 is carried by a clamping assembly 20 for selectively moving the idler assembly 18 toward and away from the driver 14. The clamping assembly 20 is movably captured within the frame 12. The clamping assembly 20 may translate or pivot with respect to the frame 12. A control system 22 (see FIGS. 16-18) controls the operation of the clamping assembly 20 and the driver 14. A guard 24 may guide a crushed tube 11 away from the frame 12.
A driver 14, in general, may include a wheel or its equivalent for urging a tube 11 out of a position (e.g., in a bulkhead or tube sheet). The wheel may be toothed, knurled, tired, or otherwise treated to grasp a tube 11 and crush it. A driver 14 may include for example a wheel, sprocket, gear, chain, belt, or track. A driver 14 advances the crushed tube 11 even while crushing it. A driver 14 is used to engage a tube 11 and move it in a longitudinal direction. A driver 14 includes the associated axles and bearings, and supports to operate within a frame 12.
The frame 12 is understood by reference to FIGS. 1-4 in which a head block 30 and a foot block 32 are attached together by a left side block 34A and right side block 34B. A bearing aperture 36 may, for example, be formed within each of the side blocks 34A, 34B. A cover plate 38 may be provided and may be positioned and sized to provide protection within the frame 12. The cover plate 38 may be a structural, load-bearing member, depending on the sizing of the head block 30 and foot block 32. Ways 40A, 40B may be provided in the frame 12 to restrain the clamping assembly 20 to movement along a single linear direction. Brace blocks 42 may be connected at selected locations between the side blocks 34A, 34B to improve structural integrity or to serve as guides or guards. (See FIGS. 12-13.)
The driver 14 is best understood by reference to FIGS. 1-5. The driver 14 includes a wheel 50, that may be constructed to have teeth 52. The teeth 52 have a depth 53 permitting the edge 54 of the teeth 52 to apply sufficient force and stress against the side of a tube 11 to be pulled. A buttress 56 of each tooth 52 supports the edge 54 of the tooth 52. Since stress is force per unit area, a narrow edge 54 increases the gripping ability of the wheel 50. That is, the larger the buttress 56 portion of the tooth 52, the less the portion of the tooth 52 near the edge 54 applying force to grip a tube 11.
The driver 14 also may include bearings 84 (see FIG. 6) retained in the bearing apertures 36 for carrying an axle 60 (see FIGS. 1-5). The axle 60 supports and rotates the wheel 50. The wheel 50 is sized to provide a nip point 62. The nip point 62 is related to the nip 64, defined by the gap or clearance 66 between the driver 14, and the idler assembly 18. The nip point 62 is a position at which a tube 11 is engaged by the wheel 50 and drawn into the nip 64. Outside the nip point 62, (further away from a plane defined by the axles 60, 82) a tube 11 may simply be kicked away from the wheel 50 by the striking of the teeth 52. Inside the nip point 62, a tube 11 is captured by the teeth 52 of the wheel 50 and pulled on into the nip 64.
The power supply 16 may include a motor 70. The motor 70 may be electric, pneumatic or hydraulic. The supporting members of the power supply may include those means known in the art for driving, regulating, switching and otherwise supporting the motor 70. For example, a pneumatic or hydraulic type of system may rely on a pump driven by a motor for generating a supply of fluid under pressure. A power supply may include regulators, buffers, sumps, vents, pressure relief valves and lines (conduits) for transferring the working fluid between such components.
A motor 70 in one presently preferred embodiment of the apparatus is hydraulic. Relatively incompressible working fluids (hydraulic oil, for example) provide ready speed control in a positive displacement motor. Hydraulic motors also provide maximum torque density at the motor 70. That is, the most torque in the smallest motor 70 is typically available in hydraulic systems. However, the inlet line 72 and outlet line 74 may extend to a large pump 224 and reservoir 226 or sump 226 located remotely from the motor 70.
Thus, the torque per unit of volume provided through the shaft 60 by the motor 70 is larger than that for an electric motor 70. However, an electric motor 70 has the advantage that it does not require such a large supporting physical plant as the pump 224 and reservoir 226 or sump 226 of a hydraulic system.
Likewise, pneumatic motors 70 may serve well. Pneumatic motors operate on different principles, however, and must be treated somewhat differently. Pneumatic motors 70 can accumulate pressurized working fluid (air) when stalled. The motor may stall when a plug (large, fouling deposit) is encountered in a tube 11. The high pressure may lead to a burst of speed once the load resisting the motor 70 is overcome by the motor 70. If pressure is regulated to prevent excess pressure, torque is limited and the motor may stall until relieved. Electric motors 70 may fail if stalled. Electric motors 70 also have less torque than a similarly rated hydraulic motor 70. Therefore, these differences may affect the choice and use of electric motors 70, pneumatic motors 70, and hydraulic motors 70.
The shaft of the motor 70 may double as the axle 60. With suitable methods for mounting the bearings 58 and the motor 70, the wheel 50 may be keyed or splined to the shaft 60 directly. This arrangement may risk the shaft 60 bending under excessive loads, but results in fewer components moving with respect to one another.
The idler assembly 18 is best understood by reference to FIGS. 4-10. The idler assembly 18 includes an idler 80 supported by an axle 82. The bearing 84 may be secured inside the idler 80 to permit the axle 82 to be non-rotatably mounted. The idler 80 is free to rotate in this embodiment.
An idler assembly 18, in general, may include any wheel (idler 80) or its equivalent, having no source of power directly connected to urge rotation. Rather the idler 80 simply rotates with anything that contacts it, such as a tube 11 being moved by a driver 14.
Alternatively, the axle 82 may be fixedly mounted to the idler 80 to rotate with the idler 80. In this embodiment, the bearing 84 may be mounted in the frame 12 to support the axle 82 rotating within the bearing 84 as in FIG. 6. The idler 80 may be secured to the axle 82 by splines 86 on the axle 82 fitted to matching splines 88 in the idler 80. Alternatively, the idler 80 may be keyed like the wheel 50 of FIG. 5. The idler may be completely free to rotate, or free to rotate in only one direction.
In FIG. 7, the idler 80 may have teeth 90 having a height 92 and pitch 94 selected to engage the tube 11 being pulled (traveled). The wheel 50 of the driver 14 may be similarly constructed. However, the idler 80 and wheel 50 operate somewhat differently. The surface 98 of the idler 80 serves to crush the tube 11, although the edge 96 actually provides the principal means for engaging the tube 11, and for crushing. That is, the edge 96 tends to actually dig into a tube 11 while applying a crushing force.
The unidirectional clutch 100 (sometimes called a "no-back clutch") may be connected between the frame 12 and the idler 80. The unidirectional clutch 100 permits the idler 80 to rotate in the forward direction 106A. The idler 80 is restrained by the clutch 100 from moving in the backward direction 106B. Thus, the idler 80 does not provide power to advance the tube 11. That power is provided by the driver 14 through the wheel 50 to the tube 11 being traveled. The tube 11 actually rotates the idler 80. However, once rotated in the forward direction 106A, the idler 80 is not free in this embodiment to retreat in a backward direction 106B.
A no-back clutch 100, in general, may be any unidirectional clutch. The clutch 100 may include a mechanism that attaches to a rotating first member and a second member. The first member is free to rotate in a first direction with respect to the second member. However, the first member is restricted from rotating in a second direction opposite the first direction.
Nip points 62, 104 exist for the wheel 50 and idler 80, respectively. The nip point 104 for the unpowered idler 80 may be located more remotely from the nip 64, because the idler 80 is not powered. In one embodiment, the idler 80 can be larger than the wheel 50 to promote engagement of the tube 11 by the nip 64. In another embodiment, a series of rollers (not shown) may be located ahead of the idler 80 to promote feeding the tube 11 into the nip 64. In a less preferred embodiment, the idler 80 may be replaced by another wheel 50 and associated driver 14. However, the motion of the carriage 110, among other features, can eliminate the need to deliver power to the idler 80.
In one alternative embodiment, no unidirectional clutch 100 is used, and the teeth 90 are oriented in an opposite direction from that of FIG. 7. Thus, the tube 11 more easily engages the idler 80 to rotate the idler 80.
The carriage 110 may be embodied in a slide 112 as illustrated in FIGS. 1-4 and 8-10. The slide is free to move in the clamping direction 111A, but is restrained in the fore and aft direction 111B and lateral direction 111C. The slide 112 carrying the idler 80 operates with a stroke 113 to change the clearance 66 between the idler 80 and the wheel 50.
Alternatively, the carriage 110 may be embodied as a jaw 114 pivotably attached to the frame 12 as illustrated in FIGS. 11-13. The carriage 110 may be moved by an actuator 115, regardless of the embodiment chosen for the carriage 110.
The slide 112 may include side panels 116A, 116B fixed to a base block 118. The side panels 116A, 116B may be provided with lands 120A, 120B, respectively fitted to slide within the ways 40A, 40B, respectively, of the frame 12. (See FIGS. 1-4 and 8.) In one embodiment a front block 122 and back block 124 may be secured between the side panels 116A, 116B to add structural strength, rigidity, or both. The front and back blocks 122, 124 also serve to enclose the idler 80 for cleanliness and protection.
Alternatively, the ways 126A, 126B may be formed in the side panels 116A, 116B, respectively, for capturing therein the lands 44A, 44B. (See FIG. 9.) The lands 44A, 44B may be formed on or attached to the side blocks 34A, 34B, respectively. With proper lubrication, the trapezoidal ways 40A, 40B, 126A, 126B and their respective lands 44A, 44B, 120A, 120B may provide both retention and bearing for the slide 112 type of carriage 110.
In another embodiment, the rails 128A, 128B may be mounted to the side blocks 34A, 34B respectively. The side blocks 34A, 34B restrain and bear the slide 112 in the lateral direction 111C. The rails 128A, 128B restrain and bear the slide 112 in the fore and aft direction 111B.
The carriage 110 embodied in a jaw 114 is illustrated in FIGS. 11-13. The jaw 114 of FIG. 11 includes a mandible 130, and may have a ramus portion 131. The jaw 114 is pivotably connected to the frame 12 by the pivot shaft 132 extending between the left and right side blocks 34A, 34B.
Actuation of the slide 112 may be hydraulic, pneumatic, electric, or manual. However, the jaw 114 and the slide 112 can be actuated by analogous means. The actuation of the jaw 114, however, presents several alternatives affecting the embodiment of the jaw 114.
An actuator 115 may be a hydraulic or pneumatic cylinder 134 or equivalent apparatus for linear actuation. The cylinder 134 in the illustrated embodiment includes a base 136 having an eye 137 provided with an aperture 138 for receiving an anchor shaft 140. The anchor shaft 140 and pivot shaft 132 may be similarly attached to the frame 12.
A ram 142 is extendible from the cylinder 134, and may be selectively extendible. The ram 142 may also be selectively retractable if the cylinder 134 is a double acting cylinder. A head 144 is connected to the ram 142. The head has an eye 145 provided with an aperture 146 therein for receiving a swing shaft 148.
The mandible may be constructed as the slide 112 to have side panels 116A, 116B, base block 118, and front and back blocks 122, 124. Construction would preferably be modified to optimize the permitted physical motion of the jaw 114 in carrying the idler 80 toward and away from the wheel 50. Optional brace blocks 150 may be mounted to extend between the side panels 116A, 116B of the mandible 130 as needed for structural strength and stability.
Suitable bearings, journals, bushings or other means for friction reduction (not shown) are preferably interposed between the frame 12 and the jaw 114. Such means may be attached in an embodiment to support each shaft 132, 140, 148. Alternatively, a friction-reducing structure could be connected to support the jaw 114 on the shafts 132, 140, 148. The various combinations of these alternatives are also contemplated.
An actuator 115 may be a hydraulic cylinder, pneumatic cylinder, four-bar linkage (not shown), or equivalents, each with a somewhat different result. The actuator 115 may be capable of selective actuation.
The embodiments of FIGS. 14-15 illustrate a housing 160 having a wall 161. A ram 162 is extendible from the housing 160, and may terminate in threads 164 or other suitable means for attachment. To form a more compact frame 12, a length 163A of the housing 160 may be minimized by adding a secondary ram 165 and tertiary ram 166 located concentrically with the ram 162, as illustrated in FIGS. 1 and 15. The diameter 163B inside the housing 160 may be selected to optimize the force applied by the ram 162 for the range of pressures expected from the power supply 16.
Oil 167 may be used, (or air in pneumatic systems) as a working fluid provided by the power supply 16. Seals 168, 169 may be `O` rings 168, 169 for sealing the rams 162, 165, 166 against leakage of the working fluid. Oil 167 is substantially incompressible. That is, it will not change volume more than a few percent under contemplated operating conditions. Air by contrast is compressible, changing volume by approximately 100 percent with an approximately 50 percent decrease in absolute pressure.
A piston 170 may be secured to a ram 162 as in FIG. 14, or the ram 162 may serve the piston function as in FIG. 15. In either embodiment and their variations, an actuator 115 may be double acting. An extension line 174A may provide oil 167 under pressure from the power supply 16. The actuator 115 may receive a working fluid such as oil 167 from a power supply 16 through a retraction line 174B to retract the ram 162 into the housing 160 in a double-acting embodiment.
More than one power supply 16 may be used. For example, the actuator 115 and the motor 70 could be powered pneumatically and hydraulically, respectively. Alternatively, a single power supply 16 may be configured to provide oil 167 to the motor 70 and the actuator 115.
Other lines 174C may be added to a single-acting embodiment to conduct exiting oil 167 away. Alternatively, an actuator 115 may be single-acting and rely on a single line 174A both for introducing oil 167 for extension and for conducting away exiting oil 167 for retraction. In a single-acting embodiment, the idler 80 on the carriage 110 connected to the end 172A of the ram 162 would not be retractable under power. Instead, a means for biasing the ram 162 toward a retracted position would preferably be used. Retraction is not required, although preferred.
The buffer 180 may be separated (FIG. 14) or integrated (FIG. 15) with the actuator 115. The buffer may include a piston 182, diaphragm (not shown), or equivalent movable member having two sides 186A, 186B to separate the working fluid (oil 167 in the illustrated example) from a gas 188.
The piston preferably moves in a direction 190A in response to an impact on the idler 80. For example, when the idler 80 encounters a plug in a tube 11, the idler 80 moves away from the driver 14 and the associated wheel 50. Moving with the idler 80, the carriage 110 pushes the ram 162 into a retracted position. The oil 167, being incompressible cannot reduce appreciably in volume, but pushes against the piston 182 instead. The oil 167 may reach the piston 182 indirectly after passing through a line 174D to the buffer 180 separated from the actuator. (See FIG. 14.) Alternatively, the oil 167 may reach the piston 182 directly in an integrated buffer 180 (See FIG. 15.)
When the plug has passed by the idler, the buffer 180 returns in the direction 190B, forcing oil 167 back into the actuator 115. A stop 192 may be provided to restrict the return motion of the piston 182 or to pre-pressurize the buffer 180 at a fixed volume. The pressure of oil 167 may automatically adjust the pressure of the gas 188 in the buffer 180, particularly if the piston 182 is not arrested by the stop 192.
Control of the traveler 10 is best understood by reference to FIGS. 4 and 16-18. The frame 12 may be mounted by a suitable support (not shown) to be movable by an operator. The frame 12 may be moved directly by an operator to a tube 11 to be pulled using handles 194. Near the handles 194, an operator may control the supply of oil 167 (or other working fluid) to the motor 70 and the actuator 115. For example, the operator may activate a trigger 196 and its restrictive interlock 198 combined for safety as the switch 202 of a controller 200. Also, the trigger 196, the interlock 198, or both, may be foot-operated, hand-operated, finger-operated, thumb-operated or the like in order to insure strictly safe activation of the driver 14.
The switch 202 may operate a solenoid 204 to open and close a valve 206 as illustrated in FIG. 16. This embodiment can be used with most working fluids. However a power supply 16 providing a gas as a working fluid may preferably be regulated at one or more locations.
Alternatively, a proportional controller 208 may be provided to limit the working fluid (such as oil 167) passing from the power supply 16 to the motor 70. The proportional controller 208 may be manual, electrical, electronic, or microprocessor based. The proportional controller 208 sends a signal to an actuator 210. The actuator 210, in turn, powers movement of a proportional valve 212. The proportional valve 212, alone or in duplicate, provides a supply of oil 167 to the motor 70, the actuator 115, or both. The proportional valve 212 receives oil 167 from an inlet line 214 at high pressure. The amount of oil 167 passed by the proportional valve 212 to the motor 70 and actuator 115 is conducted out the outlet line 216. Any oil 167 bypassed by the proportional valve 212 goes to a dump line 218.
In general, a controller 200 may include a switch, valve, lever, solenoid, other device, or combination for activating a movable member of the apparatus 10. A controller 200 may be manual or automatic, and may operate on a fixed routine or may include a programmably controlled microprocessor or other electronic control.
In general, an actuator (such as actuator 210) is contemplated to be an apparatus that moves an object in a direction by applying force in that direction. Hydraulic cylinders, linear motors, ball screws, and other devices that can be attached to a source of power to translate an object under load are suitable actuators. Actuators may be provided with a control suitable for activating an actuator.
A regulator 220 may be provided to limit pressure to the motor 70 or actuator 115 in a pneumatic system. Also, the dump line 218 may simply pass air to the atmosphere.
For a hydraulic type of power supply 16, a drive motor 22 may drive a pump 224 that both receives from and discharges to a sump 226. The dump line 218 in such an embodiment, may dump oil to the sump 226. A power supply 16 and controller 200 may also be configured to provide a regulated, pressurized supply of oil 167 directly to the proportional valve 212. In such an embodiment, the dump line may not be necessary. In a single-acting hydraulic actuator 115, the valve 206 or valve 208 may be configured to receive back oil 167 from the actuator 115, passing the oil 167 on to the dump line 218 and the sump 226.
Operation
In operation, the traveler 10 is moved toward an end of a tube 11 to be pulled. The clearance 66 may be set, upon completion of the previous, complete cycle. The clearance may be set to form a nip 64 that can receive the tube 11 without interference. The operator grasps one or more of the handles 194 and moves the frame 12 toward the end of the tube 11 until the tube 11 is positioned between the idler 80 and the wheel 50 of the driver 14. The operator activates the switch 202 by holding the interlock 198 and pulling the trigger 196. The switch 202 preferably signals proportionately to its movement as a part of the proportional controller 208.
The proportional controller commands the actuator 210 which moves the proportional valve 212 open in response. Oil 167 is passed at a controlled flow rate to the outlet line 216. The outlet line 216 feeds the oil 167 to the extension line 174A on the actuator 115 and the inlet line 72 on the motor 70.
The ram 162 extends, forcing the idler 80 on the carriage 110 against the side of the tube 11. The shaft 60 connected to the motor 70 begins rotating the wheel 50. The tube 11 is clamped between the wheel 50 and the idler 80. The tube 11 collapses laterally under the force of the actuator 115, and moves longitudinally through the frame 12 between the wheel 50 and the idler 80. The guard 24 deflects the crushed, exiting tube 11 away from operators and equipment.
The operator may adjust the position of the trigger 196 to change the speed of the motor 70. The actuator 115 may be exposed to substantially the same pressure as the motor 70, and may increase the gripping force of the idler 80 if pressure rises in the oil 167.
Upon release of the trigger 196, the same trigger 196 or another may activate the proportional valve 212 to retract the ram 162, moving the idler 80 to an open position away from the wheel 50 of the driver 14. The nip 64 is ready to receive another tube 11.
The wheel 50 may operate to draw a tube 11 into the nip 64, even when the idler 80 is in a "closed" position close to the wheel 50. This is not a preferred embodiment unless the tube 11 are not to be completely crushed, or the optional unidirectional clutch 100 is connected to a toothed idler 80.
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. | A tube puller, also called a traveler, removes tubes from the tube sheet of a heat exchanger for replacement. The tubes must first be broken free from the tube sheet and moved several inches by another device not associated with the traveler. The traveler includes a frame mounting a hydraulic motor. Inside the frame, a single driver mounted on the shaft of the motor is a wheel having a toothed circumference. The teeth of the driver engage one side of the tube to be removed. An unpowered idler is positioned on the opposite side of the tube from the driver. An actuator may move the idler selectively toward and away from the driver for altering the nip between the driver and idler to initially receive the tube. The actuator then presses the idler against the opposite side of the tube, holding the tube against the driver, but has no power to advance the tube longitudinally. Together, the idler and driver apply lateral forces that tend to deform the tube and may crush the tube completely as it is pulled. The idler may be equipped with a unidirectional clutch to prevent backward rotation, particularly during initial engagement of the tube by the driver and idler. | 8 |
This is a continuation of application Ser. No. 47,804, filed June 11, 1979 now abandoned.
BACKGROUND OF THE INVENTION
The present invention relates to bi-directional overrunning clutches for vehicles and more particularly to such a bi-directional overrunning clutch used in a front hub portion of a four wheel drive vehicle.
In a two wheel drive running condition of a four wheel drive vehicle, a wheel not driven, for example the front wheel, is driven from the road surface by contact thereof with the road surface. In this condition, since the driving force or rotation of the wheel is also transmitted to various mechanisms ancillary to the front wheel, i.e. mechanisms employed for a four wheel running mode, the running efficiency is decreased by the resistance of bearings and of oil. In order to improve such efficiency, means need be provided for limiting the driving force received from the road surface to the wheel and preventing transmission thereof to such other mechanisms.
It is therefore an object of the present invention to provide a bi-directional overrunning clutch which in a two wheel running condition can limit the driving force which is received by a non-driven wheel from the road surface to that wheel only.
It is a further object of the present invention to provide a bi-directional overrunning clutch in a four wheel drive condition can effectively transmit the driving force of the drive shaft to the drive wheel.
It is another object of the present invention to provide a bi-directional overrunning clutch for a four wheel drive which can offer an extremely high running efficiency.
BRIEF DESCRIPTION OF THE INVENTION
In accordance with the present invention, a bi-directional overrunning clutch comprises a drive shaft for transmitting a rotational driving force, a drive clutch member which is rotated by rotational motion of the drive shaft, a driven clutch member in engagement with the drive clutch member to receive rotational motion thereof and movable axially to transmit such rotational motion to a hub, and a brake member to impart a desired braking force to axial movement of the driven clutch member.
BRIEF DESCRIPTION OF THE DRAWINGS
The aforementioned and other objects and features of the present invention shall be described hereinafter in detail with reference to preferred embodiments thereof shown in the accompanying drawings, wherein:
FIG. 1 is a cross sectional view illustrating a preferred embodiment of the present invention;
FIG. 2 is a cross sectional view taken along the line II--II in FIG. 1; and
FIG. 3 is a cross sectional view taken along the line III--III in FIG. 1.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 is an explanatory view of the construction of a clutch in accordance with the present invention, and showing a drive shaft aligned in an axial direction. Referring to FIG. 1, the reference numeral 1 designates the drive shaft, and 11 is a drive clutch member. The mode of operation of the drive shaft is selectable between force transmitting rotation and a stationary state that does not transmit force. The drive clutch member 11 is secured to the drive shaft 1 through a snap ring 17, the clutch member thus being assembled with the drive shaft 1 to become integral therewith. The numeral 2 designates a hub, 12 a housing, and 13 a cover, which are assembled together by means of a bolt 14. An inner peripheral surface 12a of the housing has a conical shape so as to enable frictional engagement between the inner peripheral surface 12a and a driven clutch member 10. The driven clutch member 10 is provided to transmit power of the drive clutch member 11 to the housing 12 (hub 2), and is provided with a connection between the housing 12 and the drive clutch member 11. That is, an outer peripheral surface 10c of the driven clutch member 10 has a conical shape to allow for frictional engagement with the inner peripheral surface 12a of the housing 12. On the other hand, the connection between the driven clutch member and the drive clutch member 11 also includes a ball-cam clutch and a conical-cam clutch. The ball-cam clutch is provided in that the driven clutch member 10 has formed therein a recess with a conical configuration to form a a cut portion 10a, the drive clutch member 11 has a cylindrical flange portion facing an axial end of driven clutch member 10, with an opening in such flange portion facing the cut portion 10a, and a ball 18 is positioned in such opening and is biased into contact with cut portion 10a by means of a belleville spring 15 supported in drive clutch member 11 by a snap ring 16. The conical-cam clutch shape is formed in that a cam portion 11a having a substantially conical configuration protrudes axially upwardly from the flange portion of the drive clutch member 11, and a substantially V-shaped groove 10b is formed by cutting in the end face of the driven clutch member 10 to receive cam portion 11a. As shown in FIG. 2, the conical angle α of cut portion 10a is greater than the conical angle β of the cam portion 11a and the V-shaped groove 10b, as shown in FIG. 3, taken in directions circumferentially of driven clutch member 10. A brake indicated at 4 is supported on a brake holder 6 secured to the driven clutch member 10 and is biased to a fixing system 3 by means of a ring-like spring 5. A belleville spring indicated at 8 is partly supported by means of a snap ring 7 mounted on the drive clutch member 11 to bias the driven clutch member 10 axially towards the flange portion of the drive clutch member 11. The reference numeral 20 designates a slide bearing, and 19 and 21 designate washers.
The operation of the clutch construction as mentioned above will be described hereinafter.
When the drive shaft 1 is at a standstill, the driven clutch member 10 is moved axially toward the drive clutch member 11 by the belleville spring 8, i.e. to an inoperative position. This releases a connection between the outer peripheral surface 10c of the driven clutch member 10 and the inner peripheral surface 12a of the housing 12 to provide no power transmission. That is, even if the hub 2 is rotated, the housing 12 secured to the hub 2 and the cover 13 merely rotate, and a great load is not imposed on the hub 2. Next, when the drive shaft 1 commences its rotation, the drive clutch member 11 also rotates. Since the driven clutch member 10 is biased towards the drive clutch member 11 by the belleville spring 8 and is thus in a connected state due to the connection of the ball-cam clutch power is transmitted to the driven clutch member 10. The the the driven clutch members 10 thus commences rotation against the resistance of the brake 4. Rotation of the driven clutch member 10 facilitates movement of the driven clutch member 10 axially of drive shaft 1, to the left as shown in FIG. 1, i.e. to an operative position, by action of the ball 18 and cut portion 10a. This axial movement results in frictional connection between the outer peripheral surface 10c of the driven clutch member 10 and the inner peripheral surface 12a of the housing 12 so that rotation of the driven clutch member 10 is transmitted to the hub 2. When the torque of the drive shaft 1 assumes a magnitude above a certain value, the ball 18 is urged to the right as shown in FIG. 1 and moves against the force of the belleville spring 15. At such time, the connection of the conical cam clutch performs the function of transmitting power by urging driven clutch member 10 leftwardly as shown in FIG. 1.
When the power of the drive shaft 1 is cut off, rotation of the driven clutch member 10 is immediately slowed down by the action of the brake 4 of the driven clutch member 10, and the rightward biasing force of the belleville spring 8 acts on the driven clutch member 10 to reduce the connecting force between the driven clutch member 10 and the housing 12, thus relieving the load on the hub 2.
In other words, first and second engagement structures are provided between drive clutch member 11 and driven clutch member 10 for transmitting rotational movement of drive clutch member 11 to driven clutch member 10 and for, upon rotation of drive clutch member 11, moving driven clutch member 10 axially to an operative position against the force of spring 8. The first engagement device is particularly shown in FIG. 2 and includes a surface of cut portion 10a which is inclined circumferentially of driven clutch member 10, and a surface of ball 18 which is urged against the surface of cut portion 10a by spring 15. The second engagement device is particularly shown in FIG. 3 and includes a surface of groove 10b which is inclined circumferentially of driven member 10 and an inclined surface of cam portion 11a which is inclined circumferentially of the drive clutch member 11. The angle of inclination of the surface of cut portion 10a is greater than the angle of inclination of the surfaces of groove 10b and cam portion 11a. Therefore, upon rotation of drive member 11, such rotation being transmitted via ball 18 to driven member 10 as the ball moves circumferentially along cut portion 10a, the axially directed force component of ball 18 acting against driven member 10 will be greater than the axially directed force component imparted by cam portion 11a against driven clutch member 10. As a result, the axial movement of driven clutch member 10 to the operative position in contact with hub 12 will first be due substantially the first engagement device of FIG. 2. Thereafter, when ball 18 is urged to the right to deflect spring 15, i.e. out of contact with the surface of cut portion 10a, the second engagement device of FIG. 3 will continue to urge the driven clutch member 10 axially to the operative position.
It should be appreciated from the foregoing description that the transmission of torque from the drive clutch member 11 to the driven clutch member 10 may be suitably transferred suquentially from the ball-cam clutch to the conical-cam clutch by selecting the angles α and β to be within desired ranges. However, if the ball 18 is selected to have a size so that physical properties as desired may be provided in view of the entire structure, only the ball-cam clutch will suffice without provision of the conical-cam clutch. In addition, if the brake resistance and cam angle are selected suitably, only the conical-cam clutch will suffice without provision of the ball-cam clutch. | A bi-directional overrunning clutch comprises a drive shaft for transmitting a rotational driving force, a drive clutch member which is rotated with the drive shaft, a driven clutch member in engagement with the drive clutch to receive rotational motion thereof and movable axially to transmit the rotational motion to a hub, and a brake member to impart a desired braking force to rotational movement of the driven clutch member. In a two wheel running mode, the driven clutch member is disengaged from the hub so that the driving force, which is received by a non-driven wheel from the road surface, is limited to the wheel only. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Priority is claimed to U.S. Provisional Applications No. 60/410,360, filed Sep. 13, 2002 and No. 60/443,160, filed Jan. 28, 2003 and which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] The invention relates to composite materials that provide for removable and reuseable mechanical fasteners and labels, methods of manufacture, products and uses therefore.
[0003] Hook and loop type fasteners are widely available and have a myriad of applications. A variety of devices have been developed to accomplish the task of labeling and/or bundling of materials including the securing, bundling and labeling of wires and cables. Many of these devices use hook and loop touch fastener material.
[0004] Certain of these labeling and bundling devices rely upon positioning the hook and loop material in a specific manner so that a wrapping process is necessary to accomplish the bundling task. In an example of one such wrapping device currently marketed under the trademark ONE-WRAP® by Velcro USA Inc. and as taught by Leach et al. in U.S. Pat. No. 6,551,539, a hook material is disposed on the top surface of a fastener strap while the loop material is disposed on the bottom surface. Similar bundling devices that have loop and hook elements on opposite sides of a substrate and thus require wrapping to engage the hook and loop elements are taught in U.S. Pat. No. 4,706,914 (Ground); U.S. Pat. No. 5,048,158 (Koerner); and U.S. Pat. No. 5,745,958 (Kaldor). Another type of hook and loop bundling device utilizes hook and loop elements on opposite sides of a strap material in such a way that a cinch type strap is provided. In one such cinch strap, as taught by Sastre at al in U.S. Pat. No. 6,044,525, one end of a strap has a slit through which the other end can be fed and looped back on the strap to mate the hook and loop elements. This type of device requires a significant amount of manipulation in order to secure the device around an object.
[0005] After the wrapping is complete with closure materials having hook elements on one side and loop elements on the other side, the exposed surface of the bundling device is either the hook or loop material of an indeterminate perimeter that is ill suited for displaying printed or written information. Similarly, there is no provision for a surface that accommodates printed or written information in the bundling devices having bands of hook or loop material covering both strap surfaces as taught by Hahn in U.S. Pat. No. 5,142,743.
[0006] One solution to the need for both bundling and labeling was disclosed by Tarrant in U.S. Pat. No. 4,656,767. Tarrant disclosed an identifying tag for cables in which a hook fastener panel and a separate loop type fastener panel are mounted on the same side of a plastic strip material in a spaced apart configuration. A clear pocket is mounted on an outer surface of the strip and identifying indicia may be inserted in the clear pocket to provide labeling of the cables. However, in such designs, the hook and loop material may become displaced with the shear pressure of tight bundling. Furthermore, the Tarrant cable tag does not provide for an outer surface that is directly writable.
[0007] A further cable management system having provision for branding and having separate hook and loop elements mounted on the same side of a backing material in a spaced apart configuration is disclosed by Behar in U.S. patent application Ser. No. 09/738,159, published as U.S. 2002/0073516 A1. In the Behar cable clip apparatus, the hook and loop elements are sewn or glued to an EVA foam backing and an outer piece of fabric. Neither the Tarrant nor Behar systems provide a hook and loop substrate that is resistant to shearing and provides a writable surface for identifying the object around which it is attached.
[0008] The need to organize and bundle various lengths of wire, cables and similar objects, has been long recognized. The purpose could be to save space for storage or to secure excess lengths of cable that are attached to a product in use, where the excess cable is cumbersome or hazardous. However, there is a further need for the bundling device that can be readily manufactured, is flexible, reusable and can be quickly applied with one hand. There is a further need to provide for removable and reusable labeling of objects, including bundled objects, on a surface that readily accepts writing and printing mediums. Such a device is also needed to provide reusable labeling devices that can be quickly applied and removed for such uses as identification of keys, bridles, collars and many other objects depending on the configuration of the device.
BRIEF SUMMARY OF THE INVENTION
[0009] The present invention provides a labeling and/or bundling device that can be readily manufactured, is flexible, reusable and can be quickly applied with one hand. The invention further provides for removable and reusable labeling of objects, including bundled objects, on a surface that readily accepts writing and printing mediums. In one embodiment of the invention a labeling fastener device is provided that includes a flexible fastener substrate having a plurality of loop and hook elements, wherein both loop and hook elements are permanently embedded onto and extend outwardly from a single side of the substrate, and writable film adhered to and substantially covering a second side of the fastener substrate, wherein the fastener substrate and film together form a writable fastener device that may be closed by a single folding motion.
[0010] In another embodiment of the invention, the writable surface is composed primarily of a polypropylene or polyethylene film and is adapted to receive an image applied by ink-jet printing, laser printing, silk-screen printing or embroidery. If needed the film is treated to better receive and retain such images. The writable surface may be written upon with a writing instrument such as ball-point, felt, or gel pens.
[0011] In yet another embodiment of the invention, the fastener device is dimensioned for fastening around and providing a labeling surface to one or more objects such as wires, cables, conduits, tubing, pipes, lines, ring closures and the like and combinations thereof.
[0012] In still another embodiment of the fastener device, at least a portion of the writable surface further includes a transparent pocket for insertion of a label, wherein the label is visible through the pocket and is retained securely in the transparent pocket.
[0013] In another embodiment, the writable surface has a thickness of between about 5 and about 10 mil. In a preferred embodiment, the writable surface consists primarily of a polypropylene film having a thickness of about 6 to 7 mil.
[0014] The invention also provides a method for producing a flexible fastener having a writable surface by providing a loop and hook fastener substrate comprising loop and hook elements that are permanently embedded onto and extend outwardly from a common side of the substrate. A writable film comprising polypropylene or polyethylene is adhered to the loop and hook fastener substrate thereby producing a flexible laminate sheet having the loop and hook elements substantially covering a first side of the laminate sheet and the writable film substantially covering a second side of the laminate sheet. The flexible laminate sheet can be cut into a plurality of flexible fasteners, wherein the flexible fasteners are adapted for mating of the loop and hook elements by a single pinching motion thereby providing a flexible fastener having a writable labeling surface.
[0015] The loop elements and hook elements may be intermixed on the loop and hook substrate or may be disposed in alternating bands on the loop and hook fastener substrate. In one embodiment, the substrate is manufactured by first generating a soft woven sheet of loop material followed by permanently adhering hook elements over a portion of the loop material thereby generating a single substrate comprising both loop and hook elements.
[0016] In still another embodiment, the hook elements are disposed over the substrate such that approximately one-half of a longitudinal dimension of the substrate is covered with loop elements and approximately one-half of a longitudinal dimension of the substrate is covered with hook elements. Folding of the substrate in half along its lateral dimension fully engages the hook elements against the loop elements. In another embodiment, the fastener substrate is provided in rolls having a desired width of the final fastener. In certain embodiments the width of the fastener substrate is approximately about 4 to about 8 inches in width and has hook elements covering approximately one fourth to one-half of the width. Thus, for a fastener substrate having a width of 4 inches, the hook elements may be disposed over approximately 1-2 inches of the width of the 4 inch roll. In one embodiment the hook elements cover one-half of the total width of a fastener substrate having a total width of about 4, 5, 6, 7 or 8 inches. In another embodiment wide fasteners having a total width of up to about 13 inches and thus a folded together width of approximately 6½ inches is provided.
[0017] In yet another embodiment of the invention, printed images are applied to the writable film prior to adhering to the hook and loop substrate. The images may optionally be printed using a high volume roll-fed printing press, such as for example a flexographic printing press.
[0018] In one embodiment a printable fastener substrate is provided including a flexible laminate sheet having a light weight loop and hook fastener substrate substantially covering a first side of the laminate sheet and a 5 to 10 mil polypropylene film substantially covering a second side of the laminate sheet, wherein the loop and hook fastener substrate comprises hook and loop elements that are permanently embedded onto and extend outwardly from the substrate and are exposed on the first side of the laminate sheet, and wherein the polypropylene film is adapted for receiving printed images. The substrate can be supplied for custom consumer printing either directly on the fastener substrate or using transfer film. The substrate is optionally provided with perforations for separation of individual fasteners after printing.
DESCRIPTION THE DRAWINGS
[0019] [0019]FIG. 1 is a diagram of the hook and loop fastener side of one embodiment of the invention.
[0020] [0020]FIG. 2 depicts a writable surface side of one embodiment of the invention.
[0021] [0021]FIG. 3 diagrammatically depicts a fastener substrate to which a removable label can be placed on top of the writable surface or can be inserted in a transparent sleeve on the writable surface.
[0022] [0022]FIG. 4 diagrammatically depicts certain steps in the manufacture of a bundling and labeling device according to one embodiment of the invention.
[0023] [0023]FIG. 5 depicts the bundling and labeling device being used to bundle cables in accordance with one embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0024] In one aspect of the present invention, a flexible bundling device is provided having a unique orientation of hook and loop material on a single inside surface of a substrate so that no wrapping process is required to secure wires or cables. This orientation frequently proves to be an easier process than that of the wrapping oriented bundling devices. In addition, provision of a substrate having both hook and loop material integrally bonded provides for high resistance to shear forces when bundling device is tightly wrapped such as when a large number of cables are secured together. Further, due to this orientation of the hook and loop material where the hook and loop elements are formed on the same substrate and cannot slide away from each other when mounted on a further substrate, the device provides additional functionality for the outside surface of the substrate, so that it can be used to display information that has been either preprinted on the device, preprinted on a label capable of attaching to the substrate, or hand-written onto the substrate itself. Both the outside surface characteristics and the label insertion option, provide the capability for a high quality rendering of printed material. This will be suitable for corporate advertising, information that is uniquely provided by the individual consumer, or a combination of both. The information can be text or graphic images or a combination of both.
[0025] Where used in a bundling application, information provided by the consumer would typically be of a labeling nature, so as to distinguish the cable, wires, lines or conduits in the bundle from other bundled objects. This is particularly useful for applications where multiple devices with power cables are plugged into an AC power strip, where without labeling it is difficult to uniquely identify the equipment associated with a particular cable.
[0026] In one embodiment of the invention, the primary function of the fastener is labeling rather than bundling. For example, removable labels according to one embodiment of the present invention are dimensioned for attaching and providing a labeling surface for keys attached to rings such as at a car dealership or for valet parking. The labeling embodiment is useful for other indications where removable identification is required such as for example for placement on animal collars, halters etc. in veterinary and kennel operations. By using certain suitable markers, identifying indicia placed on the label can be removed and the label reused. As a consequence using a printable film applied to the fastener, advertising and promotional materials are readily and inexpensively produced. Where light weight hook and loop material is desired, the writable surface not only provides a printable surface for advertising but provides the important property of conferring sufficient rigidity for the label to be applied with a single pinching motion.
[0027] Hook and loop fasteners consist in simplest form of two mating elements. The loop elements typically comprise a mat of small soft loops. The loop elements can be napped or unnapped. Napped loop material consists of woven loops, typically nylon, that are “randomly disoriented” in a separate operation after weaving. Unnapped loop material is a woven loop material that has not been napped.
[0028] The hook elements are small flexible hooks that may be single crooks, double hooks, palm shaped hooks or mushroom shaped projections that engage loops of the loop elements when the hook and loop elements are pressed together resulting in closure of a fastener having opposing hook and loop elements. A closure of hook and loop elements is opened by peeling the hook and loop elements apart. Opening and closing of the hook and loop elements is termed a “cycle.” Typically, heavy duty hooks have lower cycle life than lightweight hooks.
[0029] In one embodiment, the hook and loop elements are formed on a common substrate material and both the hook and loop elements face the same direction. Engagement of the hook and loop elements is accomplished by folding. With this configuration, it is impossible for the hook and loop segments to shear in opposing directions, which is direction of shear pressure that occurs while bundling a cable for example. The common substrate material can be accomplished by either intermixing the hooks and loops, forming alternating rows of hook and loop on the same surface, or forming a portion of the common substrate with loop elements and another portion with hook elements. An example of an intermixed hook and loop configuration is presented in U.S. Pat. No. 5,515,583. An example of an alternating row configuration is the VELCRO-OMNI-TAPE fastener.
[0030] In a preferred embodiment, the hook and loop substrate is formed by a process in which a strip, sheet or mat of loop material is first formed. In a following step, hook elements are fused directly to the loop material across the entire back of the hook material but in such a way that portions of the loop material remain exposed. Thus, the resulting laminate substrate has both hook and loop elements disposed on the same side of the same substrate, the hook elements covering and thus abolished underlying loop elements. Such a method of manufacture is taught by Krantz et al. in U.S. patent application Ser. No. 09/808,395, published as U.S. 2002/0022108 AI, assigned to Velcro Industries.
[0031] Referring to FIGS. 1 - 3 , various embodiments of the invention are depicted. FIG. 1 depicts the fastener side of a bundling or labeling device. Hooks 10 and loops 12 are attached to the inside surface 15 of fastener substrate 16 . The hook and loop material can be attached to the substrate by a variety of common bonding techniques, it can be stitched to the substrate, or the creation of the substrate with hook and loop material can be an integrated manufacturing process. In FIG. 1, area 14 is left open with no hook or loop and the substrate surface is exposed. Open area 14 may allow the device to more easily bend around the cable and wires to be bundled but is optional. In other embodiments it is preferred that the hook and loop areas abut one another and area 14 may be virtually absent in embodiments where the hook regions abut loop regions. The dimensions of the device are variable and will be offered in a range wide enough to address a variety of consumer applications. Typical dimensions for use in relatively small bundles of one or more wires, cables, conduits, tubing, pipes, lines, and combinations thereof would be a width of approximately ½ to one inch and length of approximately 4 to 8 inches.
[0032] [0032]FIG. 2 depicts outside surface 18 , which is capable of containing information 20 that has been pre-printed or has been written onto the substrate by the user of the device. As shown in FIG. 2, the device can optionally be provided with a notch or tab 19 to facilitate separation of the hook and loop elements.
[0033] [0033]FIG. 3 depicts an alternate embodiment in which a removable label 22 is placed on the back of the writable surface 18 . Alternatively, the fastener can be provided with a transparent sleeve 24 affixed to the writable surface 18 of fastener substrate 16 . In this embodiment, a label can be inserted into the transparent sleeve 24 . FIG. 5 depicts a typical view of one embodiment of the device securely bundling cables and providing a printed or writable surface for identifying the cable bundle.
EXAMPLE 1
[0034] In developing the present invention cable ties were produced utilizing a vinyl writable surface sheet that provided a good combination of flexibility, durability and printability. The hook and loop material was attached in two sections. One section was for the hook and a separate section for the loop. The middle gap between the hook and loop sections was about ⅛th of an inch. The hook and loop material came from Velcro Corporation and was pre-coated with a rubber based pressure sensitive material.
[0035] However, after about two months of use, the bond of the adhesive became gooey with the hook and loop sections sliding away from each other in a lateral direction. This created a larger gap in the middle, up to ½ of an inch or more, with the hook and loop sections exposed on the ends and extending beyond the writable surface. The problem was magnified when the tie was in use with large cables and experiencing a significant shear stress against the adhesive bond. Heat (such as experienced in an automobile) also weakened the bond. It was determined that the inexpensive binder grade vinyl contained a plasticizer that evaporates over time. This attribute was responsible for the change in the strength of the adhesive bond.
EXAMPLE 2
[0036] In order to avoid the problem of separation of the fastener portions from the writable surface, a vinyl with a higher quality plasticizer or an extruded vinyl (both higher cost) or a polymeric material without a plasticizer could be employed for the writable surface sheet or film. Polymeric films such as those containing primarily polyolefin, polypropylene or polyethylene that do not contain plasticizers were tested. The polyolefin film tested was produced in layers which separated. Single layer material is preferred to avoid this result. Although polyethylene is not as readily commercially available, it could be alternatively employed.
[0037] Polymeric film containing polypropylene was found to have the advantages of general availability, strength with retained flexibility, and the ability to accept printing from printing presses such as flexographic high volume printing presses used by many printers. In one embodiment for use in cable ties and labels for affixing to rings, the polypropylene is about 5 mil to about 10 mil in thickness.
[0038] In one embodiment, a writable polymeric film at least primarily composed of polypropylene having an approximately 6.5 mil thickness is employed. One suitable polypropylene sheet or film material is commercially available under the trade name ALPHAMAX from FLEXcon Corporation, 1 FLEXcon Industrial Park, Spencer, Mass., USA 01562-2642. ALPHAMAX EXPP 650 F is a flexible polypropylene film having a 6.5 mil thickness that is top-coated with a waterbased TC-106 coating to make the film printable. This material is compatible with acrylic adhesives such as the V-606 adhesive from FLEXcon. The 6.5 mil thickness was found to have a desirable combination of flexibility and strength for use such applications as cable ties. In one embodiment, the polypropylene film is ordered with the desired adhesive and size.
[0039] Polypropylene film was evaluated together with various acrylic adhesives. For commercial purposes the combined attributes of strength and cost effectiveness are relevant. Sheet or film material, such as 5 to 10 mil polypropylene, may be ordered with or without pressure sensitive adhesive on the back.
[0040] Where the sheet material is supplied without adhesive, a pressure sensitive adhesive can alternatively be supplied in the form of a separate transfer tape and applied as a secondary process. Polypropylene with the pressure sensitive adhesive already applied by the factory that produces the polypropylene may provide cost advantages.
[0041] A suitable adhesive should provide a strong and durable bond to the writable surface film. Particularly where the hook and elements are not formed on the same substrate, the adhesive must provide shear resistance. One suitable adhesive is the FLEXcon 606 adhesive and is preferably applied to the polypropylene film in a thickness of about 1.9 to 2.1 mil.
[0042] When hook and loop material is bonded to the sheet film that lacks volatile plasticizers, such as for example polypropylene, it has stronger resistance to shear due to the absence of plasticizer. Hook and loop material from various manufacturers is available in various configurations of the hooks and loop themselves as will as in different overall heights, and with different depths to the actual end of the hook. These characteristics influence the strength of attachment between the hooks and loops when engaged together.
[0043] In one embodiment, the hook and loop are on a common substrate material and both the hook and loop face the same direction. Engagement of the hook and loop elements is accomplished by folding. With this configuration, it is impossible for the hook and loop segments to shear in opposing directions, which is the direction of shear pressure that occurs while bundling a cable for example.
[0044] Various hook/loop configurations were tested. In one embodiment, a desirable combination of hook elements and loop elements for use in cable ties was selected for manufacture by Velcro Corporation on a common substrate that is 4 inches wide. Such material can be custom manufactured in various widths. In one embodiment, the preferred loop is a soft, lightweight loop material, such as is commercially available from VELCRO USA, INC. of Manchester, N.H. under the designation style LP 3905.
[0045] Of available choices, a VELCRO HTH 830 (polypropylene) hook was selected for combination with a 3905 knit nylon loop. The VELCRO 3905 loop is a low profile unnapped nylon warp knit. The VELCRO 830 hook is a polypropylene member of the High Technology Hook (HTH) 29 profile series and is characterized by 1700 hooks per square inch and a hook height of 0.5 mm. This hook was selected for superior engagement with low profile loops such as the VELCRO 3905 loop. This combination of hooks and loops material is characterized by a moderate peel strength between the hook/loop, but the materials were also compatible with a technology referred to by Velcro as FLEXZONE technology that forms hooks directly onto the loop fabric such that both hooks and loops are integral to a common substrate. Where the hooks and loops are formed on a common surface, they are not susceptible to movement against the writable film surface in response to the pressure of tight bundling or as a result of repeated cycling.
[0046] Velcro manufactures this material by a two step process as depicted in part in FIG. 4. In the first step, a common substrate 34 comprising nylon loops 33 is produced in various widths on a roll X yards long. A secondary process 32 as disclosed in Krantz et al. U.S. patent application Ser. No. 09/808,395, published as U.S. 2002/0022108 AI and assigned to Velcro Industries, forms a myriad of hooks 30 , on top of the loops 33 in a hot injection molding process resulting in final hook and loop fastener substrate 40 . However, such integral hook and loop material could alternatively be generated in several ways known to those of skill in the art including by fusing a strip of hook material to the loop substrate or weaving hook material with or through the loop fabric followed cutting or topping of the hook elements.
[0047] A number of configurations are possible. For example the loop material might be of a final desired width with hook elements disposed in a single longitudinal strip that may be approximately one fourth to one half of the total width. Alternatively, a wide mat of loops may serve as the base for alternating bands of overlaid and fused hook material that is subsequently cut to final desired dimensions. For example, to make 4 inch wide fasteners, the loop material could be 4 inches wide with a single 2 inch wide band of hooks, 8 inches wide with two 2 inch wide bands of hooks that is later cut in half longitudinally, twelve inches wide with three 2 inch wide bands of hooks that is later cut in three strips and so on. Fasteners of several final widths may be manufactured in a single run where, for example, 12 inch wide loop material has a two inch band of hooks laid down from 2 to 4 inches from one side and a second approximately 4 inch wide band laid down at approximately 8 inches from the same side. The resulting product is cut at 4 inches resulting in a roll of 4 inch fastener material and a roll of approximately 8 inch wide fastener material. Alternatively, hook and loop fastener substrates of virtually any width that can be manufactured on a single substrate can be used for the production of fasteners of this final width according to the invention. For example, hook and loop substrate material having widths of about 13 inches can be used to produce fasteners having a folded in half dimension of 6½ inches wide.
[0048] In the example depicted in FIG. 4, fastener substrate 40 is an X inch wide material hundreds of yards long, with a band of hook 38 and a band of loops 36 running in a longitudinal dimension. Fastener substrate 40 is preferably generated by an in situ hot injection molding process that forms hooks 30 directly on loop substrate 34 . No adhesive is required to adhere the hook elements because they are formed in situ on the loop fabric. As depicted in FIG. 4, when using light weight loop material 34 , the loop fabric is soft and flexible while in situ formation of hooks, such hooks 30 on loop substrate 34 , results in a fastener substrate 40 that has a relatively stiff hook portion 38 and a relatively soft and floppy loop portion 36 .
[0049] Referring again to FIG. 4, the following process may be employed to fashion a device in accordance with the invention. A common hook and loop fastener substrate 40 is provided in a custom configuration, X yards long. Polypropylene film 42 is supplied in rolls X yards long having a dimension essentially the same as that of hook-loop fastener substrate 40 . In one embodiment, high volume roll-fed equipment prints images and text on polypropylene film 42 . A pressure sensitive adhesive 44 is applied to the film 42 , typically before printing. The polypropylene 42 is bonded to the hook and loop substrate 40 , resulting in an essentially permanent laminate having a hook and loop fastener surface 52 and a writable polypropylene surface 50 wherein the application of the polypropylene film 42 confers a stiffening of the loop portion 36 . As a consequence of the stiffening provided by the film, the fastener can be formed of thin flexible low profile hook and loop material and yet can be closed by a single pinching motion. The rolls of laminate are cut at points 48 to the desired width dimension, preferably in a high speed automated process. The final product 46 is a removable device that can be attached to an object and provides a labeling function and/or a bundling function.
[0050] This configuration was tested under the stress of large diameter cables and atmospheric temperatures over 90° F. for prolonged periods. Where the hook and loop was provided in the same substrate, the material was not observed to shear against the polypropylene.
EXAMPLE 3
[0051] In another embodiment, a portion of the polypropylene film surface is covered with a transparent pocket as depicted in FIG. 3 that allows insertion of a printed label, wherein the printing on the label is visible and the label is retained securely between the transparent film and the surface of the substrate.
EXAMPLE 4
[0052] In yet another embodiment, a version of the product that is printable by the consumer is provided. In this embodiment, the writable fastener material is supplied in sheet or roll form that is compatible with home and small office printers, either ink-jet or laser, that are able to accommodate thick stock sheets or rolls. Common software applications are employed in the creation of designs to be printed on the sheet or roll or on transfer film that is then applied to the fastener material. In one embodiment, the sheet or roll has perforations that define a final size of the writable fastener. The final custom printed fasteners are either cut to desired size or are separated at perforations.
EXAMPLE 5
[0053] In still another embodiment of the invention, the primary function of the fastener is labeling rather than bundling. For example, removable labels according to this embodiment are dimensioned for attaching and providing a labeling surface for keys attached to rings such as at a car dealership or for valet parking. The labeling embodiment is useful for other indications where removable identification is required such as for example for placement on animal collars, halters etc in veterinary and kennel operations. By using certain suitable markers, identifying indicia placed on the label can be removed and the label reused. As a consequence of printable film applied to the fastener, advertising and promotional materials are readily and inexpensively produced. Where light weight hook and loop material is desired, the writable surface not only provides a printable surface for advertising but provides the important property of conferring sufficient rigidity for the label to be applied with a single pinching motion.
[0054] While the invention has been disclosed with respect to a limited number of embodiments, numerous modifications and variations will be appreciated by those skilled in the art. It is intended, therefore, that the following claims cover all such modifications and variations that may fall within the true sprit and scope of the invention. | A flexible device for labeling and/or bundling objects such as wires, cables, conduits, ring closures and the like, which includes a hook and loop fastener substrate adhered to a writable surface dimensions so that when the device is folded in half, the hook and loop material is engaged and accomplishes the labeling and/or bundling purpose. | 1 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to windows generally and, more particularly, but not by way of limitation, to a novel replacement window that is economically and rapidly installed and to a method of installing such a window.
2. Background Art
There is a major problem with replacing steel frame windows, particularly those in brick, block, and/or stone walls, in that the replacement usually involves having to do a certain amount of rebuilding of the window openings. This procedure is relatively expensive and also requires that the area in which the window is located be isolated for a fairly long period of time. The problem is especially serious in health care facilities where, typically, whole floors must be closed during window replacement because of the reconstruction activities. Also, most known replacement windows reduce the amount of glass area.
Accordingly, it is a principal object of the present invention to provide a replacement window for steel frame windows that can be quickly installed and a method of installing such a window.
It is a further object of the invention to provide such a window that is economically constructed.
It is an additional object of the invention to provide such window and method that do not require rebuilding of brick/block and/or stone walls in which the replacement windows are installed.
It is another object of the invention to provide such a replacement window which does not decrease the amount of glass area in the window.
Other objects of the present invention, as well as particular features, elements, and advantages thereof, will be elucidated in, or be apparent from, the following description and the accompanying drawing figures.
SUMMARY OF THE INVENTION
The present invention achieves the above objects, among others, by providing, in a preferred embodiment, a method of replacing an existing window of the type having an existing fixed metal frame mounted in an existing window opening, comprising: removing elements of said existing window, except said existing fixed metal frame, while leaving said existing fixed metal frame in place and without rebuilding said existing window opening; providing a replacement window having a glazed monolithic frame member; and attaching said monolithic frame member to said existing metal frame by inserting fasteners through said monolithic frame member directly into said existing fixed metal frame.
BRIEF DESCRIPTION OF THE DRAWING
Understanding of the present invention and the various aspects thereof will be facilitated by reference to the accompanying drawing figures, submitted for purposes of illustration only and not intended to define the scope of the invention, on which:
FIG. 1 is a fragmentary, cross-sectional, side elevational view taken along line "1--1" of FIG. 9.
FIG. 2 is a fragmentary, cross-sectional, side elevational view taken along line "2--2" of FIG. 9.
FIG. 3 is a fragmentary, cross-sectional, side elevational view taken along line "3--3" of FIG. 9.
FIG. 4 is a fragmentary, cross-sectional, side elevational view taken along line "4--4" of FIG. 9.
FIG. 5 is a fragmentary, cross-sectional, plan view taken along line "5--5" of FIG. 9.
FIG. 6 is a fragmentary, cross-sectional, plan view taken along line "6--6" of FIG. 9.
FIG. 7 is a fragmentary, cross-sectional, plan view taken along line "7--7" of FIG. 9.
FIG. 8 is a fragmentary, cross-sectional, plan view taken along line "8--8" of FIG. 9.
FIG. 9 is a front elevational view of a window constructed according to the present invention, installed in a masonry wall.
FIG. 10 is a fragmentary, cross-sectional, plan view of a conventionally constructed steel frame window having a fixed sash.
FIG. 11 is a fragmentary, cross-sectional, plan view of a conventionally constructed steel frame window having an operating sash.
FIG. 12 is a fragmentary, perspective view illustrating a method of forming spacers in situ, useful in the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Reference should now be made to the drawing figures, on which similar or identical elements are given consistent identifying numerals throughout the various figures thereof, and on which parenthetical references to figure numbers direct the reader to the view(s) on which the element(s) being described is (are) best seen, although the element(s) may be seen also on other views.
Reference first should be made to FIG. 10 which illustrates a conventional, fixed sash window, generally indicated by the reference numeral 20, set in a wall 22 which may be of brick, block, and/or stone construction. Window 20 includes a frame, generally indicated by the reference numeral 24, typically constructed of steel, fixedly mounted in wall 22 by conventional means (not shown). Frame 24 includes rear, intermediate, and front flange members 26, 28, and 30, respectively. A glass pane 40 is set in frame 24 against rear flange 26, with a compressible filler strip 42 disposed between the pane and the rear flange. A caulking material 44 disposed between intermediate flange 28 and the edge of the outer surface of pane 40 secures the pane in place in frame 24.
FIG. 11 illustrates another conventionally constructed metal frame window, generally indicated by the reference numeral 20', of the operating sash type. Here, pane 40' is set in a movable frame 50 which is hingedly attached to front flange 30' of window frame 24' by means of an operator 52.
FIG. 9 illustrates a replacement window, generally indicated by the reference numeral 100, constructed according to the present invention and installed in a masonry wall 102. It may be assumed that window 100 has replaced, for example, window 20 or 20' of FIGS. 10 and 11, respectively, as will be described in detail below. Window 100 is shown as having three sections 104, 106, and 108, window sections 104 and 108 being fixed and window section 106 being of the opening type; although, window 100 may be provided, if desired, as a single fixed window section, a single opening window section, or some other arrangement of window sections.
Reference should now be made to FIGS. 1, 5, and 6 for an understanding of the construction of window section 104. It will be understood that sections taken through window section 108, similar to FIGS. 5 and 6, will be identical thereto.
Window section 104 includes a frame, generally indicated by the reference numeral 120, extending around the top and sides of the window section. Frame 120 is preferably an aluminum extrusion. Frame 120 includes a rearwardly extending rear flange member 122, a forwardly extending front flange member 124, and a cross-wisely extending intermediate flange member 126 extending between and joining the rear and front flange members.
A double glass pane unit 140 is mounted in frame 120, with a strip of double-faced adhesive tape 142 disposed between the edge of the inner surface of the pane unit and intermediate flange member 126 and a strip of resilient material 144 disposed between the edge of the pane unit and front flange member 124. Pane unit 140 is secured in place by means of structural silicone material 146 and 148 placed against strip 144 and tape 142, respectively. A trim strip 150 covers the distal end of front flange member 124 to cover a groove not used in fixed sash.
Reference now should be made to FIGS. 7 and 8 for an understanding of the construction of window section 106. Here, a double glass pane unit 140', rather than being mounted in frame 120, is seated in a movable frame 160 in a manner similar to that described above with reference to the seating of double glass pane unit 140 in frame 24. Movable frame 160 is removably sealed to frame 24 by two weatherstrips 162 when the movable frame is in its closed position shown on FIGS. 7 and 8. An operator 164 is provided to cause movable frame 160 to move outwardly from frame 24 in a conventional manner.
Referring now to FIGS. 2 and 3, it will be seen that horizontal tubular frame members 170 are provided at the junction of window sections 104 and 106 and at the junction of window sections 106 and 108, the tubular frame members preferably being aluminum extrusions. Conventional four-arm hinges 172 are disposed between tubular frame members 170 and movable frame 160 to permit the movable frame to move outwardly from frame 120 (FIGS. 7 and 8) and thus open window section 106.
Referring to FIG. 4, it will be seen that frame 120 at the lower edge of window section 108 is attached to a sill unit, generally indicated by the reference numeral 180. Since the configuration of sill unit 180 may be varied greatly from installation to installation, no description of the components thereof will be given, except to note that sill unit 180 includes a horizontal flange member 182 extending horizontally from the rear thereof.
All the elements of replacement window 100 described above may be conveniently and economically assembled as shown in a shop remote from the location of installation of the window. This greatly minimizes the time that must be spent at the job site.
To install window 100 in wall 102 (FIG. 9), if the existing window is fixed sash 20 (FIG. 10), first the existing glass pane 40 (FIG. 10) is removed from frame 24, leaving the frame in place. If the existing installation is operating sash 20' (FIG. 11), movable frame 50 and operator 52 are removed from frame 24, again leaving the frame in place. Should there be any horizontal or vertical intermediate frame members (not shown), those would be cut out of frame 24. Also, any remnants of sealing or bedding materials would be cleaned from frame 24.
Next, window 100 as described above is placed against frame 24 (FIG. 5, for example) with intermediate flange member 126 of frame 120 abutting front flange member 30 of frame 24. Now, a plurality of self-drilling, self-tapping steel screws 190 are used to fasten rear flange member 122 of frame 120 to intermediate flange member 28 of frame 24 and to fasten horizontal flange member 182 (FIG. 4) to the intermediate flange member.
To finish the installation, a back rod 192 (FIG. 5, for example) is placed between wall 102 and front flange member 124, slightly inwardly from the distal end of the latter and a caulking material 193 placed in the cavity thus defined thereby. A similar sealing arrangement is provided at the front edge of sill unit 180. A compressible filler material 194 (FIG. 5, for example) is placed between the distal end of rear flange member 122 and rear flange member 26. Trim panels 196 (FIG. 5, for example) are snapped in place, as shown, to cover screws 190.
In mounting frame 120 to frame 24, it has been found desirable to be able to form, in situ, resilient spacers between rear flange member 122 of frame 120 and intermediate flange member 28 of frame 24. The method of doing so will be described with reference to FIG. 12. Here, two, generally vertically aligned, closely spaced, upper and lower holes 200 and 202, respectively, are drilled in rear flange member 122 and a screw 190 is inserted into lower hole 202 and started into intermediate flange member 28. Then, a resilient epoxy material 204 is injected into upper hole 200 and fills a portion of the space between flange members 28 and 122. Screw 190 is then tightened a desired amount to align window 100 (FIG. 9). When epoxy material 204 subsequently cures, it forms a resilient spacer of precisely the proper thickness between flange members 28 and 122.
It will be noted that the open glass area of window sections 104 and 108 (FIGS. 5 and 6) is as great as that of window 20 (FIG. 10) and that the open glass area of window section 106 (FIGS. 7 and 8) is nearly as great as that of window 20' (FIG. 11).
It will be understood that frame 120 may be modified as required to fit different configurations of frame 24; however, the basic method of the present invention will remain the same. That is, the removal of the glass pane(s) from an existing metal frame, while leaving the frame in place, and the direct attachment to the frame of a replacement window unit.
It will thus be seen that the objects set forth above, among those elucidated in, or made apparent from, the preceding description, are efficiently attained and, since certain changes may be made in the above construction without departing from the scope of the invention, it is intended that all matter contained in the above description or shown on the accompanying drawing figures shall be interpreted as illustrative only and not in a limiting sense.
It is also to be understood that the following claims are intended to cover all of the generic and specific features of the invention herein described and all statements of the scope of the invention which, as a matter of language, might be said to fall therebetween. | In a preferred embodiment, a method of replacing an existing window of the type having an existing fixed metal frame mounted in an existing window opening, the method including: removing elements of the existing window, except the existing fixed metal frame, while leaving the existing fixed metal frame in place and without rebuilding the existing window opening; providing a replacement window having a glazed monolithic frame member; and attaching the monolithic frame member to the existing metal frame by inserting fasteners through the monolithic frame member directly into the existing fixed metal frame. | 4 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The invention relates generally to the field of passivation of metal surfaces. More specifically, the invention relates to passivation of metal surfaces on conductors used in cardiac leads which shelter polymeric electrical insulation adjacent thereto from metal and metal ions in the lead.
[0003] 2. Description of the Prior Art
[0004] Medical devices and components thereof often comprise significant amounts of metal or metal alloys. While metals are typically selected based on their biocompatibility, it is often the case that structural demands on the device require that materials which are not entirely biocompatible or which are not entirely compatible with other components of the device, particularly non-metal components, are employed. One example of this is in the field of cardiac pacemakers, where electrically conductive leads extend from the pacemaker to the heart of the recipient and comprise metal conductors with electrical insulation along their length.
[0005] In cardiac pacemaker lead bodies, the metals used are chosen based on a number of factors. Among these is fatigue-resistance; cobalt is known to improve the fatigue-resistance to an acceptable degree. The insulating materials are also carefully chosen and flexible polymer compositions, for example, polyether-based polyurethane are commonly used. One problem which can arise from this combination, though, is that the polymer insulation rapidly degrades if it is in direct contact with metal, particularly cobalt, and/or reactive species produced in the lead body. This catalytic degradation of the polymer insulation can lead to device failure or injury to the patient, both of which should be avoided whenever possible.
[0006] The degradation phenomenon is referred to as metal ion-induced oxidation or MIO. Some solutions to the problem of improving compatibility between metal-containing devices and insulating layers, i.e., ways to prevent or reduce MIO, are known. For example, a barrier formed of a material such as polytetrafluoroethylene (PTFE, a.k.a. TEFLON) or ethylene tetrafluoroethylene (ETFE) can be placed over the conductor or along the inside of the insulating layer to shield the insulation from the metal or metal alloys of the device. This process does have drawbacks; the addition of a third component in the device increases its size and makes the manufacturing process more complex and costly. Furthermore, creating bonds and joints in the resultant three-layer component is more complex.
[0007] With particular regard to cardiac pacemaker leads, researchers face intense pressure to maintain or even reduce the small diameter of present cardiac leads, meaning solutions that increase size are avoided whenever possible.
[0008] One way to reduce MIO without making drastic increases in final product dimensions is to provide a layer of conductive metal on the conductor, which metal is tolerated by the insulator. An example is platinum. This increases the overall dimensions by a lesser degree and typically does not present new issues during joining and bonding. However, the additional complex process steps to provide the layer and the materials themselves tend to be prohibitively expensive for many applications.
[0009] To meet the strict size demands and minimize manufacturing costs, other solutions have been proposed. For example, a voltage stabilizing additive (VSA) can be added to a polymeric insulating layer as taught in U.S. Pat. No. 6,879,861. However, such polymers can be difficult and expensive to produce and the VSAs incorporated therein can leak into the patient, causing injury.
[0010] Alternatively, two layers of polymers with different characteristics can be used, the layer closest the metal being selected from those which are particularly resistant to MIO, while the outer layer is chosen based on qualities such as insulating ability and glidability. U.S. Pat. No. 5,375,609, among others, provides examples of this configuration. While this might provide improved MIO-resistance in the outer insulating layer, the product cannot be optimized as the first layer must be considered, which may make the overall device less flexible, thicker, etc.
[0011] To help addressing the issues of flexibility, the inner layer of insulation can be a silicone layer, U.S. Pat. No. 5,628,774. However, this results in a device which still has undesirably large dimensions.
[0012] Thus, despite the advances described above, there remains a need in the art to improve known techniques and optimally provide improved devices which reduce the stress on the insulators without compromising device dimensions or other beneficial properties such as flexibility.
SUMMARY OF THE INVENTION
[0013] An object of the present invention is to provide improved implantable devices which have an electrically conductive metal or metal alloy having an outer surface.
[0014] This object is achieved by an implantable medical device, having an electrically conductive metal or metal alloy having an outer surface; a passivated area on at least a portion of the metal or metal alloy outer surface; and an insulating layer having an inner surface configured to fit over at least part of said passivated area.
[0015] The electrically conductive metal or metal alloy can include cobalt, and/or the insulating layer can be polymer-based, such as polyurethane. The improvement resides in providing the metal or metal alloy with a passivated surface, such that metal ion-induced oxidation (MIO) will be reduced.
[0016] The electrically conductive metal or metal alloy can be the conductor in an elongated lead, such as a cardiac pacemaker lead.
[0017] Preferably the metal conductor surface is depleted of Co atoms, and more preferably it is also enriched in Cr atoms.
[0018] The passivated metal surface can be provided by chemical treatment, such as acid treatment.
[0019] The insulation layer can be provided around the entire passivated surface of the conductor.
[0020] According to a further aspect of the invention, a method of preparing an implantable medical device comprising an insulated conductor is provided, the method comprising providing an elongated metal or metal alloy conductor having an outer surface, treating the conductor with a suitable acid, such as HNO 3 , and providing an insulation layer around at least a portion of the metal alloy conductor.
[0021] According to a further aspect of the invention, a method of protecting electrical insulation, suitably polymeric insulation, from metal ion-induced oxidation is provided, which has providing an electrically conductive metal or metal alloy having an outer surface, passivation treatment of at least a portion of the conductive metal or metal alloy outer surface, and positioning the polymeric electrical insulation on the passivated surface.
[0022] According to a further aspect of the invention, a kit for preparing an implantable medical device is provided, which comprises an electrically conductive metal or metal alloy, a means to provide the metal or metal alloy with a passivated area in the form of a layer or a film, and an insulating layer configured to fit on the electrically conductive metal or metal alloy.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0023] As used herein the term “passivation” means a chemical treatment rendering the surface less prone to cause or contribute to metal ion-induced oxidation (MIO). Consequently a “passivated surface” or “passivated metal” shall be taken to mean a surface or metal that has been treated to exhibit a reduced degree of MIO in any application, preferably medical applications.
[0024] As noted above, the present invention provides a new configuration for implantable medical devices which allows for a slim profile while protecting insulating layers from MIO. This is achieved by providing a passivated surface on the medical device, suitably as a passivated layer or film, on at least part of the metal or metal alloy-containing device. This passivated surface layer or film shields the overlying insulating layer from MIO while having a negligible effect on the dimensions and mechanical properties of the device. The thickness of this film or layer is 1 nm-20 nm, preferably 2 nm-5 nm. In particular the passivated layer is depleted of Co and suitably enriched in Cr.
[0025] Acid treatments of metal surfaces for passivation purposes are known in the art. For example treatment of stainless steel by subjecting it to HNO 3 is a commonly used procedure to enhance corrosion resistance. Other known chemical treatments are e.g.
[0026] a) submersion in a chromic acid bath for 30 minutes at 46° C.,
[0027] b) submersion in a chromic acid bath for 60 minutes at 56° C.,
[0028] c) submersion in a tricresyl phosphate (TCP) bath for 2 days at 107° C.,
[0029] d) exposing the steel to citric acid solution, typically 4-10% by weight.
[0030] In a presently preferred embodiment HNO 3 is used as the acid for the chemical treatment. Suitably an aqueous solution of HNO 3 is used, the concentration of which is 5-30% by weight. More preferably the concentration is 8-20% by weight, most preferred 10-15% by weight.
[0031] The resultant passivated metal conductor has a layer of a modified alloy which is extremely thin, in the area of 1 nm to 20 nm. This allows the present invention to provide a device which does not measurably exceed current product dimensions. Furthermore, the passivated metal conductor maintains the advantageous properties of the underlying material, whether those are strength, flexibility, or other.
[0032] The devices and methods of the present invention are particularly effective at shielding polyether-based polyurethane insulations from cobalt present in conductors in cardiac pacemaker leads. This is both because the passivated layer effectively depletes the surface of Co, but also because the passivated layer does not have a significant effect on product dimensions and mechanical properties, two factors that are exceedingly important with cardiac pacemaker leads.
EXAMPLES
Example 1
Passivation Using HNO 3
[0033] A passivation treatment of pacemaker lead coils was performed using 10.5% HNO 3 (aq) in order to improve the corrosion resistance as described below.
[0034] A cardiac pacemaker lead conductor was formed according to known methods from the fatigue-resistant electrical conducting material 35N LT (a non-magnetic, nickel-cobalt-chromium-molybdenum alloy available from FWM (Fort Wayne Metals, Indiana, USA); composition: approx 35% Co, 35% Ni, 20% Cr and 10% Mo by weight).
[0035] Sample lead coils (both inner and outer coils) were immersed in a 10.5% (by weight) HNO 3 (aq) bath at a temperature of 35° C. for a time of 150 minutes. Stirring could be beneficial.
[0036] However, the treatment can be performed at different temperatures. The temperature could be as low as 0° C. but suitably not exceeding boiling temperature for the solution, i.e approx. 100° C. A suitable interval is room temperature (20° C.) up to 75° C., suitably 30 to 60° C., ideally 30 to 50° C.
[0037] The treatment period could vary between 1 min and up to 24 hours, preferably 30 minutes up to 6 hours, most preferred 2 hours to 4 hours.
[0038] The release rates of metal from the alloy during the passivation treatment was followed by measuring the concentration of the metals in question in the bath liquid using ICP-AES (Inductive Coupled Plasma—Atomic Emission Spectroscopy). Data from the experiment are shown in Table 1
[0000]
TABLE 1
Metal
Metal release
(μg/cm2/h) SD
Co
0.13
0.008
Cr
0.03
0.005
Mo
0.02
0.000
Ni
0.12
0.036
[0039] As can be seen, the release rate is considerably higher for Co and Ni (the largest alloy constituents) than for Cr and Mo. Of the total amount of metal released, Co accounts for 43%, Ni 40%, Cr 10% and Mo 7%. Thus, these results show preferential dissolution of Co and Ni during the passivation in the strong acidic solution. Relatively lower release rates of Cr and Mo may be a result of formation of stable oxides of these elements. When stainless steel is passivated in an acidic solution, the passive surface film becomes enriched in Cr, as a consequence of selective dissolution of Fe. Similarly, preferential dissolution of Co and Ni leads to a Cr enriched passive oxide film on the Co-base alloy.
Example 2
Release of Metal in Synthetic Biological Media
[0040] The release of Co, Ni, Cr and Mo from non-passivated and passivated 35N LT, respectively, was investigated by immersing lead coils in PBS (phosphate buffer saline) with 100 mM H 2 O 2 , a synthetic biological media. Total immersion time was 3 hours (180 minutes). The addition of H 2 O 2 is done to take into account accelerated corrosion due to generation of aggressive species in the biological system during inflammatory response. The metal release rates are shown in Table 2, which compares passivated and non-passivated lead coils made of alloy 35N LT.
[0000]
TABLE 2
Metal
Metal release
(μg/cm 2 /h) SD
Co, pass.
0.12
0.02
Co, non-pass.
0.23
0.04
Cr, pass.
0.17
0.01
Cr, non-pass.
0.19
0.06
Mo, pass.
0.09
0.00
Mo, non-pass.
0.13
0.01
Ni, pass
0.55
0.19
Ni, non-pass.
0.76
0.07
[0041] The table clearly shows that the passivation treatment resulted in a decrease in metal release, in particular of Co, from the alloy 35N LT in PBS+100 mM H 2 O 2 . This can be explained by the enrichment of Cr and depletion of Co in the passive oxide film provided by the passivation treatment.
[0042] Since MIO is believed to be caused by metal (notably Co) ions originating from the alloy, the results show that chemical passivation treatment according to the present invention is beneficial in reducing MIO in applications were metals are exposed to corrosive environments.
Example 3
[0043] A lead coil as in Example 1 is submersed in a chromic acid bath for 30 minutes at 46° C. A passivated surface is obtained.
Example 4
[0044] A lead coil as in Example 1 is submersed in a chromic acid bath for 60 minutes at 56° C. A passivated surface is obtained.
Example 5
[0045] A lead coil as in Example 1 is submersed in a tricresyl phosphate (TCP) bath for 2 days at 107° C. A passivated surface is obtained.
Example 6
[0046] A lead coil as in Example 1 is exposed to citric acid solution typically 4-10% by weight. A passivated surface is obtained.
[0047] The resultant passivated, insulated lead can be connected to a cardiac pacemaker at a proximal end, inserted into a patient and connected to the patient's heart at a distal end.
[0048] The lead described herein offers improved resistance to degradation of the polymer insulation without possessing any statistically significant increase in product dimension. Furthermore, the flexibility, fatigue-resistance, glidability and other beneficial properties of the insulated lead are maintained. The passivated layer on the conductor thus provides the additional benefit of extending potential product life. Extending product life in a product such as a pacemaker lead reduces the risk of complications or injury to the patient while also reducing the chance that an additional procedure is required to remove and replace a lead, which also reduces the risk of adverse outcome for the patient while minimizing medical treatment costs.
[0049] Although modifications and changes may be suggested by those skilled in the art, it is the intention of the inventor to embody within the patent warranted heron all changes and modifications as reasonably and properly come within the scope of his contribution to the art. | An implantable medical device is made more durable and long-lasting by providing a passivating layer or film on at least a portion of a metal or metal alloy outer surface of an electrically conducting device. An insulating layer is placed on the passivating layer or film. The passivation can be a chemical passivation, and is preferably an acid treatment. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is the U.S. National Phase of PCT/EP2014/053277 filed Feb. 20, 2014, which claims priority of German Patent Application 10 2013 206 545.0 filed Apr. 12, 2013.
BACKGROUND OF THE INVENTION
Field of the Invention
The invention relates to steerable wheel sides of a drive axle for heavy crane vehicles or the like, having a knuckle support which is arranged in a steerable manner at an axle guard of a middle axle section and which has a knuckle axially passed through by a drive shaft part, at which a wheel hub and/or a hub carrier having a wheel hub gear is rotatably supported, with the wheel hub gear being drive-connected to the drive shaft part at an input side.
Description of the Prior Art
Axles which are configured as drive axles and which have Ackermann steering for heavy freight vehicles and/or special-purpose vehicles regularly have steerable wheel sides of the initially named kind.
Such axles are inter alia used for heavy vehicles, for example for crane vehicles, usually with 25 inch tires. In this respect, multi-part rims have so far been required its order to be able to mount the tires typical of such vehicles, on the one hand, and to be able to provide sufficient construction space for the brake system, on the other hand. Since the axle loads which are permissible in road traffic are limited, powertrains, with a small weight are generally aimed for. Having regard to weight-critical cases of application, expensive, dismantlable aluminum rims are customary in this connection. This is where the invention comes in, in that it is proposed not to replace the customary multi-part steel rims with multi-part aluminum rims in case of weight problems, but rather with integrally formed drop center rims which can also be composed of steel in cases that are weight-critical. In addition to a substantial cost advantage, such rims provide the advantage of a particularly high robustness which is desirable above all in rough conditions of use.
However, the use of drop center steel rims has previously failed in that the spatial conditions at a drive axle having Ackermann steering does not permit the use of disk brakes (preferably actuated by compressed air). This is because in contrast to the multi-part dismantlable rims which can have a very flat rim base due to their dismantling capability, a sufficient accommodation space for disk brakes dimensioned in accordance with the conditions of use of the respective vehicles is not available radially within the drop center steel rims, with the additional difficulty that the customary 25 inch tires require a particularly deep drop center for their mounting.
SUMMARY OF THE INVENTION
For this reason, it is the object of the invention to provide new wheel sides for driven axles having Ackermann steering, with the wheel sides permitting the combination of disk brakes and drop center steel rims (for the previously customary 25 inch tires).
This object is satisfied in accordance with the invention in that a wheel flange dimensioned for an integrally formed drop center rim and a drop center rim which can be screwed to the wheel flange are provided at the wheel hub and in that, within an axial range having a diameter which is small in comparison with the diameter of the wheel hub gear, the wheel hub has a brake disk which is axially displaced towards the axle guard with respect to the drop center rim and which cooperates with a service brake which is axially screwed to the knuckle support.
The invention is based on the recognition that the price advantage of steel drop center rims with respect to multi-part aluminum rims can overcompensate possible cost disadvantages in the axle construction and that a sufficient accommodation space for suitable pneumatic disk brakes can be provided at the wheel side on a reduction of the diameter of the wheel hub in the region between the rim and the axle guard.
In accordance with a particularly preferred embodiment of the invention, it is provided that a brake anchor plate, to which a brake caliper, preferably two brake calipers, is or are axially screwed, is axially screwed to a wall of the knuckle cap of the knuckle support, with the wall being axially adjacent to the joint connection and the knuckle cap being pivotably connected to the axle guard. An axial screw connection is understood such that the screw longitudinal axis is aligned (approximately) in parallel with the wheel axle. The brake anchor plate can be arranged at a flange surface orthogonal with respect to the axis of the knuckle at the outer side of the aforesaid knuckle cap. An arrangement is hereby advantageously possible in which the brake caliper or the brake calipers can be mounted at, the brake anchor plate from the wheel side.
It is furthermore advantageous when the axle guard spacing is dimensioned in accordance with a size which substantially corresponds to the cross-section or the spatial requirement of the joint connection between the shaft part passing through the knuckle and a drive shaft arranged in the middle axle section.
On an actuation of the steering, the knuckle pivots in a conventional manner about a pivot axis which is slightly inclined with respect to the vertical (so-called spreading of the pivot axes) and which moves away from the wheel plane in an upward direction and approaches the wheel plane in a downward direction. This has the consequence that the vertically lower end of the axle guard can restrict the possible construction space for the brake system and can restrict the brake anchor plate, as the lower end of the axle guard has a smaller spacing from the wheel plane, the deeper it is arranged. In that the lower end of the axle guard is now provided as high as possible in accordance with the preferred embodiment of the invention, this means at an upper position at which the connecting joint is still given sufficient space, it is ensured that the axle guard cannot form an interfering contour for the arrangement of the brake.
As a result, it is achieved in this manner that the flange surface provided at the knuckle support is (sufficiently) spaced apart from both ends of the axle guard for the mounting of the brake anchor plate.
Provision is in addition preferably made such that the axle guard and the knuckle cap pivotably connected thereto are configured narrow in a vertical plan view of the wheel side and/or of the drive axle in such a way that, on the one hand, large steering angles (>40°) can be achieved and at the same time (in a vertical plan view) component parts of the brake system (at the brake anchor plate) can still be arranged besides the knuckle cap.
Furthermore, it is expediently provided to configure the wheel hub gear as axially narrow such that the hub part receiving the wheel hub gear cannot form any interfering contour projecting axially far beyond the wheel plane. For the rest, the possible axial construction space for the brake system between the wheel and the axle guard is also increased by means of this measure.
It is preferably provided for the dimensioning of the brake disk that the brake disk diameter approximately corresponds to the vertical outer dimension of the knuckle support. On the one hand, an arrangement of the brake system protected to the greatest possible extent between the wheel and the axle guard is in this way possible; on the other hand, the necessary and/or desirable braking forces can also be ensured particularly since a double arrangement of the brake calipers is made possible with this dimensioning.
With respect to preferred features of the invention, reference is made in another respect to the claims and to the following description of an advantageous embodiment by means of the drawing.
The features shown can also be essential to the invention in a combination deviating from the drawn illustration, optionally also as individual features.
BRIEF DESCRIPTION OF THE DRAWING
In the drawing, the sole FIGURE shows an axial section of a wheel side in accordance with the invention.
DETAILED DESCRIPTION OF THE INVENTION
In accordance with the drawing, the invention relates to a drive axle having Ackermann steering. In this respect, a middle section of the axle, which as a rule comprises the respective axle differential, has an axle guard at its two ends, the axle guard having an upper guard end 1 ′ and a lower guard end 1 ″, at which ends a knuckle support 2 having a knuckle 3 connected in one piece to a knuckle cap 3 ′ is arranged in a steerable manner about a pivot axis S predefined by the guard ends 1 ′ and 1 ″. The knuckle 3 is configured as a hollow body and receives a drive shaft part 4 in an axial central bore, with the drive shaft part being connected drive-wise to a drive shaft 6 arranged in the middle axle section via a joint connection 5 arranged in a free space between the knuckle cap 3 ′ and the guard ends 1 ′ and 1 ″. A wheel hub arrangement 8 is rotatably supported at the knuckle 3 by means of roller element bearings, in particular cone bearings 7 , and is in a drive connection with the drive shaft part 4 via a wheel hub gear 9 . A drop center rim 10 preferably composed of steel is arranged at the wheel hub arrangement 8 . The wheel hub arrangement 8 comprises an axially inner housing part 8 ′ which is rotatably supported at the roller element bearings or at the cone bearings 7 and whose outer periphery tapers conically in the direction of the joint connection 5 . The inner housing part 8 ′ expands axially outward to the diameter of a wheel flange 11 which is provided for the mounting of the drop center rim 10 and which is configured as a double-wall flange, with the axially inner wall being configured as a part of the inner housing part 8 ′ and the axially outer wall being configured as a part of an axially outer housing part 8 ″ which receives the wheel hub gear 9 .
This wheel hub gear 9 can be configured as a single-stage planetary gear, with the axially outer end of the drive shaft part 4 supporting a sun gear 12 which is arranged with a corresponding inner toothed arrangement at a matching outer toothed arrangement of the drive shaft part 4 in a shape-matched and/or a rotationally fixed manner. This sun gear 12 meshes with planetary gears 13 which are rotationally supported at corresponding axle bolts at the outer housing part 8 ″ configured as a planetary gear carrier. The planetary gears 13 further mesh with an annulus gear 14 which is arranged in the outer housing part 8 ″ and which is rotationally fixedly connected to the knuckle 3 via an annulus carrier 15 in a generally known manner. For this purpose, the annulus carrier engages with an inner peripheral toothed arrangement into a corresponding outer toothed arrangement at the knuckle 3 in a shape-matched manner and engages with an outer peripheral toothed arrangement into a or into the inner peripheral toothed arrangement of the annulus gear 14 .
The annulus carrier 15 has a key-like shape which is adapted to the conical shape of the inner housing part 8 ′ approximate to the wheel flange 11 .
A brake disk 16 is furthermore arranged at the wheel flange 11 by means of a sleeve-shaped brake disk plate 17 which is connected to the brake disk and which is radially spaced apart from the axially inner housing part 8 ′ by an air gap. A thermal insulation of the brake disk 16 with respect to the housing part 8 ′ is thereby ensured and it is in particular avoided that seals, which are radially arranged between the knuckle 3 and the housing part 8 ′, could be thermally destroyed.
The brake disk is preferably configured as a thick solid disk which, on “violent brakings” briefly following one another, is able to take up large amounts of heat with a corresponding heating without losses with regard to its mechanical stability and is in this respect advantageous with respect to an internally ventilated brake disk.
In the example shown, the brake disk 16 is arranged, in the axial direction of the wheel hub arrangement 8 , in approximately the same plane as the axially inner roller element bearing or axially inner cone bearing 7 . The brake caliper associated with the brake disk 16 or the associated caliper can be arranged double for ensuring very high braking torques, with a brake anchor plate or a caliper bracket 18 at a flange surface at the outer side of the knuckle cap 3 ′ serving for fastening a service brake cooperating with the brake disk 16 . In order to be able to ensure a sufficient construction space for the brake calipers, the wall of the axle cap 3 ′ comprising the brake anchor plate or the caliper bracket 18 is approximated as far as possible to the joint connection 5 . A sufficient free space for the brake calipers and for the brake component parts on steering movements of the knuckle 3 is simultaneously ensured by a particularly narrow configuration of the axle guard 1 and of the knuckle cap 3 ′ on a view in the direction of arrow P:
The lower end 1 ″ of the axle guard 1 has a position vertically approximated to the joint connection 5 such that, due to the inclined pivot axis S, the lower end 1 ″ is positioned at a position maximally spaced apart from the wheel plane and cannot form any interfering contour for braking members.
It becomes clear from the drawing that the following features are of particular importance for the combination provided in accordance with the invention of a drop center rim with a disk brake arrangement at a wheel side of a drive axle having Ackermann steering:
Between the wheel plane and the facing side of the knuckle support, the wheel hub arrangement 8 has a considerably reduced diameter in comparison with the wheel hub gear 9 , wherein such a design of the wheel hub arrangement is facilitated by a knuckle 3 having a small diameter and by roller element bearings or cone bearings 7 having a reduced radial height.
Furthermore, an as large as possible axial spacing should be present between the wheel plane and the side facing the knuckle support 2 . This is, on the one hand, facilitated by a wheel hub gear 9 which is axially narrow in construction and which can be provided at the outer wheel side without formation of an impermissible interfering contour due to its narrow design. The cap 3 ′ of the knuckle support 2 is furthermore approximated as far as possible to the joint connection 5 between the drive shaft 6 and the drive shaft part 4 , wherein the plane of the outer side of the knuckle cap 3 ′ which is usable as a flange surface also remains free of interfering contours in the region of the lower end 1 ″ of the axle guard 1 when the lower end 1 ″ of the axle guard 1 is vertically approximated as far as possible to the joint connection 5 .
Increased forces and/or torques then indeed arise at the guard ends with respect to axle guards having a larger guard spacing, but are able to be easily controlled by means of a corresponding selection of material and dimensioning.
In addition, it can be clearly seen from the drawing that the brake anchor plate or the caliper bracket 18 can be axially screwed to the knuckle cap 3 and the brake calipers 19 can be axially screwed to the brake anchor plate or the caliper bracket 18 . This facilitates a double arrangement of the brake calipers.
Overall it must be stated that a possibly increased manufacturing or constructive demand in effort and cost at the wheel side is overcompensated by the price advantages of a steel drop center rim 10 , whose use becomes possible in a simple manner by means of the invention with a further advantage being gained in that a steel drop center rim is considerably more robust, with comparable weight advantages, than previously customary multi-part aluminum rims. A weight advantage is furthermore achieved.
REFERENCE NUMERAL LIST
1 axle guard
1 ′, 1 ″ upper guard end, lower guard end
2 knuckle bearing
3 knuckle
3 ′ knuckle cap
4 drive shaft part
5 joint connection
6 drive shaft
7 roller element bearing or cone bearing
8 wheel hub arrangement
8 ′, 8 ″ axial inner housing part, axially outer housing part
9 wheel hub gear
10 drop center rim
11 wheel flange
12 sun gear
13 planetary gears
14 annulus gear
15 annulus carrier
16 brake disk
17 brake disk plate
18 brake anchor plate or caliper bracket
19 brake caliper
S pivot axis
P direction of arrow | The wheel side of a drive axle with wheel member steering having a drop center rim, preferably made of steel, is provided on the wheel hub and is combined with a disc brake, which is axially inwardly offset relative to the wheel plane and which preferably has compressed an actuation. The necessary space for the disc brake arrangement is guaranteed by the sufficiently low diameter of the wheel hub in the region of the brake disc and by a comparatively large axial space for the brake system, which is created by an axially narrow design of the wheel hub transmission and a by a new design of the steering knuckle bearing and of the pertaining axle guard. | 5 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Patent Application Ser. No. 62/235,310, filed on Sep. 30, 2015, and entitled WATER JET MINING SYSTEM AND METHOD, which is incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present application relates to the field of subterranean water jet/hydraulic borehole mining. More specifically, the present invention relates to a new and novel high pressure system and method to perform economic, high production, continuous commercial mining by water jet borehole mining within a target ore body either in fully submerged conditions below the water table or under full atmospheric conditions.
BACKGROUND OF THE INVENTION
[0003] In situ hydraulic borehole mining equipment and techniques are known in the art and are the subject of patents that disclose systems for the mining of uranium, phosphate and heavy oil resource bodies, such as U.S. Pat. No. 4,915,452 issued to Dibble; U.S. Pat. No. 4,296,970 issued to Hodges; and U.S. Pat. No. 4,348,058 issued to Coakley et al. However, the mining systems and methods in these representative disclosures do not effectively address the fluid dynamics associated with maximizing effective jet horsepower, do not provide an economical alternative for mining in an isolated flooded environment, and do not effectively address the ability to efficiently lift a subterranean resource to the surface. More specifically, these prior patents disclose equipment systems designed solely to lift ore back to the surface by the use of a high-pressure eduction system. Notwithstanding the advances made by these inventions, to date, no prior art hydraulic mining system has attained commercial success of the shortcomings being attributable to the ineffective and inefficient utilization of fluids and the sub-optimization of the mining extraction processs. Prior art systems do not fully integrate the critical components of water jet borehole mining to optimize reach and production rates on the one hand and to minimize energy consumption on the other. Thus, continual economically justifiable and sustainable commercial production rates have not been achieved, and the operating costs of prior art borehole mining systems are too high to effectively replace conventional commercial mining systems and techniques.
[0004] In addition to the foregoing, the very mining pipe associated with prior art mining systems is the source of frustrating and costly operational problems. The threaded portions used to couple various sections of the mining pipe are prone to galling and eventually become unusable. In a threaded connection with multiple telescoping pipes, several sets of threads must be properly aligned in order to make up the mining string. Even with small misalignments, threads become galled, rendering a piece of mining pipe unusable. With the three concentric parallel strings of the subject invention, the pipe is aligned and threaded together with only one pipe, preferably, the outermost pipe, while the other two pipes employ tapered coupling or connecting portions, which self-align, virtually eliminating any chance of damaging the mining pipe sections. With the threaded connections and tapered internal pipes of the system invention, the problem of galling of threads is eliminated, inasmuch as the threads interconnecting all but the outermost section have been eliminated.
[0005] Another problem associated with prior art mining systems is the tendency of the systems to collect oversized particles in the bottom of the mining cavity. These particles clog up the system. When the system becomes blocked, advancement stops, requiring tripping out of the hole and drilling the rock fragments up by conventional methods. This interruption, which is eliminated by the system disclosed herein, severely affects operating economics and completely stops advancement under block caving conditions.
[0006] Water jet borehole mining has several advantages over conventional mining techniques. One of the key attributes exploited through the borehole mining technique is the ability to selectively target and mine high-grade resources. With water jet borehole mining, the highest-grade section of the resources can be selectively mined while leaving the remaining lower grade resources in place. With traditional mining techniques, the overburden is removed or worked around in order to access the targeted resource. The usual expense and dilution of the economics of the project can render the project economically unfeasible. The use of the subject invention and associated techniques allows a small borehole to be drilled into the resource body, thereby permitting the target ore to be efficiently and economically mined and moved to surface without disturbing the overburden. Non-turbid lamination of the water flow to the jet is one component of the subject invention in terms of ultimate production and reach of the jet in the cavern in both atmospheric and submerged conditions.
[0007] The environmental impact of an underground hydraulic borehole mining process is exponentially less than that of a conventional open pit mining application. Highly mobile equipment deployable at any angle on commercially available modern drilling rigs allows high accessibility to horizontal surface based, high slope and marine based applications. Small-scale equipment used in the process minimizes site impact and decreases mining risk of groundwater and surface contamination by cased isolation of the mining system and effective protection of groundwater. Leaching of resources such as uranium or contaminated fluids or acids such as those generated through oil sands or heavy minerals mining is minimized, if not completely eliminated. A unique aspect of the system herein disclosed is that, compared to prior art systems, it can operate both in a fully submerged state and in an atmospheric state. Operating in an atmospheric state extends the reach in certain geology by increasing net delivered horsepower at the rock face.
[0008] In some cases, total elimination of open pit access allows safe access to the resource. The effective mining of the resource can allow stripping the target components within the ore, such as the ablation of U308 particles from sandstone or stripping target minerals from mineral sands and the corresponding reinjection of the waste tails in situ by blended sealing with cementitious grout. Effectively, remediation costs and requirements are significantly reduced, less overburden is moved, less in situ groundwater is affected, less surface impact is created and the carbon footprint of mining operations using the invention is greatly reduced compared to conventional mining operations or prior art hydraulic borehole mining technology. Personnel head count can be reduced and exposure to high-risk ore such as uranium can be greatly reduced by effective and economic commercial hydraulic borehole mining. It is not necessary to expose personnel to radiation risk underground. Moreover, the invention provides closed loop fluid circulation, thereby limiting oxygenation of the resource, and reducing environmental exposure of radiation, salt water and acid onto the surface and in situ mining sector.
[0009] Within the United States and in multiple countries around the world a vast inventory of projects exist that have either reached the end of their known economic mining life, or that cannot be initiated into production due to unachievable economics or operational or technical inaccessibility. This invention with the complete modernization of new, conceptual and proven hydraulic engineering components will provide a new opportunity to reestablish prior mined resource areas, to create new jobs by economic resource creation and to enrich both private industry and government owned resource bases. Further, this invention will allow the establishment of a new realm of mining potential in environmentally sensitive areas which are not accessible currently because of destructive surface mining or risk of exposure to undesirable mining circumstances. Additionally, the mobility and accessibility of this invention allows the resource owner to target smaller reserves with more discerning accuracy of mining, thereby increasing established resource and reducing capital and regional impact.
[0010] Resource body types exist that are not currently available, such as metallurgical coal seams in steeply dipping planes along the environmentally sensitive slope of the Rockies, the steep hills of Appalachia, and the ultra-heavy oil reserves of west Texas and California. The shale oil reserves on the Eastern Rockies slopes are sub-economic to conventional mining. The deep in situ uranium deposits in New Mexico, Colorado and Texas and the kaolin and phosphate deposits of the Southeastern states all have development, reserve and resource potential beneficial to private industry and government with the effective deployment of this system and apparatus. The Kimberlite reserves of Saskatchewan, Canada cannot be developed with conventional mining methods, yet exist as the largest Kimberlite reserves in the world. Kimberlite pipes which only allow fractional accessibility through conventional mining, Kimberlite and Lamprolite pipes in Australia and South Africa that have reached economic limit because dewatering costs are too high or the size of the pipes and the incline of the hanging walls are too steep for conventional mining, all may be accessed by the system and methods herein disclosed. The same may be said of millions of tons of other known resources that cannot be mined or declared as economic reserves because the ore is inaccessible due to high water tables and or excessively steep access ramps. This invention allows the resource owner to drill deep into pipes and target high-grade ores and minerals selectively and, under certain conditions, up to depths never achievable with conventional mining techniques. Offshore mining of granular resources such as tin can be in situations where conventional dredges cannot access the resource through deep overburden. Technical accessibility to otherwise unavailable resources with the system of the present invention significantly enhances mining potential while simultaneously offering low surface and environmental disturbance.
[0011] In the hydrocarbon resource sector, the system allows further development of oil shales, oil sands, oil rock and gas shales by cavity creation. Cavity creation allows significant opening of the natural fractures of the rock and may be used as a replacement to hydraulic fracturing or “fracking.” This advancement alone may have a significant impact on the conventional oil industry in areas where fracking creates potential for disturbance or is completely banned.
[0012] The nature of the system allows the operator to excavate the oil in situ and transport the oil bearing rock to the surface. The subject invention will allow unique access to depleting fields that have significant quantities of oil not currently economically recoverable with known technology. The mining system of the present invention could be used in countries where fracking is completely banned and as a substitute where shallow heavy oil deposits exist.
SUMMARY OF THE INVENTION
[0013] The subject invention provides an economic mining alternative to the energy consumption and fluid requirements of the prior art mining technology employing sole eduction systems by utilizing hydraulic airlift and/or eductor system technology to lift the resource to the surface through the vertical lift section. The configuration of the mining pipe of the present invention includes at least two concentric annular rings or pipes structured and arranged to selectively deliver air, high pressure water and low pressure water to the extraction site. The mining pipe system further includes an inner bore reverse circulation system differential which allows an operator to inject a small amount of low pressure air into the return fluid column, reducing its density and creating a vacuum at the system inlet to efficiently lift most resources to surface.
[0014] When compared to prior art stand-alone eductors, the airlift system of the subject invention can operate very efficiently with very limited energy. The reduced horsepower and diesel consumption during operation of the mining system of the present invention creates dramatic capital and operating cost savings.
[0015] The eduction system is an effective method to return the slurry to the surface. In some conditions such as with horizontal mining, eduction works in conjunction with the other components of the mining system. However, as a stand-alone method of lifting, the energy requirements are very high and need a very high ratio of fluid and pressure be circulated to the bottom of the well bore to educt the disaggregated resource material back to surface. The subject invention addresses this and other problems associated with prior art systems by being designed to work while jetting in atmospheric conditions or in submerged conditions. The eduction built into the system is provided and allows access to long horizontal resource beds from the surface by providing a low pressure fluid eductor at the inlet of the miner to push the slurry coaxially through the horizontal section of the mining pipe and up into the vertical section of the well bore thru to surface with the ability to use the hydraulic airlift at that point to help boost the fluid the rest of the way to the surface through differential hydraulic pressure.
[0016] The pipe connections within the system herein disclosed address the galling problems noted above and are critical and unique to the system. The high-pressure fluid streams have no tolerance for leakage. The jetting connections operate at extremely high pressures (up to 8,000 psi) and the fluid must remain fully, safely and properly sealed for the entire length of the mining system. A pressure or fluid loss at a connection is intolerable due to the safety risk at high pressures and the critical need to control jet volumes and consistent delivery pressure at the outlet. The system design overcomes this by using the middle section of the pipe to carry the high-pressure cutting fluid. Accordingly the outer pipe acts as a protective sleeve.
[0017] More particularly, the method of the subject invention involves economically mining subterranean resource in situ comprising the steps of drilling a surface hole into subsurface material to access the target resource, injecting high pressure fluid via a borehole mining tool into the resource thereby forming a jet to disaggregate the subsurface material creating a slurry of solids and fluid, injecting a low pressure water stream for eduction to mix with and transport the slurry, injecting low pressure air into the slurry return line to create suction via differential pressure whereby the slurry is lifted to the surface, separating solids and fluid at the surface and recycling the fluid for reuse in the method.
[0018] The novel system herein disclosed comprises a borehole mining system including at least one multi-conductor high pressure swivel for redirecting high jet pressure fluid and lower pressure eduction fluid in separate sections through the system. The swivel is adapted to pass a generated slurry though a center bore and to redirect the generated slurry at the surface. The system further includes an inner tube for injection of air to assist the return of the slurry to the surface, a lamination device within the mining pipe for placing the high pressure water into laminar flow, a monitor pipe that maintains the laminar flow of the fluid into the quartic-straight jet nozzle, an eductor system for mixing and returning the slurry to the surface, a plurality of internal flush connection subs joining the high pressure section, and a turning section including a plurality of splitter vanes for maintaining the laminar flow of the water during the turn into a jet nozzle.
[0019] The mining system herein disclosed operates at the torque and stress level required for drilling operations while mining. This feature allows an operator to progress the well without removing the mining system, a distinct advantage over prior systems that had to be first removed from the well to progress it. The inlet up the side wall of the monitor allows the continuous mining of soft formation caving, ores, such as mineral sands, and also advancement of the wall.
[0020] Depending upon site requirements, the system of the present invention may be configured to align at least two circular ring high-pressure fluid and/or air supply lines from the pumps at surface; although more circular ring supply bins may be used as needed. The aligned fluid flows travel in parallel to a point in the mining pipe where they are introduced to laminar flow chambers created by sectionalized vanes that align the fluid into laminar flow. The current invention utilizes replaceable and serviceable blade or vane sections that may be quickly and economically repaired for ongoing operations. The vanes become damaged over time by the passing of fluid over them, they may be removed by unbolting the housing and replacing them. Prior art designs often resulted in a pipe split which had to be welded back together or which was otherwise unserviceable and disposable. The laminar flow pipes connect to the mining head itself.
[0021] The plumbing configuration maintains the laminar flow to the delivery section of the miner where the fluid exits the jet nozzle. The system of the subject invention maintains the alignment of the laminated flow in order to maximize the distance and the effectiveness of the jet by means of inset replaceable x-vanes that turn the high-pressure high volume laminar flow while minimizing turbidity and tortuosity.
[0022] The hydraulic borehole mining process of the subject invention can be summarized as follows: drilling a suitably sized hole to convey the borehole mining system to the top of the resources to be mined; casing the surface hole i if necessary, and cementing as known in the art to provide stability and to protect groundwater and resource leaching; drilling a hole at least partially through the resource body; inserting a mining pipe having at least two concentric circular rings or pipes with a jet nozzle and a slurry recovery system into the borehole. A high-pressure fluid pumping system is connected to the mining string and high-pressure fluid is pumped down one of more of the circular ring pipes and out of the jet nozzle at the cutting face. The high-pressure fluid stream interacts with the rock face down hole disaggregating the rock and putting the particles into a slurried suspension; this slurry is then recovered through the center bore of a circular ring piping system and returned to the surface, where the rock that is recovered will be processed and the mining fluid is recycled and used again in the process.
[0023] The mining system of the present invention mines hydraulically at significant depth at all angles from true vertical depth to a completely horizontal setting through a narrow diameter surface drilled hole in both atmospheric and in submerged conditions. High pressure mining fluid is conveyed through the circular ring system to the cutting jet nozzle down the hole. This interaction between the mining fluid and the target rock face disaggregates, slurrifies and returns it to the surface via specific return elements in the system.
[0024] This invention can be utilized to economically and efficiently mine resources that sit from 0 to 90 degrees from the vertical and may be utilized in resource bodies that are submerged or that are dewatered. The system utilizes a fluid that can either be clean water or clean water with polymer additive to increase the hydraulic horsepower to the rock face when the tool is utilized in a submerged or atmospheric environment.
[0025] The entire process occurs in a closed loop system beginning with the high-pressure fluid delivery elements extending from the surface down the borehole to the return elements back up into the surface processing facilities. The system further includes a sealed surface annulus connected to a pump that boosts the pressure on the annulus space, thereby aiding in the return of the slurry to the surface
[0026] Thus arranged, the system maximizes effective hydraulic horsepower and fluid density properties by lamination of fluid flow through the circular pipe mining system down the well bore and though a tight radius turn of the jet stream.
[0027] The mining system of the present inventionis designed to operate within the plane of the ore body that yields the greatest resource production at any angle from vertical to completely horizontal. The system is deployed either by directionally controlled drilling or vertically controlled stabilized drilling.
[0028] All of the elements of this mining system are designed to maximize fluid flow efficiency both down and up the wellbore. This fluid circulation with the laminar hydraulic jet stream and the return to surface using eduction and differential pressure allows a significant reduction in equipment, energy and costs compared to prior art hydraulic borehole mining systems, thus providing the minimization of economic and cost effective operating footprint and personnel prove to define commercial economics in multiple target ore types.
[0029] These and other advantages and novel features of the present invention will become apparent from the following description of the invention when considered in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0030] FIG. 1 is a general schematic of a hydraulic borehole mining system situated at a mining site in accordance with an embodiment;
[0031] FIG. 2 is a side elevation view of the hydraulic borehole mining string of the system of FIG. 1 ;
[0032] FIG. 3 is a side partial sectional view of a monitor subassembly for the hydraulic borehole mining string of FIG. 2 having shielding portions removed to show the elements thereof in greater detail;
[0033] FIG. 4 is a sectional view of a low pressure and high pressure combination swivel in accordance with an embodiment;
[0034] FIG. 5 is a side perspective view of the monitor subassembly with shielding and bit attached for hydraulic borehole mining applications in accordance with an embodiment.
[0035] FIG. 6 .A is a side perspective viewof a quark straight nozzle in accordance with an embodiment.
[0036] FIG. 6 .B is a sectional view of the nozzle shown in FIG. 6 .A;
[0037] FIG. 7 .A is a side perspective view of a mining pipe in accordance with an embodiment; and
[0038] FIG. 7 .B is a side sectional view of the mining pipe shown in Fig. TA having portions removed to show the elements thereof in greater detail.
DETAILED DESCRIPTION OF THE INVENTION
[0039] Referring now to FIG. 1 , a system and a process of hydraulic borehole mining for a subterranean resource in accordance with the present invention is described in detail. A rig shown generally at 1 is brought to the mining site, situated at a preferred location at the site, and operated to drill a well, wellbore or borehole, (as the terms are used in the art) 2 to the top of the resource body. The wellbore may be drilled at any angle from vertical to horizontal depending upon the geotechnical mining conditions down-hole and the structure of the ore body itself. If required, casing string, 3 is then run into the initial wellbore and cemented into position to give it strength. A conventional drilling string is then fed into the casing string, and a pilot hole is drilled at least partially into or through the resource body. The conventional drilling string (not shown) is thereafter removed from the hole.
[0040] Referring now to FIG. 2 , a mining string 5 is illustrated in greater detail. The mining string is run into the wellbore and includes a bottom end 6 , a top end 7 , an elongate portion 8 extending co-axially along a longitudinal axis 9 thereof intermediate the top and bottom ends, and, an eductor bit 10 positioned at the bottom end of the string and attached to a high pressure monitor pipe 12 . The monitor joint or pipe houses at least one quartic-straight jet nozzle 15 ( FIGS. 6 .A and 6 .B) and a plurality of integrated laminar flow vanes within the high pressure monitor pipe 12 as will be described in greater detail below. The monitor pipe 12 , is secured to the bottom end 6 of the mining string 5 that extends from the surface 14 and is operatively connected to a rig floor or platform 16 and associated surface equipment down to a subterranean resource deposit 21 ( FIG. 1 ).
[0041] The mining string includes a swivel 22 operatively connected to the top end 7 of the mining string. As shown in greater detail in FIG. 4 , swivel 22 , connects the mining string 5 via port 120 to the surface equipment providing air and high and low pressure water. As well be described in greater detail below, the swivel 22 consists of a combination of high pressure and low pressure fluid courses; the interconnections of which provide all of the fluid connections needed for the process. The swivel takes the high pressure feeds of water for the quartic-straight jet nozzle, the air to the air lift system, high and low pressure fluids for the eductor turns these fluids and air ninety degrees and sends them down the respective lines or annular concentric pipes in the mining pipe to the attachments down the string. The swivel 22 also provides a passageway or a return line 130 to conduct the slurry up the hole and to direct the slurry to one or more surface processing facilities, generally shown at 26 in FIG. 1 . A unique and novel feature of the system of the present invention is the significantly enhanced ease of maintenance and efficiency of its operation as compared to any prior art systems and methods.
[0042] Referring again to FIG. 1 , the configuration of the surface portion of the mining system is illustrated in greater detail. The surface equipment includes high-pressure, high-volume jet mining pump(s) (not shown), which deliver water down hole via the swivel and high pressure line 32 . An air compressor delivers air to the swivel via high pressure line 36 to be delivered down hole to an airlift exit pipe. A lower pressure water pump delivers water to the backside of the well head via low-pressure water line 44 to keep the surface hole full of water. The supply of low pressure water to the backside optionally may be forced in past a seal, introducing an additional amount of pressure and force to the backside of the pipe. This additional force above the weight of the column of water on the backside gives a boost to the recovery system by essentially forcing fluid under pressure up the mining string's lower density return line and thereafter to surface.
[0043] The return line 130 runs from the swivel to a dewatering system via a low-pressure slurry return line 50 . This portion of the system removes the water from the resource and returns the water to a dirty water storage pond or tank (not shown). A storage facility 56 stores the dewatered resource while awaiting further processing by the mine. The water from the dewatering system then flows to a settling pond where any fines that have collected into the water are permitted to settle before flowing into a clean water storage area (not shown). The clean water storage area holds the clean water, which feeds all of the pumps.
[0044] The clean water is boosted into one or more high pressure pumps and then pressurized and pumped into the high pressure mining swivel 22 ( FIG. 4 ) where it is turned 90 degrees and down the mining string 5 through the mining pipe. The pump(s) feeds the mining pipe line via high-pressure line inlet 32 . The line is connected to the swivel 22 and then runs the length of the pipe via one ring 96 of the concentric annular triple wall mining pipes illustrated in greater detail in FIGS. 7 .A and 7 .A.
[0045] Referring now to FIGS. 7 .A and 7 .B, the elements of the mining string 5 are shown in greater detail. In the embodiment shown, by way of example and not of limitation, the string includes three elongate cylindrical tubes or pipes (also referred to in the art as “subs”), 70 , 72 and 74 , of selectively decreasing diameter, d, with respect to an outer surface 71 of the mining string (only one of which diameters is shown) concentrically disposed about and extending substantially parallel with one another along a longitudinal axis 9 . The inner most pipe 7 forms a center return line or bore 92 for returning the slurry to the surface. Tube 70 cooperates with tube 72 to form an outside annular ring or pipe 94 , and tube 72 cooperates with tube 74 to form an annular ring or pipe 96 extending circumferentially around the bore 92 ; the bore 92 and the annular rings 94 and 96 being concentric with one another. The interconnections between progressive adjoining sections of the mining string 5 utilize full flow concentric connections at each joint to provide a high pressure seal between each inner concentric mining pipe sections 72 and 74 and an adjoining section (not shown) via special high pressure, expandable O-rings 86 ( FIG. 7 .A) seated in grooves 78 formed in a first end 75 , 77 of each of the concentric pipes 72 , 74 respectively ( FIG. 7 .B). The end of each of the subs fits inside a corresponding mating flange (not shown) ona second end of each of the concentric pipes. This novel configuration allows for the full inside diameter (internally flush) of the concentric lines of the mining pipe to be maintained in a concentric relationship with one another to the connection sub. The connection subs are utilized in the connection of the individual segments of the entire mining pipe string 5 ( FIG. 2 ) and the connection of the monitor pipe 12 ( FIG. 3 ). Due to the internally flush-full bore, restriction-free structure of the subs, the pressure drop in the concentric high pressure rings at the connections is substantially reduced over prior art systems, an advantage which manifests itself over a large number of connections in a string, where the pressure drop over the overall distance would be significant. Moreover, the threaded connections found in prior art system, which are subject to galling are eliminated in the internal portions, thereby significantly reducing system downtime and extending the useful life of the mining string. Only the external pipe 70 includes a male threaded end 80 , which is adapted to be threadably connected to a corresponding female threaded end of an adjacent section.
[0046] The monitor joint or pipe 12 contains laminar flow vanes positioned perpendicular to one another and which are structured and arranged to create and maintain a laminar flow of the mining fluid. The monitor includes laminar vanes (not shown) which are adapted to preliminarily align the otherwise turbid flow of the water into a laminar flow stream configuration, thereby providing increased hydraulic horsepower to the jet stream. As noted above, the laminar flow is established utilizing the vanes to split and align the flow. The vanes are formed of a suitable material such as steel and are positioned securely in the monitor.
[0047] Referring to FIG. 3 , and, as shown in greater detail in FIG. 7 .A., the annular high pressure water rings 94 , 96 of the mining pipe feed the water flow to the monitor pipe 12 where the water becomes laminar, thus ensuring that laminar flow is maintained while the water is joined to and then forced through the monitor 12 . In an embodiment, the high pressure water flow may be limited to only the inner annular ring or pipe 96 , the outer annular ring 94 serving to deliver low pressure water and also as a safeguard against any high pressure leakages. The monitor maintains the water flow in a laminar stream without introducing turbidity and then turns the water flow into at least one quartic-straight jet nozzle 15 ( FIGS. 6 .A and 6 .B). As a result, more water at a higher velocity can be provided through the system because of the continuation of the laminar flow. The quartic-straight jet nozzle delivers the laminar flow into a focused jet through a nozzle orifice 90 delivering a high pressure, high volume stream of fluid at supersonic velocity into the rock face.
[0048] As the water jet impacts the rock face it begins to disaggregate the material. The disaggregated material mixes with the water creating a slurry stream which is then carried to the eductor bit 10 as shown in FIGS. 2 and 5 . The eductor bit pushes the slurry stream up a slurry return pipe 92 in the monitor 12 which is connected to the slurry return pipe 92 ′ in the mining string, whereupon it is accelerated by a vacuum created in the return pipe 92 by the combination of airlift assist and the pressure applied to the outside of the mining string 5 , in part via the low pressure water line 44 as described above. This vacuum is created in two unique ways. First, the airlift assist is charged by air from a compressor and is carried through the mining pipe via an air line (not shown) that runs inside the internal slurry return pipe 92 where it terminates at the ideal airlift placement, depending on conditions, typically at a depth of approximately 200 feet. The air then escapes through the open ended pipe within the slurry return 92 via the airlift entry point. The tiny bubbles that are introduced at depth expand as they move up the slurry return line. The bubble expansion lowers the density in the slurry return line which causes a u-tube effect on the outside of the mining string, and fluid moves through an eductor bit opening 108 and into the mining pipe slurry return line. This suction recovers the slurry created by the quartic-straight jet nozzle 15 and the disaggregated ore.
[0049] The airlift assist line is typically placed at depth in a vertical well at a level to maximize the lift of slurry. This depth is adjusted according to the type of resource being mined. For instance, when mining Kimberlites, the depth of the airlift sub in the well is controlled closely to keep velocities of the resource lower to limit diamond breakage. For mining uranium, on the other hand, an example of ore where grain size after cutting is not monitored, the airlift housing is placed lower in the well to increase the tonnage/mining rate per hour. On horizontal wells the airlift release is generally within the vertical section of the well for lift, and the eductor pushes the cut ore through the horizontal section. Critical velocities are matched to each ore type and the direction of the well to ensure the slurry is maintained in suspension without erosion of the system. The airlift assist is a significant improvement over previous systems that only incorporate a fluid eductor for the recovery of the slurry, inasmuch as the airlift assist reduces the total amount of horsepower that is needed on location to drive the system. It is through this reduction of horsepower that a significant reduction of overall capital costs is attained, not only by eliminating an additional pump, but also by reducing the overall cost of the operating expenses as a result of the lower horsepower demands.
[0050] The second part of the slurry return system and a key element of the system and method of the present invention is the eductor bit 10 discussed above with reference to FIG. 2 . The eductor bit is operated with relatively low pressure and with a high volume stream of water. This water stream is selectively delivered through one of the concentric rings 94 , 96 in the mining pipe 5 . This water is delivered to the monitor pipe which houses the eductor assembly and turned 180 degrees via a conduit and directed back up the inner bore or slurry return line 92 of the mining string 5 . The water flow creates a suction that draws slurry into the educator and forces it up the hole.
[0051] The slurry passes through a narrower gauge 92 ′ of pipe within the eductor housing while being simultaneously boosted through that section of the eductor with the clean water from the surface via the outside concentric ring 94 . The acceleration of the fluids through the narrow section and then up the slightly larger inner bore of slurry return line 92 of the mining pipe causes a vortex and, effectively, a vacuum on the down hole side of the eductor. The two fluid streams converging in the narrow body of the eductor accelerate and then are released into the larger return pipe diameter. The differential pressure does not allow the fluid out the bottom of the bit, so it accelerates the flow up the well bore continuously. The slurry is then carried up the hole, through the swivel 22 and through and out of the swivel 22 , via aperture 130 where it is sent to the surface dewatering facility 26 via a slurry return pipe 50 ( FIG. 1 ).
[0052] Each resource type dictates the specific mining strategy utilized. The formation of the mined cavity can be by drilling a pilot ahead and through the resource body and starting at the bottom of the hole and mining up or back towards the rig in the case of a horizontal well, or starting at the top of resource body and utilizing the eductor bit of the present invention to drill and mine at the same time from the top down. The competency of the formation of the target resource and the geotechnical parameters surrounding it dictates the mining approach and strategy. In either direction, the cavity is developed through the disaggregation action of the hydraulic jet and the rotation of the mining string. The string is rotated at a preselected rotational speed, by a rotation apparatus operatively connected thereto, for example, an electrical motor coupled to the string via a gear mechanism or the like, the speed of rotation being determined by the competency of the formation and the distance or length of the cut at any given point within the resource body. The jet is rotated sufficiently slowly to allow enough effective interaction between the hydraulic jet and the rock face to perform the disaggregation and the slurrification of the resource. The rotational speed is determined by the amount of material that is returned and sent through the dewatering facilities. The time on the ore face coupled with the combination of flow and pressure is adjusted to maximize production. As the mining string is slowly rotated, a larger and larger cavity is created. This cavity in a vertical application can be a full 360 degree circle or pillars can be left in place to support the surrounding resource as the cavity is cut. As the returns diminish, the tool string is moved vertically and another rotational pass is made. This basic technique is continued until the desired cavity is cut from the targeted zone. Several times during the process, the mining string can be dropped to the bottom and the suction system can be used to remove any slurrified material that passed the mining string and fell to the bottom of the hole. Dependent on the resource being cut polymer can be added to the jet stream to increase the effective hydraulic horsepower at the ore face, which increases the cutting distance of the tool. The entire cutting process is repeated to enlarge the cavity. Upon completion of the cavity mining the entire mining string is removed from the borehole.
[0053] When the hydraulic borehole mining is performed in a high angle or horizontal application, the technique used to create the cavity can be different than that of the vertical application. In a horizontal application, the system of the instant invention is ideally drilled and directed to the bottom of the targeted resource. A pilot hole will be drilled from the surface to the bottom of the targeted resource body and then horizontally out as far as reasonably possible into the formation. on the depth of the horizontal hole depends upon the characteristics of the formation material. The hole will be drilled out as far as possible without collapsing on top of the tool string. The drilling string will be removed and replaced with the mining string of the present invention. The mining system will be run out in the lateral direction to the end of the hole. Thereafter, the jet will be turned on. In the horizontal application, the monitor pipe will be rotated no more than 180 degrees. Since the tool is on the bottom of the resource zone, the targeted areas will be to the side and the top of the monitor pipe. In thicker resource zones, one lateral well can be mined above the other. If the competency of the resource body is low, then the monitor pipe can be manipulated to perform 60-degree sweeps to either side of the tool, thereby making a bowtie pattern in the resource body. The advantage to this pattern in a low competency formation is that it permits recovery of the resource on the sides, which is facilitated by the natural subsidence of the formation over the mining string. As a section of the cavity is excavated, the mining string is slowly extracted, making the cavity larger and longer as the tool is retracted into the surface casing string. Upon completion of the cavity the mining system is removed from the hole.
[0054] Although the present invention has been described with reference to a particular embodiment thereof, it will be understood by those skilled in the art that modifications may be made without departing from the scope of the invention. Accordingly, all modifications and equivalents which are properly within the scope of the appended claims are included in the present invention. | A water jet borehole mining system controlled and operated aboveground includes a high-pressure cutting nozzle that is delivered to an underground resource body through a relatively small diameter borehole. A series of water and air streams at various pressures are delivered to the resource body, and the target resource is disaggregated and/or fluidized and conveyed back to surface via the water jet borehole mining pipe which serves as the conveyor of the system. The mining pipe is used to transport a high-pressure stream of water fluids that have been directed and aligned into laminar flow to a focused water jet cutting head. The central bore of the mining pipe brings the disaggregated and slurrified resource to the surface. The mining pipe transports the slurry via airlift, fluid eduction or a combination of both. | 4 |
TECHNICAL FIELD
[0001] The present disclosure relates generally to a device that retains curtains, draperies, or the like, in a desired orientation (such as, for example in a poufed orientation to create a bishop sleeve or simply in a tied back position) and methods for using the device.
BACKGROUND
[0002] Devices and accessories for drawing back curtains, draperies, or the like not only enable sunlight to enter a room but also may provide a decorative flair to the window treatment or decor of the room.
[0003] Simple holdback devices, such as a tie back, consist of a rope or similar device that is looped around the drape and tied to a wall mounted hook. While these devices provide the ability to adjust the amount the drape is drawn back, the tie back must ultimately be mounted to a wall, prohibiting portability and damaging the wall.
[0004] Therefore, a continuing need exists for an improved device and an improved method for retaining drapes in a desired configuration.
SUMMARY
[0005] The present disclosure is directed to an apparatus for retaining curtains. The apparatus includes a clip tethered to a retainer. The clip is capable of securing to a curtain. The retainer includes a bore for receiving a curtain therethrough.
[0006] In embodiments, the clip is retractably tethered to the retainer by a retractor. The retractor includes a housing and a retractable tether disposed within and extendable from the housing. The retractable tether is capable of being extended in a first direction and retracted in a second direction, and is biased in the second direction by a biasing element. In embodiments, the retractor includes a lock capable of maintaining the tether at a desired length when extended from the retractor.
[0007] In embodiments, the retainer is in mechanical cooperation with and end of the retractable tether and the clip disposed on an outer surface of the housing of the retractor. In other embodiments, the retainer is in mechanical cooperation with the housing of the retractor and the clip disposed on an end of the retractable tether.
[0008] In aspects of the present disclosure, the retainer is a toroid.
[0009] In embodiments, a decorative element is secured to the retainer.
[0010] In embodiments, the retainer includes first and second jaw members movable from a first open position to a second approximated position. In the approximated position, the first and second jaw members of the retainer form a bore through which a curtain may be received. The first and second jaw members of the retainer are rotatably affixed on a first end and capable of movement relative to each other. In embodiments, a second end of the first jaw member of the retainer is releasably coupled to a second end of the second jaw member of the retainer while first and second jaw members of the retainer are in an approximated position. In embodiments, a biasing element biases the first and second jaw members of the retainer toward the approximated position.
[0011] In embodiments, the retainer includes an elongate body having a first and second end. The retainer is affixed to an end of the retractable cord between the first and second ends of the elongate body. The first end of the elongate body is releasably coupled to the second end of the elongate body to define a bore through which a curtain can be placed. In embodiments, the first end of the elongate body is releasably coupled to the second end of the elongate body by at least one magnet or by hook and loop fastener.
[0012] A method for holding curtains provided in accordance with the present disclosure includes positioning a curtain through a bore defined through a retainer at a first location on a curtain, elevating the retainer to an elevated height that allows curtain material to billow over the retainer, and securing a clip that is tethered to the retainer to the curtain at a second location on the curtain vertically above the first location to maintain the retainer at the elevated height. In embodiments, the clip is retractably tethered to the retainer and the method further includes extending a retractable tether from a retractor housing, wherein the retractable tether is biased by a biasing element to pull the clip towards the retainer.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] The above and other aspects, features, and advantages of the present disclosure will become more apparent in light of the following detailed description when taken in conjunction with the accompanying drawings in which:
[0014] FIG. 1 illustrates an apparatus in accordance with the present disclosure;
[0015] FIGS. 2A, 2B and 2C illustrate the steps of a method of using an apparatus in accordance with the present disclosure;
[0016] FIG. 3 illustrates an apparatus in accordance with another embodiment of the present disclosure;
[0017] FIG. 4 illustrates the apparatus of FIG. 3 with the tether in an extended position;
[0018] FIG. 5 illustrates an apparatus in accordance with another embodiment of the present disclosure;
[0019] FIG. 6 is a perspective view of another apparatus for holding a curtain provided in accordance with the present disclosure shown in an open position;
[0020] FIG. 6A is a perspective view of the apparatus of FIG. 6 shown in an approximated position;
[0021] FIG. 7 is a perspective view of another apparatus for holding a curtain provided in accordance with the present disclosure shown in an open position;
[0022] FIG. 7A is a perspective view of the apparatus of FIG. 7 shown in an approximated position;
[0023] FIG. 8 illustrates an apparatus in accordance with another embodiment of the present disclosure;
[0024] FIG. 9 illustrates the apparatus of FIG. 8 installed on a curtain; and
[0025] FIGS. 10A, 10B, 10C, and 10D illustrate exemplary embodiments of decorative elements useful in connection with the embodiment of FIG. 8 .
DETAILED DESCRIPTION
[0026] Embodiments of the present disclosure are now described in detail with reference to the drawings in which like reference numerals designate identical or corresponding elements in each of the several views. In the drawings and in the description that follows, terms such as front, rear, upper, lower, top, bottom, and similar directional terms are used simply for convenience of description and are not intended to limit the disclosure. In the following description, well-known functions or constructions are not described in detail to avoid obscuring the present disclosure in unnecessary detail.
[0027] FIG. 1 illustrates a curtain holding device 10 provided in accordance with the present disclosure that generally includes a retainer 20 and a clip 40 tethered to retainer 20 by tether 50 . Retainer 20 includes a bore 21 defined therethrough. As illustrated in FIG. 1 , retainer 20 is generally shown as being toroidal, although other configurations are also contemplated, such as square, rectangular, or the like. Bore 21 is configured and/or dimensioned to enable a curtain “C” to be advanced therethrough. Retainer 20 can be made of any material, including metal, plastic, rubber, and the like. In embodiments, the material of construction from which retainer 20 is made will have sufficient frictional engagement with a curtain positioned through bore 21 to maintain retainer 20 at a desired position on the curtain.
[0028] Clip 40 may be any type of clip within the purview of those skilled in the art, such as, for example, any articulating clip, such as an alligator clip. As illustrated in the exemplary embodiment of FIG. 1 , clip 40 includes first and second jaw members 43 , 44 capable of movement relative to each other. A biasing element (not shown) biases first and second jaw members 43 , 44 toward a closed position.
[0029] Tether 50 can be a cord, yarn, string or narrow length of fabric. In embodiments, tether 50 is made of an elastic material, thereby biasing clip 40 toward retainer 20 when a curtain is positioned through bore 21 and clip 40 is attached to the curtain at a position remote from retainer 20 . The length of tether 50 is not critical, and can range, for example, from about 1 inch to about 30 inches, in other embodiments, from about 3 inches to about 20 inches, in yet other embodiments from about 6 inches to about 18 inches.
[0030] In operation, curtain holding device 10 retains a curtain in a desired configuration, such as, for example in a poufed orientation to create a bishop sleeve or simply in a tied back position. Initially, curtain “C” is positioned through bore 21 of retainer 20 at a first location on the curtain as shown in FIG. 2A . Retainer 20 is then elevated to an elevated height that allows curtain material to billow over the retainer as shown in FIG. 2B . Clip 40 is then secured to the curtain at a second location on the curtain vertically above the first location on the curtain to maintain retainer 20 at the elevated height via tether 50 as shown in FIG. 2C . As will be appreciated, when in place, retainer 20 is not visible beneath the billowed or poufed fabric of the curtain.
[0031] Turning now to FIGS. 3 and 4 , a curtain holding device 100 provided in accordance with another embodiment of the present disclosure generally includes a retainer 120 , a retractor 130 , and a clip 140 retractably tethered to retainer 120 by tether 150 . Retractor 130 can be any type of retractor within the purview of those skilled in the art, such as retractor reels of the type know for holding keys, badges and the like. Suitable retractor devices are disclosed, for example in U.S. Pat. Nos. 7,007,882, 6,290,158, 6,073,875, and 6,364,237, the entire disclosure of each of which is incorporated herein by this reference.
[0032] In embodiments, retractor 130 includes a ratchet mechanism so that the tether can be locked at a desired length when extended. Such retractable reels are typically lockable through a mechanism exerting some amount of force on the reel to prevent the tether from being retracted and therefore keep the tether at a desired length. Suitable lockable retractor devices are disclosed, for example in U.S. App. Pub. No. 2005/0011982 and U.S. Pat. Nos. 6,199,785; 6,019,304; 7,364,109, and 7,384,013, the entire disclosure of each of which is incorporated herein by this reference.
[0033] As illustrated in the exemplary embodiment of FIG. 3 , retractor 130 includes a housing 131 to which clip 140 is affixed. Although shown as being rigidly affixed to an outer surface of housing 131 , it is also contemplated that clip 140 may be affixed to an outer surface of housing 131 such that clip 140 is capable of swiveling 360 degrees about a center region of the outer surface of housing 131 .
[0034] Retainer 120 includes a lug 122 that is affixed to an outer surface thereof. As illustrated in FIG. 3 , lug 122 is integral to retainer 120 , although other configurations are also contemplated.
[0035] While not explicitly shown in the drawings, those skilled in the art will appreciate that the internal structure of retractor 130 includes a reel (not shown) rotatably supported within the interior of housing 131 and around which tether 150 can be wrapped. A biasing element (not shown) is affixed to housing 131 on a first end and to the reel (not shown) on a second end, thereby biasing the reel towards a direction that winds tether 150 about the reel. Tether 150 is secured on a first end to the reel (not shown) and may be any extended from and refracted back into housing 131 . End stop 136 is secured to a second end of tether 150 and is configured and/or dimensioned to prohibit tether 150 from being wound fully within housing 131 . A second end of end stop 136 includes a bore 137 defined through an upper and lower surface thereof. A ring 138 is advanced within bore 137 and is configured and/or dimensioned to engage lug 122 such that refractor 130 and retainer 120 are coupled.
[0036] In operation, curtain holding device 100 functions in the manner described above with respect to curtain holding device 10 to retain a curtain in a poufed configuration or in a tied back position. Initially, curtain “C” is positioned through bore 121 of retainer 120 at a first location on the curtain. Retainer 120 is then elevated to an elevated height that allows curtain material to billow over the retainer. Retractable tether 150 is then extended from retractor 130 and clip 140 is secured to the curtain at a second location on the curtain vertically above the first location on the curtain to maintain retainer 120 at the elevated height via retractable tether 150 .
[0037] In the alternative embodiment of curtain holding device 200 shown in FIG. 5 , retractor 230 is affixed to retainer 220 and clip 240 is secured to an end of retractable tether 250 . In operation, curtain holding device 200 functions in the manner described above with respect to curtain holding devices 10 , 100 to retain a curtain in a poufed configuration. Initially, curtain “C” is positioned through bore 221 of retainer 220 at a first location on the curtain. Retainer 220 is then elevated to an elevated height that allows curtain material to billow over the retainer. Retractable tether 250 is then extended from retractor 230 by pulling on clip 240 . Clip 240 is then secured to the curtain at a second location on the curtain vertically above the first location on the curtain to maintain retainer 220 at the elevated height via retractable tether 250 .
[0038] Another embodiment of a retainer 320 which can be used with any of curtain holding devices 10 , 100 , 200 is illustrated in FIGS. 6 and 6A . Retainer 320 includes first and second jaw members 301 , 302 capable of movement relative to each other. First and second jaw members 301 , 302 are rotatably affixed at a first end using any suitable means, such as a pin 304 . A second end includes a lock 303 thereby retaining first and second jaw members 301 , 302 in an approximated position. Lock 303 may be any suitable lock such as magnets, pins, hook and loop, etc.
[0039] In operation, a curtain holding device including retainer 320 functions in the manner described above with respect to curtain holding devices 10 , 100 , 200 to retain a curtain in a poufed configuration or in a tied back position. Retainer 320 is utilized by moving first and second jaw members 301 , 302 into an open position and while in the open position, first and second jaw members 301 , 302 are positioned around a curtain at a first position on the curtain. First and second jaw members 301 , 302 are then moved into an approximated position, to surround the curtain within bore 321 and locked in the approximated position. Retainer 320 is then elevated to an elevated height that allows curtain material to billow over the retainer. A tethered clip can then be used to secure retainer in the elevated height as described hereinabove.
[0040] Another embodiment of a retainer 420 which can be used with any of curtain holding devices 10 , 100 , 200 is illustrated in FIGS. 7 and 7A . Retainer 420 includes an elongate body 401 having first and second ends. Elongate body 401 may be constructed of any suitable material being having compliant properties, e.g., rope, fabric, composites, etc. Elongate body 401 is affixed to retractor 130 at a location between the first and second ends. A lock 403 is disposed on the first and second ends of elongate body 401 such that elongate body 401 may be locked into a loop defining a bore 421 capable of retaining a curtain therein. Lock 403 may be any suitable lock such as magnets, pins, hook and loop, etc. It is also contemplated that the first and second ends of elongate body 401 may be tied together, thereby locking elongate body into a loop including a bore 421 capable of retaining a curtain “C”, drape, or the like therein.
[0041] In operation, a curtain holding device including retainer 420 functions in the manner described above with respect to curtain holding devices 10 , 100 , 200 to retain a curtain in a poufed configuration or in a tied back position. Retainer 420 is utilized by wrapping elongate body 401 around a curtain at a first location on the curtain to surround the curtain within bore 421 and locked in this position using lock 403 . Retainer 420 is then elevated to an elevated height that allows curtain material to billow over the retainer. A tethered clip can then be used to secure retainer in the elevated height as described hereinabove.
[0042] In embodiments, the curtain holding device of the present disclosure includes a decorative element for aesthetically embellishing a curtain. As seen in the illustrative embodiment of FIG. 8 , curtain holding device 500 includes a retainer 520 and a clip 540 tethered to retainer 520 by tether 550 which is secured to lug 522 . Retainer 520 includes a bore 521 defined therethrough as in previous embodiments and decorative element 590 secured thereto.
[0043] Decorative element 590 can be secured to retainer 520 in any manner within the purview of those skilled in the art such as, for example, by the use of a magnet, adhesive, welding, hook and loop fastener, a loop of wire, or a mechanical fastener (e.g., a screw, tack, staple, or the like). Those skilled in the art will appreciate that certain securement techniques will allow the decorative element to be changed when desired, while other securement techniques will result in permanent attachment. In the exemplary embodiment shown in FIG. 8 , decorative element 590 is secured to retainer 520 using screw 560 , which allows for decorative element 590 to be removed (due to the accessibility of screw head 562 ) and replaced as desired.
[0044] Decorative element 590 may include a standoff 570 to create a space between retainer 520 and decorative element 590 to accommodate a curtain “C” therein, so that decorative element 590 is visible and provides an aesthetically pleasing embellishment to the curtain, while maintaining retainer 520 hidden from view when curtain holding device 500 is installed as shown in FIG. 9 .
[0045] Decorative element 590 may be made from any suitable material, such as textiles, plastics, metals, ceramics, or the like, or any combination of materials. In embodiments, the decorative element may include jewelry elements, such as decorative stones, for example diamonds, rhinestones, pearls, or the like, or a precious metal, for example, silver, gold, platinum, or the like.
[0046] Decorative element 590 may be of any desired, aesthetically pleasing design, such as may be achieved by a combination of any artistic features, such as shape, coloring, and/or texture. For example, the decorative element may be a disc which is adorned by a decorative motif or design on one side. An illustrative example of a domed, disc-shaped decorative element 590 A is shown in FIG. 10C . Alternatively, the decorative member may be in the shape of a flower, including but not limited to fabric flowers, plastic molded flowers, or even fresh flowers. An illustrative example of a flower decorative element 590 C is shown in FIG. 10C . An illustrative example of a decorative element 590 B in the form of holly as shown in FIG. 10B is especially useful in embodiments where the securement technique employed allows the decorative element to be changed seasonally or for holidays. Alternatively, the decorative member may be in the shape of an ornamental bow, such as, for example, a rosette bow, double loop rosette bow, bow and flower, tri-color rosette (requires three coordinating fabrics), or combinations and variations of the above-mentioned ornamental bows. An illustrative example of a decorative element 590 D in the form of a bow is shown in FIG. 10D . Those skilled in the art reading this disclosure will readily envision other aesthetically pleasing designs for decorative element 590 .
[0047] Persons skilled in the art will understand that the structures and methods specifically described herein and shown in the accompanying figures are non-limiting exemplary embodiments, and that the description, disclosure, and figures should be construed merely as exemplary of particular embodiments. It is to be understood, therefore, that the present disclosure is not limited to the precise embodiments described, and that various other changes and modifications may be effected by one skilled in the art without departing from the scope or spirit of the disclosure. Additionally, the elements and features shown or described in connection with certain embodiments may be combined with the elements and features of certain other embodiments without departing from the scope of the present disclosure, and that such modifications and variations are also included within the scope of the present disclosure. Accordingly, the subject matter of the present disclosure is not limited by what has been particularly shown and described. | An apparatus for holding curtains includes a retainer and a clip tethered to the retainer. The tether is optionally retractable by a retractor. A decorative element is optionally secured to the retainer. The present disclosure is directed to an apparatus for retaining curtains. The apparatus includes a clip tethered to a retainer. The clip is capable of securing to a curtain. The retainer includes a bore for receiving a curtain therethrough. | 0 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to inflatable air bags for use as an automobile passenger restraint in the event of an automobile collision. More particularly, a metal bladder is inflated by a gas generator when the automobile is struck with excessive force.
2. Description of the Related Art
Front mounted air bags that inflate in an automobile collision are mounted in the steering wheel column, the glove box or the dashboard of many motorized vehicles. In the event of a front end collision, the air bags are inflated by a gas and substantially fill that portion of the passenger compartment not occupied by the driver or a passenger. The combination of a seat belt and an air bag is effective to restrain an automobile passenger in the event of a front end collision, minimizing the likelihood of severe injury.
Front mounted air bags, while highly effective for front end collisions, are less effective for side impact collisions and collisions occurring at more than 30° from a front end collision. Accordingly, there is a need to provide automobiles with air bags effective to restrain a passenger in a side impact collision.
U.S. Pat. No. 5,308,112 to Hill et al discloses a fabric air bag for side impact collisions. The air bag is mounted within a door panel in an unfurled, deflated position. The unfurled bag deploys more quickly and provides more reliable orientation than air bags stored in a rolled, furled or coiled state.
U.S. Pat. No. 5,316,336 to Taguchi et al discloses a rubber or fabric air bag for providing passenger restraint in the event of a side impact collision. The air bag is mounted in a door panel above a gas generator. On impact, the bag is unfurled and extends laterally upward along the inside of the door. The orientation of the air bag relative to the gas generator provides more efficient use of generated gas and more rapid inflation of the air bag.
The rate of deployment of a fabric or rubber air bag is limited. These flexible fabric bags can not tolerate high inflation gas temperatures. At higher temperatures, the bag may burn exposing the passengers to hot gas.
Fabric air bags are also designed to vent gases into the vehicle interior. Therefore, the chemical composition of the gas generator used to inflate the air bag must be limited to compositions that generate non-toxic gases at relatively low temperature. The gas stream further may not contain excessive amounts of solid particles or flammable gases.
The flexibility of fabric air bags is a detriment. The air bags must be precisely folded or supported in a specific orientation to ensure rapid deployment. Over extended periods of time, as the automobile is subject to the bumps and centrifugal force of normal driving, it is possible for the flexible air bag to shift position and effective deployment of the air bag impaired.
Another method to protect the occupants in a collision is the use of energy absorbing structural components mounted in hollow sections of the automobile such as inside the door panel, under the hood or in the trunk adjacent to the bumper.
U.S. Pat. No. 3,888,502 discloses energy absorbing components for an automobile. Hollow drawn or spot welded tubes are filled with plastic beads and inserted into the walls of the automobile. The plastic beads absorb impact energy and cause a more uniform, controlled collapse of the hollow members.
U.S. Pat. No. 4,050,537 to Bez, discloses a hollow metallic member installed within an automobile wall. On impact, the hollow member is pressurized, typically by an explosive charge, deforming the walls of the hollow metallic member outward to increase resistance to buckling.
These structural elements, while effective, are of limited value. The polymer beads have a volumetric weight of 75-150 kg/m 3 and contribute undesirable weight to the automobile. Structural members that can withstand an explosion without bursting must be carefully designed and protected from corrosion, heat and other strength reducing conditions.
The above problems with both side impact air bags and internal structural members are solved by the use of an inflatable metal bladder. Inflatable metal bladders to disperse munitions have been disclosed in U.S. Pat. No. 5,107,767 to Schneider et al. However, that patent is oriented toward providing propulsive forces to propel munitions and does not suggest mechanisms under which metallic bladders may be used to restrain or otherwise protect an automobile passenger.
There remains a need for an air bag assembly utilizing an inflatable metal bladder that does not suffer from the problems of the prior art.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the invention to provide a metallic bladder that inflates in the event of an automobile collision. It is a feature of the invention that the metallic bladder is particularly suited as a side impact air bag, as an inflatable knee bolster to prevent lower leg injuries, as a structural member inserted within the automobile or as a bumper.
Among the advantages of the invention are that the inflatable metallic bladder is more robust than a fabric or rubber air bag and is not porous. The metallic bladder does not shift during operation of the automobile and is not likely to rupture. Since the metallic bladder is not porous, the constituents of the gas stream need not meet as strict toxicity standards as when a porous, fabric bag is employed. The result is a greater selection of energetic gas generating compounds may be employed.
Another advantage of the invention is that the metallic bladder is not flammable and high temperature gases may be used for inflation. The use of a high temperature gas permits faster deployment at higher gas pressure and reduces the mass of gas generating chemicals needed for inflation. This reduces the size and weight of the inflation mechanism.
In accordance with the invention, there is provided an air bag assembly for a motorized vehicle. This assembly includes an inflatable metal bladder and a gas generator. The gas generator generates a gaseous stream when the motor vehicle is struck with excessive force. A conduit directs the gaseous stream to the inflatable metal bladder.
The above mentioned objects, features and advantages, as well as others, will become more apparent from the specification and drawings that follow.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a metallic bladder in accordance with the present invention.
FIG. 2 shows in cross-sectional representation a first embodiment of the metallic bladder of FIG. 1.
FIG. 3 shows in cross-sectional representation a second embodiment of the metallic bladder of FIG. 1.
FIG. 4 illustrates a metallic bladder as a side impact air bag prior to deployment.
FIG. 5 illustrates the metallic bladder of FIG. 4 after deployment.
FIG. 6 shows a second embodiment of the metallic bladder as a side impact air bag prior to deployment.
FIG. 7 shows the air bag of FIG. 6 after deployment.
FIG. 8 shows a metallic bladder used as a knee bolster to reduce lower leg injuries and to assist in occupant positioning.
FIG. 9 shows an inflatable structural member mounted in an automobile door.
FIG. 10 shows in isometric view a second inflatable structural member.
FIG. 11 shows the use of a metallic bladder as an automobile bumper.
DETAILED DESCRIPTION
FIG. 1 shows in planar view a metallic bladder 10 in accordance with the invention. The metallic bladder 10 is formed from a thin sheet of metal capable of plastic deformation that melts at a temperature above 600° C. and preferably, the metal melts at a temperature in excess of 1000° C. The gas used to inflate the metallic bladder 10 may enter the bladder at temperatures of up to about 2200° C. (4000° F.). The low heat capacity of the gas combined with the excellent heat dissipating characteristics of the metallic bladder 10 prevents melting of the bladder.
Suitable materials for the metallic bladder 10 include copper, copper alloys such as brass (copper/zinc alloys), aluminum, aluminum alloys and various iron based alloys such as low and medium carbon steel and stainless steel. The sheets have a thickness of from about 0.1 millimeter to about 0.75 mm (0.004-0.030 inch). The preferred thickness is from about 0.15 mm to about 0.30 mm (0.006-0.012 inch).
Thicknesses below these minimums are difficult to resistance weld and result in delicate elements that are difficult to assemble and maintain within an automobile. Materials thicker than these maximums produce very stiff structures when inflated and do not provide optimum attenuation characteristics when in contact with the automobile occupants.
Where the inflatable metal bladders 10 are to be mounted external to the automobile to serve as stiffening members, such as internally pressurized front, rear and side bumpers, thicker sheets of metal are preferred to enhance robustness.
For corrosion resistance and ease of resistance welding, stainless steel is most preferred.
The metallic bladder 10 is formed into a desired shaped such as a disk or a rectangle. Using conventional metal shaping techniques, thin sheets of metal may be formed into complex shapes to match the contours of the automobile such as door interiors, door panels, dash boards, windshield headers, knee bolsters, etc. Apertures may be formed in the metal sheet for providing an ingress site 12 for the inflation gas or a vent hole 14.
With reference to both FIGS. 1 and 2, the metallic bladders 10 are formed by welding together a first 16 and a second 18 metal sheet. The edges of the sheets are most effectively joined by a melt down edge weld or machine rolling resistance weld 20. Welding is preferred over brazing, soldering and joining methods using an additional bonding agent. The edge joints are subject to peeling loads when the bladder is inflated. Bonding agents do not have the capacity to resist these peel loads. Also, bladder edge welds can be accomplished very rapidly when using machine resistance roll welders which result in economical bladder construction.
To enhance the volume occupied by the inflated bladder, one or both of the metal sheets may include a folded portion 22 as illustrated in FIG. 3. This portion may be folded accordion style or in any other easily opened pattern. Because the metal is more rigid than a fabric or rubber, the folded section 22 will not shift during normal operation of the automobile.
FIG. 4 illustrates the metallic bladder 10 as a side impact air bag. The first metal sheet 16 forms a portion of the panel 24 forming a car door 26. The surface 28 of the first metal sheet 16 exposed to the automobile occupant 30 may be exposed as decorative trim or covered with a fabric, leather or wood veneer.
Attached to the second metal sheet 18 is a gas generator 32. The gas generator produces a voluminous stream of gases when ignited. Typically, a sensor (not shown) mounted in the automobile sends an activating signal to an electric igniter when the automobile is struck at excessive force. Due to the low heat capacity of the gas generated by the gas generator and the excellent thermal dissipation capacity of the metal constituting the first metal sheet 16 and second metal sheet 18, an energetic compound such as nitrocellulose may be used in the gas generator 32.
When a nitrocellulose base gas generant is ignited, a large volume, about 4 moles of gas per gram, is generated. The gas is at an elevated temperature and inflates the bladder 10 in less than about 15 milliseconds. By optimizing the chemical composition and positioning of a conduit 34 that directs the gas stream to the metallic bladder 10, inflation times of under 5 milliseconds have been achieved.
Any gas generating chemical composition that generates a copious volume of gas in a few milliseconds may be employed. Typically, the gas stream generated is at an elevated temperature on the order of from about 600° C. to about 2200° C.
The metallic bladder 10 is much more resistant to tearing than a fabric or rubber air bag. The occupant 30 is not likely to be exposed to the gases generated by the gas generator 32. Since the gas is contained in a non-porous bladder, it is acceptable to employ gases that exceed previous exhaust toxicity levels. Flammable gas can also be considered in view of the enhanced containment.
The higher allowable temperature of the gas results in a lower mass of propellant gases being required to inflate the metallic bladder, minimizing the size of the gas generator 32 and simplifying construction. The gas generator 32 does not require cooling screens or other devices to reduce the inflation temperature of the gas. Reducing the size of the inflator, limits the interference of the metallic bladder 10 with operation of the automobile window 36, door handle 38 or linkages 40 that actuate these components.
FIG. 5 illustrates the metallic bladder 10' after inflation. The metallic bladder 10' extends inward into the passenger compartment forming a restraining surface for the occupant 30. For use as a side impact air bag, an inflation pressure of from about 5 psig to about 50 psig and preferably from about 10 psig to about 40 psig is used.
FIG. 6 illustrates the metallic bladder 10 mounted behind the panel 24 in a second embodiment of the invention. With this embodiment, the automobile manufacturer does not have to change the outline of the panel 24. The first metal sheet 16 is bonded to the panel 24 by any suitable means such as by welding, brazing, soldering or bolting. The gas generator 32 is actuated when the automobile is impacted with sufficient force to inflate the separation 42 between the first metal sheet 16 and second metal sheet 18.
As illustrated in FIG. 7, when the metallic bladder 10' is deployed, the panel 24 is distorted. The panel is usually coated with a decorative trim such as leather or fabric that restrains the occupant 30. This embodiment likely results in destruction of the car door 26 and damage to the linkage 40. However, the car doors are usually damaged in a side impact collision so this damage is tolerable.
In FIG. 8, the metallic bladder 10 is mounted underneath a dash board 44 and is either integral with a padded knee bolster 45 or disposed behind the padded knee bolster. The metallic bladder 10 is rapidly inflated in a collision. The inflated knee bolster 10' offers improved energy absorption. The under dash knee bolster inflates more rapidly, typically in from about 3 to about 10 milliseconds, than the driver or passenger front mounted air bag 49 and the automobile passenger is prevented from submarining under the front mounted air bag 49.
The occupant's legs are more rigid than the occupant's sides, so the gas generator 32 delivers a higher inflation pressure to the separation 42 than utilized in the side impact metallic bladder described above. Preferably, the inflation pressure to deploy the air bag 10' is from about 20 psig to about 150 psig and more preferably from about 25 psig to about 75 psig.
FIG. 9 illustrates another application of the inflatable metallic bladders of the invention. The metallic bladder 10 is a hollow beam that may be formed by conventional tube drawing or by welding as illustrated in FIG. 10. The hollow beam is easily stored within the confines of an automobile door 26 and does not interfere with the door and window operation. The hollow beam 10 is light weight and does not significantly contribute to the overall weight of the automobile. The uninflated hollow beam 10 does not provide significant lateral stiffness. However, when the hollow beam is deployed to an internally pressurized tubular structure, it affords considerable strength addition to the door.
While the door interior and exterior may be deformed and the window and door linkages displaced or destroyed during inflation of the hollow beam, these elements would have probably been ruined by a side impact event anyway. The rapid inflation of the internally pressurized hollow beam assists in deceleration of the object striking the automobile and increases the stiffness of the automobile door, both effects contribute to minimize the likelihood of occupant harm during the collision.
A conventional air bag generator (not shown) is connected to the hollow beam 10 through a conduit. For maximum stiffness, the air bag preferably generates a pressure within the separation 42 of from about 2000 psig to about 5000 psig.
FIG. 11, the metallic bladder 10 forms the bumper of an automobile 46. On impact, the metallic bladder 10 inflates to the position 10' with the separation 42 pressurized to at least 2000 psig and preferably from about 5000 psig to about 10,000 psig. Inflation of the metallic bladder 10' decelerates the object striking the automobile 46 and provides cushioning, minimizing the impact of the collision.
While the metallic bladders of the invention have been described in reference to automobiles, they are useful restraint devices for other types of motorized vehicles as well. Such other motorized vehicles include, but are not limited to planes, boats and trucks.
It is apparent that there has been provided in accordance with this invention an inflatable metallic bladder that fully satisfies the objects, means and advantages set forth hereinbefore. While the invention has been described in combination with specific embodiments thereof. It is evident that many alternatives, modifications and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, it is intended to embrace all such alternatives, modifications and variations as fall within the spirit and broad scope of the appended claims. | There is disclosed a metallic bladder that is inflated by a gaseous stream generated by a gas generator. The inflatable metallic bladder is useful as a side impact air bag for motorized vehicles. The heat dissipating capability of the metallic bladder permits the use of energetic chemical compositions that generate a high temperature gas and very rapidly inflate the metallic bladder. The heat conducted by the gas is dissipated by the metallic bladder avoiding harm to occupants. | 1 |
This application is a divisional of application Ser. No. 09/388,727, filed Sep. 2, 1999, now U.S. Pat. No. 6,359,314, status allowed.
BACKGROUND OF THE INVENTION
1. Technical Field
The present invention relates generally to semiconductor integrated circuit processing, and in particular to electrostatic discharge protection for semiconductor device. Still more particularly, the present invention relates to a method and apparatus for providing electrostatic discharge protection in complimentary metal oxide semiconductor integrated circuits.
2. Description of the Related Art
An electrostatic discharge is basically more or less a sudden violent redistribution of electrons between bodies, such that in their new special equilibrium position, the electrons end up as far away from each other as they could possibly get. The charges always position themselves outside the skin of a conductive body because of the repulsion between the charges.
Whenever movement occurs, a static charge may be produced. Electrostatic discharge (ESD) is caused by the rapid flow of charge between two objects. Voltages as low as 200 volts can damage the vices. Typically, a person feels ESD at greater than 3,000 volts. ESD may cause gate oxide breakdown, junction spiking, and latch-up in various integrated circuit devices.
It has been shown that voltage potentials up to 28 kV can be generated and discharged in less than 10 nanosecond through an IC device when handled by a person. Electrostatic charge can also be accumulated on pin of the lead frame of a packaged IC device during shipping, storage or while being integrated into an electronic system which is discharged when another pin is grounded. The discharge of the high electrostatic voltage can result in a current of about two amperes. The high current must flow through the IC device when another pin or pad is grounded. MOS devices are particularly susceptible to discharge of the electrostatic charge because the thin gate oxide can be easily ruptured by the voltage induced by the high current.
ESD events can and do happen to semiconductor devices during normal handling or operating procedures associated with transportation, manufacturing, and testing. A device, which suffers from damage, may fail to operate correctly.
CMOS integrated circuit devices are vulnerable to electrostatic discharge (ESD) induced failure. ESD events or spikes are typically short-duration, high-voltage electrical pulses that are caused, for example, by discharge of a static charge. ESD causes failure of a MOS integrated circuit device by overheating components due to overcurrent, breakdown of thin oxide, or other conditions. ESD can damage or destroy integrated circuit devices unless measures are taken to reduce ESD effects on the input pins and output pins of the devices. Various techniques have been used to self-protect output buffers or other input-output nodes against ESD failures. Some of these measures include diode clamps, lateral punch-through devices, and guard ring collectors around and input-output bonding pad. These circuits are reasonably effective for protecting input circuits, but are less effective for protecting output circuits from high transient voltages.
These internal ESD structures are employed typically to bypass over-voltage events to either a power supply voltage, such as VCC, or a lower power supply voltage, such as VSS, or ground. Metal oxide semiconductor (MOS) and complimentary metal oxide semiconductor (CMOS) devices within gate oxides are particularly susceptible to ESD events.
All integrated circuit (IC) devices are sensitive to ESD to some degree. However, as IC devices are made smaller, ESD damage is more likely to occur and render the device inoperable in response to an ESD event. Particularly susceptible are MOS and CMOS devices with thin gate oxides.
The need for ESD protection in IC devices that can handle the high current produced by an ESD event has been recognized for many years. However, it is typical that ESD protection circuits are designed to provide protection against electrostatic charge levels of between 500 volts to 3.0 kilovolts because once the IC device has been inserted into a system, the need for ESD protection is minimized since most such systems generally incorporate sophisticated ESD protection. However, prior to insertion, IC devices are particularly vulnerable to ESD pulses applied to the IC device's pins or pads.
As CMOS integrated circuits are scaled to thinner oxides, the input/output (I/O) circuitry is becoming more sensitive to ESD. Salicided source/drain defusions tend to further aggravate this ESD sensitivity as output transistors have less series resistance to limit the current through any given cross section of the device.
As the output data path transistors, transistors actually involved in chip-to-chip data transmission, become more and more ESD sensitive, it is increasingly common to deploy a dummy device of some sort to discharge ESD pulse. The intent is to alleviate all ESD-driven constraints on the output transistor by having a separate element disperse the charge in the ESD pulse.
One problem with this approach is finding an ESD protection element, which will always trigger before the data path transistor. Numerous elements have been employed including metal oxide semiconductor field effect transistors (MOSFETs), silicon controlled rectifiers (SCRs), zener diodes, and bipolar devices. In almost every case, additional process steps are required to ensure that the protection device has a lower breakdown or trigger voltage compared with the data path transistor. The additional process steps increase the time and increase the complexity of manufacturing integrated circuits.
Therefore, it would be advantageous to have an improved method for manufacturing an ESD protection element that does not require additional process steps to set a lower breakdown voltage compared to that of a data path transistor.
SUMMARY OF THE INVENTION
The present invention provides a method and apparatus for manufacturing an electrostatic discharge protection device. A first gate structure and a second gate structure are formed for the electrostatic device and a data path transistor. A first lightly doped drain and a second lightly doped drain is formed for the electrostatic discharge protection device. A third lightly doped drain and a fourth lightly doped drain is formed for a data path transistor, wherein the first lightly doped drain and the second lightly doped drain have a higher doping level relative to the third lightly doped drain and the fourth lightly doped drain.
BRIEF DESCRIPTION OF THE DRAWINGS
The novel features believed characteristic of the invention are set forth in the appended claims. The invention itself however, as well as a preferred mode of use, further objects and advantages thereof, will best be understood by reference to the following detailed description of an illustrative embodiment when read in conjunction with the accompanying drawings, wherein:
FIG. 1 is a diagram of an electrostatic discharge (ESD) protection circuit in accordance with a preferred embodiment of the present invention;
FIGS. 2A-2D are cross-sections illustrating a process for manufacturing an electrostatic protection device used with high voltage devices in accordance with a preferred embodiment of the present invention;
FIGS. 3A-3D are cross-sections illustrating the process used in creating a electrostatic device used with a low voltage data path transistor in accordance with a preferred embodiment of the present invention;
FIG. 4 is a planer view of an electrostatic discharge protection system for use in I/O buffers in accordance with a preferred embodiment of the present invention; and
FIG. 5 is a table illustrating the changes in masks used to process ESD and data path transistors in accordance with a preferred embodiment of the present invention.
DETAILED DESCRIPTION
The process steps and structures described below do not form a complete process flow for manufacturing integrated circuits. The present invention can be practiced in conjunction with integrated circuit fabrication techniques currently used in the art, and only so much of the commonly practiced process steps are included as are necessary for an understanding of the present invention. The figures representing cross-sections of portions of an integrated circuit during fabrication are not drawn to scale, but instead are drawn so as to illustrate the important features of the invention.
With reference now to FIG. 1, a diagram of an electrostatic discharge (ESD) protection circuit is depicted in accordance with a preferred embodiment of the present invention. Circuit 100 is part of a data path between chips for data transmission. Bonding pad 102 is an output pad in the depicted example and is connected to transistors 104 and 106 . Transistor 104 is a p-channel metal oxide semiconductor (MOS) transistor while transistor 106 is an n-channel metal oxide semiconductor (NMOS) transistor. In this example, the source of transistor 104 is connected to an upper power supply voltage, VCC, with the source of transistor 106 being connected to a lower power supply voltage, VSS. The drain of transistors 104 and 106 are connected to each other and bonding pad 102 . Data is transmitted to bonding pad 102 via signals controlled by the gates of transistors 104 and 106 . Transistor 108 is an ESD device employed to disperse the charge in the ESD pulse. In accordance with a preferred embodiment of the present invention, this element, transistor 108 , is designed to always trigger before a data path transistor. Transistors 104 and 106 are data path transistors. Transistor 108 is a NMOS transistor having a drain tied to bonding pad 102 and its source connected to lower power supply voltage, VSS. In addition, the gate of transistor 108 also is connected to lower power supply voltage, VSS.
The present invention provides an improved ESD protection device that may be created without adding additional process steps to ensure that the protect device has a lower breakdown voltage compared with the data path transistor. In particular, the present invention provides this advantage by adjusting the mask artwork to “swap” lightly doped drains (LDDs) and to create two additional device types. In one case, a low voltage device with a thin oxide is created with a relatively low LDD dose. In another case, a high voltage device is created with a thick oxide, but a relatively high LDD dose. Whether one of the two additional devices is used as a protect transistor, such as to prove ESD protection or as a data path transistor, depends on whether the data path transistor is a high voltage element or a low voltage element. In the depicted example, a high voltage element is a transistor operating at 3.3-volts or more while low voltage elements operating at 2.5-volts or less.
In the situation in which data path transistor 106 is a high voltage element, transistor 108 , the protect device is adjusted to a non-standard device. The mask artwork used to create transistors is modified such that transistor 108 has a thick gate oxide. In other words, the gate oxide of transistor 108 is thicker relative to transistors for core logic devices. Core logic devices are devices located within the integrated circuit that are not part of the I/O buffers. In addition, transistor 108 will have a high LDD doping, which would normally go into a low voltage transistor. Further, other common techniques may be employed in conjunction to help transistor 108 trigger first with respect to triggering of transistors 104 and 106 . These techniques may include remote p-well ties, gate-to-drain coupling, resistance in series with the gate, modified gate length, and salicide-block such that transistor 108 triggers non-destructively. Transistor 106 is fabricated as a standard high voltage data path transistor. In other words, transistor 106 will have a thick gate oxide and reduced LDD doping. This doping is reduced relative to the transistors in the core logic devices of the integrated circuit.
In the case where the data path transistor, such as transistor 106 , is a low voltage element, the data path transistor is adjusted to a non-standard device in accordance with a preferred embodiment of the present invention. In such a situation, the mask artwork for transistor 106 is modified to have a thin gate oxide, but with a LDD, which would normally go into a high voltage transistor. In this case, transistor 106 is a low voltage data path transistor. Such a change will effect the electrical properties by ten percent or more, requiring new models. With a low voltage system, transistor 108 is a low voltage protect device that is kept standard. For example, transistor 108 will have a thin gate oxide and a higher doped n type LDD (NLDD). In these examples, the LDD implants are NLDD implants. In addition, other common techniques may be employed to help transistor 108 trigger prior to the data path transistor, transistor 106 . For example, removing p-well ties, gate-to-drain coupling, resistance in series with the gate, and salicide block may be used so that transistor 108 triggers non-destructively.
In this manner with swapped LDDs, a highly effective protect device may be created, which will trigger before the data path devices. This advantage is provided by adjustment of mask artwork to swap LDDs between low voltage and high voltage devices to create effective ESD protection devices.
With reference now to FIGS. 2A-2D, cross-sections illustrating a process for manufacturing an electrostatic protection device used with high voltage devices is depicted in accordance with a preferred embodiment of the present invention. In this example, a high voltage device is considered a device operating at 3.3 volts or greater. In FIG. 2A, substrate 200 is a silicon substrate. Depending on the implementation, substrate 200 also may be made of other materials or combinations of materials, such as a silicon on illustrator (SOI) substrate. Field oxide regions 202 , 204 , and 206 have been formed in an area of substrate 200 to separate active areas within substrate 200 . These field oxide regions are formed through thermal oxidation in the depicted examples. Also shown in FIG. 2A are gate structures 208 , 210 , 214 , 216 , and 218 . Gate structure 208 includes a polysilicon layer 220 over a gate oxide layer 222 . Gate structure 208 is the gate structure for an ESD transistor device and is about 70 angstroms thick and is designed to operate at high voltages, such as 3.3 volts. Similarly, gate structure 210 is a gate structure for a data path transistor, such as transistor 106 in FIG. 1 . Gate structure 210 includes a polysilicon layer 224 and a gate oxide layer 226 , which are about 70 angstroms thick. Gate structures 214 , 216 , and 218 have polysilicon layers 228 , 232 , 236 , and gate oxide layers 230 , 234 , and 238 , respectively. These gate structures are about 50 angstroms thick and form gate structures for transistors for high performance core logic devices. These devices are designed to operate at 2.5 volts in the depicted example. As mentioned before, core logic devices are devices other than those used in the I/O buffers.
A photoresist layer 240 in FIG. 2B is deposited on substrate 200 and patterned and etched to form an opening in section 242 . In the depicted example, the device in section 242 is a NMOS transistor, such as transistor 108 in FIG. 1 . Photoresist layer 240 has a thickness of about 7000 angstroms. Photoresist layer 240 may range in thickness from about 5000 angstroms to about 11000 angstroms. Thereafter, an n-type LDD (NLDD) implant is performed. In this example, the LDD implant is made using a dose having concentration of about 1E13 cm −3 to about 1E14 cm −3 for a high voltage LDD. The implant energy for this implant is typically from about 25 keV to about 75 keV. The dopant typically used is either phosphorus or arsenic for this step.
Normally, section 244 would also receive the implant because it is a 70 angstrom, 3.3 volt device. The doses and implant energies described in these examples are those for low voltage devices having a voltage of 2.5 volts and for high voltage devices operating at 3.3 volts. If other voltages are used, different doses and implant energies may be used depending on the actual voltages and depending on the line widths. In accordance with a preferred embodiment of the present invention, section 244 remains part of a low voltage LDD covered with photoresist layer 240 to prevent high voltage LDD doping from occurring in section 244 . The device in section 244 is a NMOS data path transistor, such as transistor 106 in FIG. 1 . In this example, the core logic devices also are blocked from receiving this high voltage LDD implant. This doping is illustrated in FIG. 2 B. High performance core logic devices are found in section 246 in FIG. 2 B. The LDD implant of an N type does not form NLDD regions 248 and 250 .
Thereafter, a LDD implant is made for the core logic devices, which are low voltage high performance devices in this example. This LDD implant is accomplished by depositing photoresist layer 252 in FIG. 2C prior to implantation.
The photoresist layer shown in FIG. 2C has been patterned and etched to leave photoresist layer 252 in section 242 while sections 244 and 246 remain exposed for the LDD implant. The photoresist thicknesses for this process are similar to those for the used and the high voltage LDD implant. Thereafter, a LDD implant is performed to form LDD regions 254 , 256 , 258 , 260 , 262 , and 264 . The concentration of the implant for a low voltage LDD implant is from about 6E13 cm −3 to about 4E13 cm −3 using an energy from about 10 keV to about 50 keV. In this example, the dopant used would be arsenic. Further, a implant, also referred to as a “halo” or “pocket” implant may be performed. This type of implant involves implanting the opposite type of species into the device. For example, boron or a BF 2 implant may be made at moderate doses, such as about 1E12 cm −3 to about 5E12 cm −3 . The dose may be at a higher energy than that of the low voltage LDD implant or the implant may be at a tilt angle. This type of implant further shallows the LDD by cutting off the bottom of the junction.
Normally, the device in section 244 would not receive this LDD implant because it is a 70 angstrom, 3.3 volt device as opposed to the core logic devices, which are 50 angstrom, 2.5 volt devices. In accordance with a preferred embodiment of the present invention, however, the device in section 244 receives this reduced LDD doping. In this manner, the ESD protection device formed in section 242 will trigger prior to the data path device in section 244 .
Thereafter, oxide spacers 266 - 284 are formed for the various devices along with source/drain implants to form source/drains 286 - 299 as shown in FIG. 2 D. As a result, the device in section 244 is a 70 angstrom, 3.3 volt device with a NLDD for a 2.5 volt device.
With reference now to FIGS. 3A-3D, cross-sections illustrating the process used in creating a electrostatic device used with a low voltage data path transistor is depicted in accordance with a preferred embodiment of the present invention. In FIG. 3A, substrate 300 is a silicon substrate. Depending on the implementation, substrate 300 also may be made of other materials or combinations of materials, such as a silicon on illustrator (SOI) substrate. Field oxide regions 302 , 304 , and 306 have been formed in an area of substrate 300 to separate active areas within substrate 300 . These field oxide regions are formed through thermal oxidation in the depicted examples. Also shown in FIG. 3A are gate structures 308 , 310 , 314 , 316 , and 318 . Gate structure 308 includes a polysilicon layer 320 over a gate oxide layer 322 . Gate structure 308 is the gate structure for an ESD transistor device and is about 50 angstroms thick and is designed to operate at high voltages, such as 2.5 volts. Similarly, gate structure 310 is a gate structure for a data path transistor, such as transistor 106 in FIG. 1 . Gate structure 310 includes a polysilicon layer 324 and a gate oxide layer 326 , which are about 50 angstroms thick. Gate structure 314 , 316 , and 318 have polysilicon layers 328 , 332 , 336 , and gate oxide layers 330 , 334 , and 338 , respectively. These gate structures are about 50 angstroms thick and form gate structures for transistors for high performance core logic devices. These devices are designed to operate at 2.5 volts in the depicted example. As mentioned before, core logic devices are devices other than those used in the I/O buffers.
A photoresist layer 340 in FIG. 3B is deposited on substrate 300 and patterned and etched to form an opening in section 342 . In the depicted example, the device in section 342 is a NMOS transistor, such as transistor 108 in FIG. 1 . Photoresist layer 340 has a thickness of about 7000 angstroms. Photoresist layer 340 may range in thickness from about 5000 angstroms to about 5000 angstroms. Thereafter, a high voltage LDD implant is performed. Thereafter, an n-type LDD (NLDD) implant is performed. In this example, the LDD implant is made using a dose having concentration of about 1E13 cm −3 to about 1E14 cm −3 for a high voltage LDD. The implant energy for this implant is typically from about 25 keV to about 75 keV. The dopant typically used is either phosphorus or arsenic for this step.
The device in section 342 normally would not receive this LDD implant because it is a low voltage I/O device. Section 342 receives the implant to raise the snap back voltage. When a drain of an n-channel transistor breaks down, the voltage collapses to a low value. This effect is called a “snap back”. The drain voltage required to trigger the n-channel transistor is the snap back voltage and the voltage that the transistor drops down to or holds at is the snap back hold voltage.
In accordance with a preferred embodiment of the present invention, sections 344 and 346 remain covered with photoresist layer 340 . The device in section 344 is a NMOS data path transistor, such as transistor 106 in FIG. 1 . High performance core logic devices are found in section 346 in FIG. 3 B.
A low voltage high performance LDD doping is performed for sections 344 and 346 in FIG. 3 C. The LDD implant using N type dopants forms NLDD regions 348 and 350 . The concentration of the implant for a low voltage LDD implant is from about 6E13 cm −3 to about 4E13 cm −3 using an energy from about 10 keV to about 50 keV. In this example, the dopant used would be arsenic. Further, a implant, also referred to as a “halo” or “pocket” implant may be performed. This type of implant involves implanting the opposite type of species into the device. For example, boron or a BF 2 implant may be made at moderate doses, such as about 1E12 cm −3 to about 5E12 cm −3 . The dose may be at a higher energy than that of the low voltage LDD implant or the implant may be at a tilt angle. This type of implant further shallows the LDD by cutting off the bottom of the junction. Thereafter, an LDD implant is made for the core logic devices, which are low voltage high performance devices in this example. This LDD implant is accomplished by depositing photoresist layer 352 in FIG. 3 C.
The photoresist layer shown in FIG. 3C has been patterned and etched to leave photoresist layer 352 in section 342 while sections 344 and 346 remain exposed for the LDD implant, which is a low voltage high performance LDD implant. Thereafter, an LDD implant is performed to form LDD regions 354 , 356 , 358 , 360 , 362 , and 364 . In accordance with a preferred embodiment of the present invention, however, the device in section 342 does not receive this reduced LDD doping. In this manner, the ESD protection device formed in section 342 will trigger prior to the data path device in section 344 .
Thereafter, oxide spacers 366 - 384 are formed for the various devices along with source/drain implants to form source/drains 386 - 399 as shown in FIG. 3 D. As a result, the data path device in section 342 is a 50 angstrom, 2.5 volt device.
With reference now to FIG. 4, a planer view of an electrostatic discharge protection system for use in I/O buffers is depicted in accordance with a preferred embodiment of the present invention. In FIG. 4, substrate 400 contains pads 402 , 404 , and 406 . In this example, an electrostatic device 408 is connected to pad 404 along with inverter 410 , which includes data path transistor 412 and 414 . Data path transistor 412 is a PMOS transistor while data path transistor 414 is a NMOS transistor. Data path transistor 412 includes a source 418 and a drain 420 . Source 418 is connected to upper power supply voltage VDD. Data path transistor 414 includes a source 420 and a drain 422 in which source 420 is connected to a lower power supply voltage VSS. Drain 420 of data path transistor 412 and drain 422 of data path transistor 414 are tied together to pad 404 . Data path transistors 412 and 414 have a common gate 424 , which is connected to an input.
ESD device 408 has a drain region 426 , a source region 428 , and a gate region 430 . Source region 428 and gate region 430 are tied to lower power supply voltage VSS while drain region 426 is connected to pad 404 . In the depicted example, changes to the mask artwork in creating these devices is made in order to swap the LDD implants to provide for triggering of the ESD device prior to the data path transistor without increasing the number of processing steps. When high voltage devices are used for data path transistors, the masks for LDD implants are altered for the area indicated by dotted line 432 , such that the ESD device receives the LDD implant used with core logic devices rather than the normal LDD implant used with high voltage devices. In this manner, the ESD device receives the high LDD doping, which is normally used in a low voltage transistor, such as those found in core logic devices operating at 2.5 volts. This LDD doping is higher than the high voltage devices used in the data path transistors operating at 3.3 volts. In this manner, the ESD device will trigger prior to the data path transistor. With respect to using low voltage elements in the data path, the region indicated by dotted line 434 has alterations in the mask artwork such that data path transistor 414 receives the LDD doping normally used with high voltage devices. The ESD device and the core logic devices received the normal low voltage LDD dopings. In this manner, the snap back voltage is raised for the data path transistor.
With reference now to FIG. 5, a table illustrating the changes in masks used to process ESD and data path transistors is depicted in accordance with a preferred embodiment of the present invention. As can be seen in table 500 , both the ESD device and the data path transistor both receive a low NLDD doping when low voltage devices are used in the data path transistors. In accordance with a preferred embodiment of the present invention, the masks are altered such that the data path transistor receives a high voltage NLDD doping while the ESD device still receives the low voltage NLDD doping. As a result, the ESD device receives a heavier implantation and triggers prior to the data path transistor. When high voltage devices are used in the data path transistors, the masks normally both result in the ESD device and the data path transistor having high voltage NLDD dopings. In accordance with a preferred embodiment of the present invention, the masks are altered such that the ESD device receives a low voltage NLDD doping while the data path transistor still receives a high voltage NLDD doping. As a result, the ESD transistor will trigger prior to the data path transistor.
The description of the preferred embodiment of the present invention has been presented for purposes of illustration and description, but is not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiment was chosen and described in order to best explain the principles of the invention and the practical application to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated. | A method and apparatus for manufacturing an electrostatic discharge protection device. A first gate structure for the electrostatic device is formed. A first lightly doped drain and a second lightly doped drain for the electrostatic discharge protection device is formed. A second gate structure for a data path transistor is formed. A third lightly doped drain and a fourth lightly doped drain for a data path transistor is formed, wherein the first lightly doped drain and the second lightly doped drain have a higher doping level relative to the third lightly doped drain and the fourth lightly doped drain. | 7 |
TECHNICAL FIELD
The invention relates to the general class of welders known as stud welders. In stud welding, the parts to be welded are brought into engagement, followed by a slight lifting of the upper electrode to create a small gap between the parts and draw an arc thereacross, whereafter the parts are driven into reengagement, and weld together.
BACKGROUND
Stud welders are known in the art. An upper electrode holds a part which is lowered to engage another part on a lower electrode, and then lifted by an energized magnetic coil to start an arc between the parts, followed by spring biased driving force pushing the upper electrode downwardly such that the parts reengage and weld together. Another type of stud welder uses spring bounce to start the arc. In both types of stud welders, the follow-up force is provided by a compression spring.
A disadvantage of prior stud welders is their inability to weld certain materials, for example brass. It has been found that after the arc-starting lift, the follow-up is too slow, and that the arc begins to disintegrate the brass into zinc fumes before the arc is extinguished by reengagement of the parts. The zinc fumes may inhibit the arc, and when the parts come together there may not be a weld formed.
The present invention provides in combination a magnetic booster coil for supplying additional and faster follow-up force driving the upper electrode downwardly after the arc-starting lift. This faster follow-up enables the welding of materials such as brass which were not weldable with prior stud welders.
Magnetic follow-up is itself known, and has been used in welding systems other than stud welding. For example, percussion welding commonly uses magnetic follow-up force to provide the percussive blow to drive the parts together. However, in percussion welding the arc is not started by lifting the weld head. Instead an arc-starter or nib is provided on one of the parts, and when the parts are brought together a high current is passed through the arc-starter nib causing it to explode and start the arc across the gap between the parts. This requires 50,000 to 100,000 amps, and an exemplary application is the welding of contacts of diameter 0.4-1.125 inch. In contrast, stud welders typically require only 2,000 to 4,000 amps, and an exemplary application is the welding of contacts of 0.1-0.375 inch diameter. Unlike percussion welders, stud welders draw the arc by means of weld head lift, which in turn entails particular structural requirements.
For a further discussion highlighting the differences between stud welding and percussion welding, reference is made to my U.S. Pat. No. 4,162,388. For further reference regarding stud welding, reference is made to the commercially available Nelson NSA-80 stud welder, Instruction and Maintenance Manual dated November, 1970, TRW Nelson Division, 28th Street and Toledo Ave., Lorain, OH 44055. For further background regarding percussion welding, reference is made to: "Percussion Welding" R. F. Manning and J. B. Welch, Welding Journal, Sept. 1960, pgs. 1-5; "Percussion Welding" Metals Handbook, 8th Edition, Vol. 6, Welding and Brazing, pgs. 177-186, prepared under the direction of the ASM Handbook Committee, American Society for Metals, Metals Park, OH., 1971; and "Percussion Welding", Welding Handbook, 6th Edition, Sec. 2, Chap. 27, edited by Arthur L. Phillips, published by American Welding Society, N.Y., 1969. For further background regarding various magnetic follow-up systems reference is made to Welch U.S. Pat. Nos. 2,769,080 and 2,776,362, and Park et al U.S. Pat. No. 2,892,068.
SUMMARY
The present invention provides in a stud welder a magnetic follow-up system in combination with an arc-drawing lift system. The invention further provides the magnetic follow-up system in addition to and in cooperation with spring biased follow-up force.
The invention further provides various structural improvements in stud welder construction, including the incorporation of a magnetic booster coil in cooperative relation with both a magnetic lift coil and a subsequent spring biased follow-up means.
In preferred form, a magnetic lift coil is rigidly secured to a vertically reciprocal mounting plate, and a magnetic follow-up booster coil is secured to the plate coaxially above the lift coil. Two piece shaft means includes a vertically reciprocal lower shaft in the lift coil and a vertically reciprocal upper shaft in the follow-up booster coil. At the bottom of the lower shaft is the upper electrode holding a part to be welded. The upper and lower shafts move down with the mounting plate until the upper electrode part engages the part on the lower electrode. The mounting plate continues to move downwardly, which in turn causes the lower shaft to move upwardly within the lift coil, and which also compresses a pressure spring.
Nonmagnetic guide pin means is mounted between the lower and upper shafts in lost motion relation, such that as the mounting plate moves downwardly after engagement of the parts, the lower shaft moves upwardly within the lift coil but the upper shaft remains stationary within the follow-up booster coil. After downward movement of the mounting plate is halted, the lift coil is energized, which raises the lower shaft and starts an arc in the gap created between the parts. This energized lift of the lower shaft also raises the upper shaft within the follow-up booster coil by means of the guide pin whose lost motion has been traveled through and taken up. Energization of the follow-up booster coil drives the upper shaft, the guide pin and the lower shaft downwardly in engagement without lost motion, and in combination with the pressure spring, to extinguish the arc and weld the parts together.
In one desirable aspect of the invention, there is enabled selective energization timing of the follow-up booster coil to afford flexibility for various applications and materials. For example, the invention enables one particularly advantageous implementation in which the follow-up booster coil is energized before deenergization of the lift coil. This eliminates any delay which might otherwise be caused during build-up of driving forces and instead applies charged magnetic follow-up force immediately upon release by the lift coil. This is particularly desirable in applications where fast follow-up is needed to drive the parts into engagement before disintegration to fumes which may otherwise inhibit the arc and the welding of the parts.
In another desirable aspect of the invention, a double bearing system is provided which prevents wobble and tilt of the weld head, which has been a problem in prior stud welders. Wobble and tilt of the welding head becomes more pronounced with age, and adversely affects reliability.
The invention further relates to improvements in the electrical control system for stud welders in combination with magnetic follow-up. The system enables variable selective control of both the timing and the amount of lift force and of follow-up force.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a pictorial illustration of a stud welder constructed in accordance with the invention.
FIG. 2 is a sectional view of the welder of FIG. 1.
FIG. 3 is a sectional view like FIG. 2 illustrating operation of the welder.
FIG. 4 is a sectional view like FIG. 2 further showing operation of the welder.
FIG. 5 is a schematic circuit diagram showing the electric control circuitry for the welder.
DETAILED DESCRIPTION
Referring to FIGS. 1 and 2, a stud welder 2 has an upper electrode 4 holding a part 6 which is lowered to engage another part 8 on a lower electrode 10 and then lifted by an energized magnetic coil 12 to start an arc in the gap created between the parts. Follow-up force provided by pressure spring 14 and magnetic booster coil 16 drive the upper electrode downwardly such that parts 6 and 8 reengage and weld together.
Lift coil 12 and follow-up booster coil 16 are rigidly mounted in coaxial relation on a vertically reciprocal mounting plate 18 by means of U-shaped clamps 20 and 22 which are fixedly secured at their distal ends to mounting plate 18 and have set screws such as 24 to be tightened against the respective coil extending therethrough. A nonmagnetic spacer plate 26, FIG. 2, is between the coils. Axial shaft means 28 extends vertically within the coils. A two piece shaft is provided comprising a lower shaft 30 in the lift coil and an upper shaft 32 in the booster coil, and further including nonmagnetic guide pin 34 mounted between the shafts in lost motion relation.
Upper shaft 32 extends freely through an upper bearing 36 rigidly secured to mounting plate 18. Upper shaft 32 extends downwardly through a nonmagnetic brass bushing 38 of a steel backing plate 40 rigidly secured to the top of booster coil 16. Upper shaft 32 extends down within the core of coil 16 and has a downwardly opening cavity 42 into which guide pin 34 upwardly extends. Upper shaft 32 is free to move vertically, and its downward limit of movement is set by engagement of its lower lip 44 with divider plate 26.
Guide pin 34 is preferably brass, and extends vertically freely through aperture 46 in divider plate 26. In FIG. 2, pin 34 resets at its bottom end 48 in an upwardly opening notch or cavity 50 of lower shaft 30. The upper end 52 of pin 34 extends partially into cavity 42 of upper shaft 32 and leaves a small gap to the top edge 54 of such cavity.
Lower shaft 30 extends downwardly out of the core of lift coil 12. A lift armature plate 56 is fixedly secured to lower shaft 30 by pin 58. A spring-stop plate 60 is fixedly secured to mounting plate 18, and has an aperture 62 through which lower shaft 30 extends. Another spring-stop plate 64 is fixedly secured to shaft 30 by pin 66. Compression pressure spring 14 is coaxially disposed around lower shaft 30 and bears between spring-stops 60 and 64. Lower shaft 30 extends further downwardly through a lower bearing plate 68 rigidly secured to mounting plate 18. The lower end of lower shaft 30 includes an electrical connection terminal 70 and upper electrode 4. Lower shaft 30 is freely vertically reciprocal in lift coil 12 and its upward movement is limited by engagement of armature plate 56 against the bottom of coil 12.
In operation, mounting plate 18 is lowered to effect engagement of parts 6 and 8, for example by means of slide system 72 and air cylinder 74, FIG. 1. Shaft means 28 moves down with mounting plate 18 until upper electrode part 6 engages lower electrode part 8. Continued downward movement of mounting plate 18 causes lower shaft 30 to move relatively upwardly within lift coil 12, compressing spring 14 between spring-stops 60 and 64, FIG. 3. This upward movement of lower shaft 30 also raises guide pin 34 upwardly to travel through the remainder of cavity 42 and take up the lost motion up to top edge 54 of such cavity in the upper shaft 32. Continued downward movement of mounting plate 18 then causes relative upward movement of upper shaft 32 within booster coil 16. The downward movement of mounting plate 18 is stopped when adjustable stop screw 76, FIG. 1, hits stop plate 78.
At the bottom of the travel stroke of mounting plate 18, adjustable trip screw 80 on bracket 82, mounted to slide system 72, trips a microswitch 84, FIG. 1. As more fully described hereinafter, the electrical control system then passes current through parts 6 and 8 between the upper and lower electrodes, and also energizes lift coil 12 to attract armature 56. This raises armature 56 into engagement with the bottom of lift coil 12, FIG. 4, which lifts lower shaft 30 and electrode 4 to start an arc in the gap created between parts 6 and 8. In the preferred implementation, the gap is between 0.020 and 0.100 inch. This arc-starting lift also raises upper shaft 32 within coil 16, and further compresses spring 14. A charge from a large capacitor through an inductor is placed across the mini-arc causing a large arc, to be described.
Deenergization of lift coil 12 releases lift armature 56 to permit downward movement of lower shaft 30. Energization of booster coil 16 applies a magnetic force on upper shaft 32, driving the latter downwardly. This magnetic follow-up force is transmitted through guide pin 34 without lost motion to lower shaft 30 in addition to the spring biased follow-up force from compressed pressure spring 14. Part 6 is thus driven into reengagement with part 8 to extinguish the arc and weld the parts together.
FIG. 5 schematically shows the electric control circuitry for the welder. It is an advantage of the invention that it may be powered from a 110 volt, 60 hertz line, as shown at 102. Disconnect switches 104 and 106 are provided for safety. In operation, capacitor 108 is charged by rectifier diode 110 through protective resistor 112 through normally closed palm button switches 114 and 116 from isolation transformer 118. The operator actuates switches 114 and 116 by depressing the palm buttons, which opens the charging circuit through the upper sets of contacts and closes the circuit through the lower sets of contacts of switches 114 and 116, putting the charge of capacitor 108 across relay coil 120, which closes relay contacts 120a. This allows current to flow through normally closed relay contacts 122a then through relay contacts 120a then through the coil of relay 122, thus energizing relay 122 to close relay contacts 122b and maintain a closed circuit through relay 122. Contacts 120a open when the charging pulse from capacitor 108 is depleted.
Energization of relay 122 further closes relay contacts 122c which completes a circuit through the solenoid valve 124 of air cylinder 74, whereby slide system 72 and mounting plate 18 move downwardly as shown in FIG. 3 and stop when screw 76 hits stop plate 78, FIG. 1. Upper electrode part 6 engages lower electrode part 8, and lower shaft 30 moves upwardly relative to coil 12 and mounting plate 18 as above described. When mounting plate 18 is at the bottom of its travel stroke, screw 80, FIG. 1, trips microswitch 84.
Referring to FIG. 5, actuation of microswitch 84 provides a high signal to the reset input of a counter 126. The high state from microswitch 84 is thus inverted low to disable the reset function, such that counter 126 is incremented by oscillator 128. The output of counter 126, designated A, is delivered to a comparator 130. A thumbwheel switch 132 provides the other input, designated B, to comparator 130. The output of comparator 130 is high when B is greater than A. The operator selects a given number for B through thumbwheel switch 132. An AND gate 134 has one input from comparator 130 and another input from microswitch 84. Upon actuation of microswitch 84, both inputs to AND gate 134 are high, whereby the output of AND gate 134 goes high and drives transistor 136 into conduction, which completes a circuit through lift coil 12 to energize the latter and provide the arc-starting lift for axial shaft means 28 and electrode 4, FIG. 4. Coil voltage is supplied through a diode rectifier bridge 138 and smoothing capacitor 140, and is selectable according to the setting of variac 142. Coil voltage is preferably 80+ volts. When the incremented contents A of counter 126 becomes greater than B, the output of comparator 130 goes low, whereby the output of AND gate 134 goes low and transistor 136 turns off, deenergizing lift coil 12.
The incremented contents A from counter 126 is also applied to another comparator 144. The other input C to comparator 144 is from a thumbwheel switch 146. Initially, A is less than C and the output of comparator 144 is low. When the incremented value A becomes greater than C, the output of comparator 144 goes high which turns on transistor 148, to close a circuit through follow-up booster coil 16, energizing the latter to provide the magnetic follow-up force described above. This coil voltage is also supplied from the power source provided by bridge 138, capacitor 140 and variac 142.
Voltage for electrodes 4 and 10 is supplied by a capacitor bank 150 which is charged through normally closed switch 152, diode rectifier bridge 154 and protective resistor 156, and returned through normally closed switch 158 and adjusted by variac 160. When energization of lift coil 12 lifts shaft system 28, the voltage from capacitor bank 150 and inductor 162 establishes a mini-arc between parts 6 and 8 due to a restricted current through bypass resistor 164. After this mini-arc is established, the full charge of capacitor band 150 through inductor 162 is applied to the electrodes by firing SCR 166. This results in a large arc between parts 6 and 8 which spreads over their facing surfaces, causing thin surface layer melting. Upon energization of follow-up coil 16 and deenergization of lift coil 12, parts 6 and 8 with their molten facing surface layers are pushed together by pressure spring 14 with an additional assist and acceleration from the magnetic follow-up force. The arc is quenched and the weld is made when the molten surfaces solidify, usually within about one millisecond.
The timing of the firing of SCR 166 into conduction is coordinated with the timing of energization of coils 12 and 16. The incremented contents A from counter 126 is delivered to a third comparator 168. The other input D to comparator 168 is selectable by the operator according to thumbwheel switch 170. When A is incremented to a value greater than D, the output of comparator 168 goes high, which triggers SCR 166 into conduction.
In preferred form, the numbers B, C, and D are chosen such that lift coil 12 is initially energized, followed by a given delay for stabilization of the arc, followed by firing of SCR 166, followed by energization of follow-up coil 16, followed by deenergization of lift coil 12. In this implementation, B>C>D. Energization of follow-up coil 16 just prior to deenergization of lift coil 12 enables charged magnetic follow-up force to be immediately applied upon release by lift coil 12, without an inherent delay for build-up of magnetic force. This faster application of downward acceleration provides faster reengagement of the parts, which is particularly desirable in the welding of certain materials. For example, in the welding of brass, the parts are reengaged before disintegration to zinc fumes which may otherwise inhibit the arc and the welding of the parts. The timing flexibility and programmability afforded by the control, including operator set thumbwheel switches 132, 146 and 170, readily facilitates the desired coordination of components in a particularly easy manner.
After completion of the weld, relay 122 may be deenergized by manual switch means, or by timed relay contacts 122a which open after a given delay. This delay must expire after completion of the weld, but is otherwise not critical relative to the coordinated timing between comparators 130, 144 and 168. In response to deenergization of relay 122, contacts 122c open, which in turn deenergizes air solenoid valve 124, whereby slide system 72 and mounting plate 18 move upwardly. In response to this upward movement, screw 80 disengages microswitch 84 and the output of the latter goes low. The low state from microswitch 84 is inverted at the reset input of counter 126 to a high state, thus providing a continuous reset signal to the counter, which in turn prevents incrementation, whereby the contents A stays at zero. The low state from microswitch 84 insures that the output of AND gate 134 will be low and keep lift coil 12 deenergized. Since the contents A is now zero, the outputs of comparators 144 and 168 go low, deenergizing coil 16 and removing gate drive from SCR 166. To prepare for the next welding operation, normally closed switch 172 is opened, which deenergizes relay 174, which in turn closes normally closed contacts 152 and 158 to charge capacitor bank 150. Before slide system 72 and mounting plate 18 start down again, switch 172 is closed to energize relay 174 and open relay contacts 152 and 158.
It is recognized that various modifications are possible within the scope of the appended claims. | A stud welder is provided with a pair of magnetic coils and a compression spring. One of the coils provides the lift to separate electrode held parts and start an arc therebetween. The other coil and the compression spring provide fast follow-up force driving the parts into reengagement to quench the arc and weld the parts together. The combined acceleration of the spring and the booster coil enables the welding of certain materials such as brass which were previously not weldable with stud welders. | 1 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is based upon and claims the benefit of priority from the prior Japanese Patent Application No. 2000-216271, filed Jul. 17, 2000, the entire contents of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relate to a computer system using a fuel cell assembly as a power supply and, more particularly, to a personal computer using a fuel cell assembly of type which directly oxidizes methanol.
2. Description of the Related Art
Various personal computers using a fuel cell assembly have been devised. In a conventional personal computer using a fuel cell assembly, the fuel cell assembly is set in the personal computer main body.
Such a personal computer is disclosed in, e.g., Jpn. Pat. Appln. KOKAI Publication No. 9-213359. The fuel cell assembly disclosed in Jpn. Pat. Appln. KOKAI Publication No. 9-213359 uses a hydrogen-absorbing metal.
A fuel cell assembly inevitably produces water. This water is normally vaporized using heat generated in the computer. In some cases, however, the vapor liquefies in the housing of the personal computer under various environmental conditions. A design for preventing the water from entering the personal computer conflicts required conditions for heat dissipation, ventilation, and the like.
That is, in the conventional personal computer, the fuel cell assembly is set in the personal computer, and when water produced from the fuel cell assembly enters the personal computer, the personal computer malfunctions.
In addition to a fuel cell assembly with a hydrogen storage unit using a hydrogen-absorbing alloy, a DMFC (Direct Method Fuel Cell) has been devised. Such a DMFC is disclosed in, e.g., Japanese Patent Application No. 10-278759 filed by the present applicant. The DMFC does not require so-called auxiliary equipment for pumping fuel and hence has no movable mechanical portion. For this reason, the DMFC is readily made compact and lightweight and therefore is suitable as a power supply of a notebook personal computer.
If, however, a DMFC is designed not to have a stacked cell structure so as to manufacture the cell at a low cost, air supplied to the cell relies on diffusion and convection. As a consequence, to supply power required for a current notebook PC, the DMFC has an excessively large area. Even if the performance of a DMFC improves to, for example, 45 mW/cm 2 , the cell needs to have an area of 1,000 cm 2 to supply 45 W.
The biggest merit in using a fuel cell assembly for a portable apparatus is that the apparatus can be used substantially unlimited time period in the AC power less embodiment, as long as a fuel is carried. When the fuel cell assembly is used, it is required to restrict a performance and function of the personal computer.
While being out as long as a fuel is carried. However, the power that can be extracted from the fuel cell assembly is limited. If a high priority is to be given to the long-term use of a personal computer even at the expense of performance, the personal computer needs to be operated with a great restriction on power consumption. However, present notebook PCs are not designed to operate on the power that can be extracted from a fuel cell assembly.
Many current notebook personal computers are designed assuming, as a main power supply, an Li ion cell charged using a dedicated AC adapter. In this case, for the viewpoint of efficiency and the like, it is supposed to be optimum to design a secondary cell with a terminal voltage of about 10V by connecting three cells in series in a battery pack.
The cell output voltage of a fuel cell assembly is about 0.5V in operation. A fuel cell assembly having a number of cells stacked (this type is hard to manufacture and be inexpensive) is generally designed to obtain such an output voltage, though it is expensive and difficult to use.
For cost reduction, a personal computer operable by a low-level voltage, which can easily be obtained by segmenting a grid into a plurality of portions in an integrated fuel cell assembly and connecting those portions in series, is necessary.
However, with the low power obtained by such a fuel cell assembly, the conventional computer system cannot normally operate when a power-consuming application is executed.
BRIEF SUMMARY OF THE INVENTION
The present invention has been made in consideration of the above situation, and has as its object to provide a computer system in which water produced from a fuel cell assembly is prevented from entering the computer.
It is another object of the present invention to provide a computer system which can be normally operated even by a low output obtained from a fuel cell assembly.
In order to achieve the above objects, according to the first aspect of the present invention, there is provided a computer system comprising a power input terminal which is provided outside a personal computer, and an external fuel cell assembly connected to the power input terminal.
According to this aspect, by externally connecting the fuel cell assembly to the personal computer, water produced from the fuel cell assembly can be prevented from entering the personal computer to result in malfunction of the personal computer.
According to the second aspect of the present invention, there is provided a personal computer comprising means for determining whether a power supply is a fuel cell assembly on the basis of a received power supply output, means for, when it is determined that the power supply is the fuel cell assembly, switching an operation mode to a fuel cell assembly mode in which the fuel cell assembly is used as the power supply.
According to this aspect, when it is determined that the power supply is the fuel cell assembly, the operation mode of the personal computer is switched to the fuel cell assembly mode in which the fuel cell assembly is used as the power supply. Hence, even when the output level of the fuel cell assembly is low, the personal computer can normally operate.
Additional objects and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objects and advantages of the invention may be realized and obtained by means of the instrumentalities and combinations particularly pointed out hereinafter.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate presently embodiments of the invention, and together with the general description given above and the detailed description of the embodiments given below, serve to explain the principles of the invention.
FIG. 1 is a view showing a notebook personal computer system according to the first embodiment of the present invention;
FIG. 2 is a block diagram showing the arrangement of the notebook personal computer;
FIG. 3 is a flow chart for explaining the operation of the power supply microcomputer of the notebook personal computer;
FIG. 4 is a flow chart for explaining the first example of the fuel cell assembly mode;
FIG. 5 is a flow chart for explaining the second example of the fuel cell assembly mode;
FIG. 6 is a flow chart for explaining the third example of the fuel cell assembly mode;
FIG. 7 is a block diagram showing the arrangement of a notebook personal computer according to the second embodiment of the present invention;
FIG. 8 is a flow chart for explaining the operation of the power supply microcomputer;
FIG. 9 is a chart for explaining mode switching;
FIG. 10 is a view showing the interface between the fuel cell assembly and the personal computer;
FIG. 11 is a graph showing the output characteristics of the fuel cell assembly when it is assumed that the personal computer is powered on after the output voltage of the fuel cell assembly sufficiently rises;
FIG. 12 is a circuit diagram showing the power supply section of the notebook personal computer of this embodiment;
FIG. 13 is a graph showing the output characteristics of the fuel cell assembly of the notebook personal computer of this embodiment; and
FIG. 14 is a circuit diagram showing another example of the power supply section of the notebook personal computer of this embodiment.
DETAILED DESCRIPTION OF THE INVENTION
The embodiments of the present invention will be described below with reference to the accompanying drawing.
<First Embodiment>
FIG. 1 is a view showing a notebook personal computer system according to the first embodiment of the present invention.
Referring to FIG. 1 , reference numeral 1 denotes a notebook personal computer; 2 , a fuel cell assembly; 3 , a support of the fuel cell assembly 2 ; and 4 , a power supply line for supplying the power from the fuel cell assembly 2 to the notebook personal computer 1 .
As shown in FIG. 1 , the fuel cell assembly 2 is externally connected to the notebook personal computer 1 through the power supply line 4 . With this arrangement, the user can process water as needed in accordance with the environmental conditions for use of the notebook personal computer 1 . In addition, since the notebook personal computer 1 need no special measure against water the notebook personal computer 1 itself can be prevented from becoming expensive.
The power supply of the notebook personal computer 1 is not limited to the fuel cell assembly 2 . The notebook personal computer 1 can have a large power supply capacity by an internal Li cell and receive power from an AC adapter 5 .
In this case, the high-speed/high-level operation using power of several ten W is possible as ever. On the other hand, when the fuel cell assembly 2 is used, the notebook personal computer 1 operates in a dedicated fuel cell assembly mode capable of executing only application programs other than some especially power-consuming application programs by a method to be described below.
FIG. 2 is a block diagram showing the arrangement of the notebook personal computer. The same reference numerals as in FIG. 1 denote the same parts in FIG. 2 , and a detailed description thereof will be omitted.
As shown in FIG. 2 , either the fuel cell assembly 2 or AC adapter 5 can be connected to a power input connector 10 of the notebook personal computer 1 . The power input from the power input connector 10 is converted into a voltage appropriate to each part of the notebook personal computer 1 by a power supply section 11 and supplied to each part of the notebook personal computer 1 .
The power supply section 11 charges a battery pack 12 or receives power from the battery pack 12 .
One of the power supply destinations of the power supply section 11 is a main board 13 . The main board 13 has a CPU 14 . As examples of peripheral devices connected to the main board 13 , a modem 15 and DVD player/recorder 16 are illustrated in FIG. 2 .
The CPU 14 controls the entire notebook personal computer 1 . The modem 15 communicates with another computer through a communication line. The DVD player/recorder 16 plays back sound and image recorded on a DVD or records sound and image on a DVD.
The power supply section 11 incorporates a DC/DC converter, power supply microcomputer, and cell charge/discharge control IC as ever. Even when the notebook personal computer 1 is kept OFF, the power supply microcomputer is operating by receiving low power so as to monitor such an event that the power switch of the notebook personal computer 1 is turned on, or power is supplied to the power input connector 10 , as ever.
One of characteristic features of the notebook personal computer of this embodiment is the operation of the power supply microcomputer of the power supply section 11 .
As a characteristic feature of the operation of the power supply microcomputer of the notebook personal computer according to this embodiment, after the power input start event, the input power supply voltage is monitored, and the subsequent operation mode of the notebook personal computer is determined in accordance with the power supply voltage.
The operation of the power supply microcomputer of the notebook personal computer according to this embodiment will be described below with reference to the flow chart shown in FIG. 3 .
First, the power supply microcomputer determines whether the AC adapter is connected (S 1 ). If YES in step S 1 , a normal mode for executing conventional operation is set (S 2 ).
If NO in step S 1 , it is determined whether the fuel cell assembly is connected (S 3 ). If YES in step S 3 , the mode shifts to a fuel cell assembly mode (S 4 ).
If NO in step S 3 , the flow returns to processing in step S 1 . Whether the AC adapter is connected or whether the fuel cell assembly is connected is determined on the basis of the input power supply voltage.
That is, when the AC adapter is connected, a power of about 15V is input as ever. When the fuel cell assembly 2 is connected, a power of only several V (about 2V as a typical value in operation) is input.
For the former case, the power supply microcomputer sets the normal mode for executing conventional operation. For the latter case, the power supply microcomputer sets the fuel cell assembly mode. Since the operation mode is automatically set in accordance with the type of power supply, any mode setting error by user's operation error can be prevented.
When neither power supplies are connected at the time of activation, the internal cell is used as the main power supply. This case is slightly complex and will be described later in the second embodiment.
The fuel cell assembly mode will be described next in detail.
In the fuel cell assembly mode, the power consumption of the notebook personal computer 1 in operation is reduced such that the notebook personal computer 1 can operate on the basis of the power supplied from the fuel cell assembly 2 .
Several methods of reducing power consumption are available. Typical examples will be described. Any other method may be used as far as it can reduce power consumption, or some of the methods to be described below may be combined.
In the first example, when the fuel cell assembly mode is set, the CPU is set in a low power consumption mode (S 11 ), as shown in FIG. 4 . Operating the power supply section 11 in the low power consumption mode is a well-known technique, and a detailed description thereof will be omitted here. In this fuel cell assembly mode, since the power consumption must be largely reduced as compared to the normal mode, the low power consumption mode is set in the following way.
Recent CPUs are designed with an emphasis mainly placed on power consumption reduction in high-speed operation, so the power supply voltage of the core in the CPU chip is made as low as possible.
This increases the leakage current of the transistor. In the fuel cell assembly mode wherein the clock speed is considerably reduced, the power supply voltage of the core is made slightly higher than that in the normal mode. Hence, the power consumption can be reduced. Conventionally, the power consumption is reduced by dropping the power supply voltage of the core.
The CPU architecture also preferably has the low power consumption mode. For example, to increase the degree of parallel processing, a recent CPU obtains a result as if a plurality of instructions designated for serial execution on the program were executed in parallel and the results were serially output without any inconsistency. In the fuel cell assembly mode, the power consumption is preferably reduced by a design for simply serially executing commands without supplying the power to a circuit for such parallel processing.
In the second example, applications, which cannot be executed in the fuel cell assembly mode or are inappropriate to execute in the fuel cell assembly mode, are not executed.
More specifically, as shown in FIG. 5 , the user designates in advance applications which cannot be executed in the fuel cell assembly mode or are inappropriate to execute in the fuel cell assembly mode (S 12 ).
In this case, the user designates the applications in advance. However, the applications may be automatically detected by software or designated in advance at the time of shipment from a factory. The designated applications are disabled to inhibit the start (S 13 ).
In this embodiment, traditional office applications (e.g., WORD available from Microsoft) and Internet accesses using the modem 15 can operate (moving image or music application cannot operate, as described above). These applications can be practically executed even by a CPU with considerably low performance and are also determined as applications whose needs for long-time use outdoor are high.
In the third example, some peripheral devices are not activated.
More specifically, as shown in FIG. 6 , some peripheral devices are disabled (S 21 ). In this embodiment, the DVD player/recorder 16 is not activated in the fuel cell assembly mode. This is because the DVD player/recorder 16 itself requires high power consumption, and a moving image as a main application that uses the DVD player/recorder 16 requires full use of CPU performance and therefore real-time processing cannot be executed by the CPU in the low power consumption mode.
In the fuel cell assembly mode, the battery pack 12 is not charged or discharged (is not used as a power supply). This is because, in the fuel cell assembly mode, the battery pack 12 is unreliable, and the user must properly understand this point. As another reason, inefficient operation of charging the cell by the low voltage of the fuel cell assembly must be prevented.
Switching between the fuel cell assembly mode and the normal mode is done only when the notebook personal computer is kept OFF. This facilitates switching to the low power consumption mode at the CPU architecture level and is also important in preventing operation error by the user.
That is, connection of the fuel cell assembly to the notebook personal computer that is operating in the normal mode is inhibited. In this embodiment, a warning message is displayed in the window, and the operation in the normal mode is continued. With this arrangement, the fuel cell assembly mode can be clearly interpreted, and discrepancy between the user's expectation and the operation of the notebook personal computer 1 can be prevented.
<Second Embodiment>
The second embodiment of the present invention will be described next.
FIG. 7 is a block diagram showing the arrangement of a notebook personal computer according to the second embodiment of the present invention. The same reference numerals as in FIG. 2 denote the same parts in FIG. 7 , and a detailed description thereof will be omitted. Only different parts will be described here.
As a characteristic feature of this embodiment, a power input connector 17 dedicated to the fuel cell assembly and an electric double-layered capacitor 18 are added.
A power input connector 10 of a notebook personal computer 1 is connected to an AC adapter 5 . The notebook personal computer 1 has the power input connector 17 dedicated to the fuel cell assembly and is connected to a fuel cell assembly 2 .
Both the AC adapter 5 and fuel cell assembly 2 are connected to a power supply section 11 . The power is converted into a voltage appropriate to each part of the notebook personal computer 1 by the power supply section 11 and supplied to each part of the notebook personal computer 1 .
The power supply section 11 is connected to a battery pack 12 so as to be able to charge the battery pack 12 or receive power from the battery pack 12 and supply the power to each part of the notebook personal computer 1 as shown, as described above.
One of the power supply destinations of the power supply section 11 is a main board 13 of the notebook personal computer 1 . The main board 13 has a CPU 14 . As examples of peripheral devices connected to the main board 13 , a modem 15 , DVD player/recorder 16 , and hard disk drive 19 are illustrated in FIG. 7 .
The operation of the power supply section in receiving power from the AC adapter 5 or receiving power from the battery pack is basically the same as the conventional operation. The power supply section 11 incorporates a DC/DC converter, power supply microcomputer, and cell charge/discharge control IC as ever. Operation performed when the power is supplied from the fuel cell assembly 2 is largely different from the conventional operation.
That is, the power supply voltage input from the AC adapter is about 15V as a typical value. For the fuel cell assembly of this embodiment, a power of only several V (about 2V as a typical value in operation) is input.
Hence, the dedicated connector 17 is used to connect the fuel cell assembly, and a dedicated DC/DC converter is prepared. The power supply microcomputer operates while clearly distinguishing between a normal mode for the conventional operation and a fuel cell assembly mode wherein the power is supplied from the fuel cell assembly.
While the notebook personal computer 1 is kept OFF, the power supply microcomputer identifies which power supply terminal starts power supply and automatically sets the operation mode. Hence, any mode setting error by user's operation error can be prevented.
More specifically, as shown in FIG. 8 , first, it is determined whether power is supplied from the power input connector 10 (S 25 ). If YES in step S 25 , the mode shifts to the normal mode (S 26 ).
If NO in step S 25 , it is determined whether the power is supplied from the power input connector 17 dedicated to the fuel cell assembly (S 27 ).
If YES in step S 27 , the mode shifts to the fuel cell assembly mode (S 28 ). If NO in step S 27 , the flow returns to processing in step S 25 .
Detailed processing including a case wherein the internal cell is used as a main power supply will be described later with reference to FIG. 9 . The fuel cell assembly mode has been described in the first embodiment, and a repetitive description thereof will be omitted.
Switching between the fuel cell assembly mode and the normal mode is done only when the notebook personal computer 1 is kept OFF. This facilitates switching to the low power consumption mode at the CPU architecture level and is also important in preventing operation error by the user.
That is, connection of the fuel cell assembly to the notebook personal computer that is operating in the normal mode is inhibited. In this embodiment, when the fuel cell assembly is connected to the notebook personal computer that is operating in the normal mode, a warning message is displayed in the window, and the operation in the normal mode is continued.
With this arrangement, the fuel cell assembly mode can be clearly interpreted, and discrepancy between the user's expectation and the operation of the notebook personal computer 1 can be prevented.
FIG. 9 is a chart for explaining mode switching of the notebook personal computer according to this embodiment. More specifically, this is implemented as the firmware of the power supply microcomputer in this embodiment.
A state 40 is the initial state. The overall power supply control of the conventional notebook personal computer is indicated by a frame 44 . In this case, the power ON sequence in a state 41 , the operation sequence in a state 42 , and the power OFF sequence in a state 43 are shown.
The state 40 is the conventional OFF state. Each processing sequence starts in accordance with an event “power SW is turned on”, “AC adapter is connected”, “resume condition is satisfied”, or “Wake On LAN condition is satisfied”.
A series of processes executed when the power switch is turned on are indicated as the states 41 to 43 .
The state 40 is the only neutral state in which transit between the fuel cell assembly mode and the normal mode is possible.
When the fuel cell assembly (FC) is connected in this state, the state transits to a fuel cell assembly mode OFF state 45 . When the power switch is turned on, the notebook personal computer 1 is activated in the fuel cell assembly mode.
However, unlike the normal mode by Li cell drive, before the power ON sequence of the notebook personal computer 1 starts, a sequence 46 for activating the fuel cell assembly is executed.
The manner the fuel cell assembly is activated largely changes depending on the design of the fuel cell assembly unit. At the start of this sequence, the fuel cell assembly unit is identified.
In this embodiment, the power input connector 17 for the fuel cell assembly has connection for I 2 C communication, unlike the normal connector 10 for the AC adapter, as shown in FIG. 10 .
CLI 2 C and DAI 2 C are clock and data lines for the I 2 C communication. For this communication, any other scheme except that for the I 2 C communication can be used as long as the required number of signal lines is small.
Basically, only an activation command need be sent from the power supply microcomputer of the notebook personal computer 1 to the fuel cell assembly through the I 2 C communication line shown in FIG. 13 as long as the fuel cell assembly unit has various auxiliary functions.
In this case, the fuel cell assembly unit autonomously increases the fuel cell assembly temperature and connects an internal dummy load to the fuel cell assembly to increase the output of the fuel cell assembly to a predetermined value. This is because the load response of a fuel cell assembly is generally very slow.
If the load largely varies, a time of about 1 sec may be required until the current stabilizes. hence, when the notebook personal computer 1 is to be directly activated using the fuel cell assembly in the no load state, no sufficient power is supplied.
For a fuel cell assembly unit of inexpensive type with only basic functions, when the power switch ON event occurs in the fuel cell assembly mode, the power supply microcomputer connects the output of the fuel cell assembly to the electric double-layered capacitor 18 to set the fuel cell assembly in the full load state, and starts the power ON sequence after checking that the output of the fuel cell assembly increases to a predetermined value or more.
Depending on the type of fuel cell assembly and environmental conditions, the cell may have to be preheated by reversely feeding the power from the secondary cell 12 to the fuel unit through the power supply lines (+ and −) shown in FIG. 10 before the power ON sequence.
It is not preferable to directly connect the capacitor to the output line of the fuel cell assembly and start the power ON sequence after the power supply voltage sufficiently rises. This is because after the power supply voltage sufficiently rises, the output current of the fuel cell assembly considerably decreases, as shown in FIG. 11 . As is known, until the output current of the fuel cell assembly rises, a very long time is required as compared to other cells.
In this embodiment, as shown in FIGS. 12 and 13 , the capacitor 18 is actively charged using a charge pump circuit 11 b through a diode 11 c under the control of the power supply microcomputer. The charge pump circuit 11 b has a function of boosting the low-level voltage from the fuel cell assembly 2 .
The power supply microcomputer monitors the state of charges in the fuel cell assembly and electric double-layered capacitor 18 , and when the fuel cell assembly is set on the operative state, turns on the notebook personal computer and executes a power ON sequence 47 of the notebook personal computer 1 .
More specifically, referring to FIG. 12 , a control signal is output to a switching transistor 11 a to turn on the switching transistor 11 a . Simultaneously, the operation of the charge pump circuit 11 b is stopped. Thus, the output from the fuel cell assembly is supplied to the notebook personal computer 1 .
In the process of activating the notebook personal computer 1 , or during the operation of the notebook personal computer 1 , the internal hard disk drive 19 is activated. At this time, since the motor of the hard disk drive is activated, a large rush current flows. The electric double-layered capacitor 18 also has a function of preventing such an abrupt variation in load from being directly transmitted to the fuel cell assembly, as shown FIG. 13 .
If the influence of some system-side load on the fuel cell assembly 2 is allowable, the power supply section 11 having the arrangement shown in FIG. 14 may be used. In this case, the capacitor 18 is charged by the charge pump circuit 11 b , and when the output from the fuel cell assembly 2 and the like reach predetermined values, switching transistors lie and 11 f are turned on.
Referring back to FIG. 9 , although the power ON sequence 47 is the same as the conventional power ON sequence 41 , the number of components to be powered on is smaller because the power consumption and function are reduced.
The subsequent sequence in the fuel cell assembly mode is almost the same as that in the normal mode, and a detailed description thereof will be omitted. A frame 51 shown in FIG. 9 represents the fuel cell assembly mode. When the notebook personal computer 1 is executing certain operation, mode transit is not allowed.
When the notebook personal computer 1 is powered off and set in the state 45 , the mode can be changed. Similarly, in the normal mode, i.e., in the state represented by the frame 44 , transit to the fuel cell assembly mode is not allowed.
In the normal mode, the power input terminal 17 from the fuel cell assembly is disconnected by the switch in the power supply section 11 . Hence, even when the user connects the fuel cell assembly while the notebook personal computer 1 is being operated by, e.g., cell drive, the fuel cell assembly is actually kept disconnected. After the user powers off a node PC, the notebook personal computer can transit to the fuel cell assembly mode through the neutral mode.
In the state 45 in which the node PC is OFF although the fuel cell assembly is connected, when, e.g., the Wake On LAN condition is satisfied, the notebook personal computer operates as if the condition were satisfied in the neutral mode.
That is, the notebook personal computer 1 is activated using the cell as the power supply, and Wake ON LAN processing is started. Since the normal mode is set at this time, the power from the fuel cell assembly is disconnected from the notebook personal computer 1 , as described above.
According to the notebook personal computer system of this embodiment, in addition to the effect of the computer system of the first embodiment, since the capacitor is charged using the fuel cell assembly until the output of the fuel cell assembly stabilizes, the energy loss in the entire system becomes small. In addition, since the capacitor is not directly connected to the system, an excess rush current can be prevented from flowing to the fuel cell assembly.
As has been described above in detail, according to the present invention, a computer system in which water produced from the fuel cell assembly is prevented from entering the computer can be provided. In addition, a computer system which can normally operate using even a fuel cell assembly for which both the output power and output voltage are low can be provided.
Additional advantages and modifications will readily occur to those skilled in the art. Therefore, the invention in its broader aspects is not limited to the specific details and representative embodiments shown and described herein. Accordingly, various modifications may be made without departing from the spirit or scope of the general inventive concept as defined by the appended claims and their equivalents. | A computer system of this invention includes a power input terminal which is provided outside a personal computer, and an external fuel cell assembly connected to the power input terminal. Hence, a computer system in which water produced from the fuel cell assembly is prevented from entering the computer can be provided. A personal computer for which an operation mode for deriving the personal computer by a fuel cell assembly is prepared to prevent any trouble due to user's misunderstanding can be provided. | 8 |
RELATION TO PRIOR APPLICATION
This application claims priority to U.S. Provisional Patent Application Ser. No. 60/183,370, filed Feb. 18, 2000.
FIELD OF INVENTION
The present invention relates to cement. More particularly, the present invention relates to a slag cement mixture and a process of making the same. While the invention is subject to a wide range of applications, it is especially suited for use in structural concrete and concrete construction.
BACKGROUND
Cement is a widely used building material. A particularly popular variety of cement is portland cement. Portland cement is used in many applications such as mortar, concrete, and cement building materials such as building blocks. Portland cement is produced by pulverizing clinker to a specific surface area of about 3,000 to 5,000 cm 2 /g or finer. Clinker is created in a cement kiln at elevated temperatures from ingredients such as limestone, shale, sand, clay, and fly ash. The cement kiln dehydrates and calcines the raw materials, and produces a clinker composition comprised of tricalcium silicate (3CaO—SiO 2 ), dicalcium silicate (2CaO—SiO 2 ), tricalcium aluminate (3CaO—Al 2 O 3 ), and tetracalcium aluminoferrite (4CaO—Al 2 O 3 —Fe 2 O 3 ).
Conventional mortar and concrete compositions contain cement, aggregates such as gravel and sand, and water to activate the hydration process. A mortar product is a hardened cement product obtained by mixing cement, a fine aggregate, and water. A concrete product is a hardened cement product obtained by mixing cement, coarse aggregate, water, and often a fine aggregate as well.
The strength properties of concrete and mortar products depend in part on the relative proportions of cement, aggregates, and water. The American Society for Testing and Materials (“ASTM”) standard test procedures, such as ASTM C192 and C39 describe the procedures for mixing, casting, curing, and testing portland cement concrete mixtures with 1, 3, 7, 14, and 28 day standards. Greater compressive strength is a desirable feature of cement, and a number of materials have been used to improve the compressive strength of cements.
One way of improving the compressive strength of hardened cement is to blend ground granulated blast furnace slag with cement to give an improved cement composition. Blast furnace slag is a by-product of the production of iron in a blast furnace consisting of silicates and aluminosilicates of calcium. A quick setting cement can be produced by grinding blast furnace slag with gypsum. (See, for example, U.S. Pat. Nos. 1,627,237 and 2,947,643). Blast furnace slag has hydraulic properties very similar to portland cement, and adding blast furnace slag to cement is routine to increase the cement's strength. (See ASTM Specification C989).
Typical North American blast furnace slag composition ranges are 32-40% Sio 2 , 7-17% Al 2 O 3 , 29-42% CaO, 8-19% MgO, 0.7-2.2% SO 3 , 0.1-1.5% Fe 2 O 3 , and 0.2-1.0% MnO. (see The Portland Cement Association Research and Development Bulletin RD112T). Blast furnaces in the U.S. are operated using a basic slag, typically defined as the slag ratio: (% CaO+% MgO)/(% SiO 2 +% Al 2 O 3 ), where the slag ratio is maintained in excess of 1.0 in order to remove sulfur from the iron produced and to facilitate producing an iron of high carbon content. The chemical composition of blast furnace slag also varies world wide, especially in alumina content. Blast furnace slags have long been recognized as very useful commodities and have been used in a number of applications. In addition to its use as cement additive, blast furnace slag has been used in asphalt, sewage trickle-filter media, roadway fills, and railroad ballast.
Blast furnace slags can be used to prevent excessive expansion of concrete mixtures that have a high-alkali content and aggregates that are alkali-reactive. Use of blast furnace slag as 40% or more of such a cement mixture can prevent excessive expansion. Blast furnace slag is characterized by its short setting time, which is the time between the addition of mixing water to a cementitious mixture and when the mixture reaches a specified degree of rigidity as measured by a specified procedure.
Steel slag is also used as a cement additive. Steel slag is formed in the process of making steel in a blast furnace, and often has a high concentration of ferrites. Because of its high ferrite composition, steel slag is generally used as a filler in cement road building material or as a feedstock raw material in cement kilns. It is possible to produce a hydraulic cement base from steel slag by adding further minerals to the slag portion, thereby reducing the ferrite composition of the slag. This additional step, while rendering a usable product, is costly and time consuming.
Mixtures of blast furnace slag and steel slag have resulted in stronger cement products, but cupola furnace slag, a by-product of cast iron production, is only rarely used in cement except as a processing addition. (See ASTM C465 and Cupola Handbook, published by the American Foundrymen's Society). Blast furnaces and cupola furnaces are operated differently and are used to make different iron products, consequently, the slag products of these furnaces are also different, both in chemical composition and in material properties. Cupola slag has different hydraulic properties than blast furnace slag. For example, cupola slag blended cement sets more slowly and at 7 days lacks the strength of blast furnace slag blended cements. Also, cupola slag is not a common concrete additive due to environmental concerns such as the possibility of rain water leaching out some of its components. Indeed, cupola slag often presents a disposal problem, which creates an additional expense, ultimately increasing the cost of the iron produced.
There is an ever present need in the cement art for harder, stronger cement products with longer setting times. There is also a need in the cast-iron production art for a disposal method for cupola slag that is environmentally safe and economically practical.
SUMMARY OF THE INVENTION
Accordingly, the present invention is directed to a cupola slag blended cement with an increased compressive strength. The principal advantage of the present invention is a cement mixture that results in a concrete which is both harder and stronger while providing a means of recycling cupola slag that is both environmentally sound and economically practical. The cement compositions of the present invention have a resistance to expansion due to sulfate attack and alkali silica reaction, and can be formulated to have a wide range of curing times.
To achieve these and other advantages and in accordance with the purpose of the invention, as embodied and broadly described, the invention is a hydraulic cement containing cupola slag ground to a fineness of greater than 4,000 cm 2 /g blended with portland cement. A preferred embodiment of the invention is a hydraulic cement containing cupola slag ground to a fineness of greater than 5,000 cm 2 /g blended with portland cement. In the most preferred embodiment, the invention is a hydraulic cement containing cupola slag ground to a fineness of between 6,000 cm 2 /g and 7,000 cm 2 /g.
In one embodiment, the invention is a hydraulic cement containing from about 20 to 50% of a ground granulated cupola furnace slag blended with portland cement. In a preferred embodiment, the invention is a hydraulic cement containing from about 30% to 40% cupola slag blended with portland cement. In another preferred embodiment, the invention is a hydraulic cement containing about 35% cupola slag blended with portland cement.
The invention includes ground granulated cupola furnace slag with a fineness of about 5,000 to about 7,000 cm 2 /g and meeting the fineness requirement of the ASTM C989 Grade 100 specification for blast furnace slag.
The invention includes ground granulated cupola furnace slag with a fineness of about 6,000 to about 6,750 cm 2 /g. The invention also includes ground granulated cupola furnace slag with a fineness of about 6,500 cm 2 /g.
In one embodiment of the invention, a blended cement mixture of about 35% cupola furnace slag displays a 28 day compressive strength of more than 7,000 psi and a flexural strength of more than 700 psi.
In another embodiment of the invention, the total heat of hydration of the blended cement mixture of about 35% cupola furnace slag does not exceed 250 J/g when measured for 72 hours, and the expansion of mortar bars does not exceed 0.20% at when measured at 14 days.
In one embodiment, the invention includes a process of using cupola slag as a raw cement kiln feedstock.
BRIEF DESCRIPTIONS OF THE DRAWINGS
FIG. 1 shows the results of conduction calorimetry tests performed on two neat cement pastes: standard portland cement (darker line), and a portland cement/cupola slag blend (lighter line).
FIG. 2 shows the results of compressive strength tests performed on concrete objects made with the same aggregates, but using either standard portland cement (solid line), or a 65/35% blend of portland cement and cupola slag (dashed line).
FIG. 3 shows the results of X-ray powder diffraction tests performed on cupola furnace slag (upper diffractogram) and on blast furnace slag (lower diffractogram).
DETAILED DESCRIPTION OF THE INVENTION
The present invention encompasses blends of cupola slag and cement with an increased hardness and strength than the cement alone.
The hydraulic cement compositions of the present invention provide a solution to the current needs of the art by converting cupola furnace slag into a useful product. The cement compositions of the invention can be formulated to have a wide range of resistance to sulfate attack as well as wide range of curing times so that they can be used for a variety of purposes such as making concrete objects. In particular, a hydraulic cement containing 35% of a ground granulated cupola furnace slag, with a fineness of at least 6,000 cm 2 /g and meeting the fineness requirement of the ASTM C989 Grade 100 specification for blast furnace slag blended with portland cement creates a composition whose superior compressive strength develops slower than the concretes currently in use thus providing a more durable concrete product. Additionally, the sulfate attack resistance of the present invention increases the useful life of any products made from cupola furnace slag blended cements thereby increasing the length of time between replacing such products and reducing the overall cost of any such project.
The chemical composition of portland cement plays an important role in the way that slag blended cements cure, age and resist chemical attack. The processing of portland cement is well known in the art, as are the various methods to alter the chemical composition during the manufacturing process. The invention is not, however, limited to portland cement. It is believed that cupola slag mixed with other cements will improve the strength of the cement/cupola slag mixture.
A cupola furnace is a vertical shaft furnace used to produce cast iron by high temperature melting of metallic and mineral charge materials. A cupola furnace contains a continuous melting shaft which can accept a wide range of raw materials including oily, wet and contaminated scrap. Compared to batch-type furnaces, the energy requirements of a cupola furnace are low. Molten iron is tapped from the bottom of the furnace. Slag is removed in a molten state via a slag hole. Cupola furnace slag is preferably rapidly quenched by submersion into water to yield a fine, granulated product, thus reducing the amount of grinding required to make the slag useful in cement. Alternatively, water may be sprayed upon the slag to quench it, or the slag may be allowed to air-cool for a time, resulting in a coarser, non-granulated product.
Cupola furnace slag differs from blast furnace slag in chemical composition; for example, cupola slag has a higher silica content and a lower calcium oxide content than blast furnace slag. While blast furnaces operate using a basic slag, cupola furnaces generally operate using an acid slag for the production of gray cast iron. (Basic slags are sometimes used in cupola furnaces for the production of ductile iron because the basic slag removes sulfur in the cupola during melting). Blast furnace operations produce about 30 percent slag per ton of molten iron, while cupola furnace operations produce 5 to 6 percent slag per ton of iron ore that is melted.
Cement users are particularly interested in setting and strength development characteristics. The maximum and minimum setting times and minimum strengths of reference cement are specified in the ASTM C150 standard specification for portland cements. A number of minor components which form in the clinker from impurities present in the raw materials or fuel can influence both the clinker formation process and the hydraulic reactivity and cementitious properties of the resulting cementitious material. In particular, the level of alkalis, such as K 2 O and Na 2 O present in cement, especially portland cement, may be of concern. For example, if the cementitious materials are combined with aggregates containing SiO 2 , the alkalis present in the cementitious materials may react with the SiO 2 to form an expansive alkali silica gel, which can lead to cracking and break up of the concrete structure. Because the detection of reactive SiO 2 in aggregates is difficult, cementitious materials with low alkali content are generally used. Blast furnace slags are generally very basic in nature. Thus, a maximum equivalent Na 2 O of about 0.6 percent is included as an optional limit in the ASTM C150 specification.
It is possible to use cement containing more than 0.60 percent equivalent Na 2 O with SiO 2 reactive aggregates while avoiding excessive expansion and reducing the total energy used to manufacture the cement. One example is to mix cement, preferably portland cement, with latently hydraulic materials such as ground granulated blast furnace slag. However, the latently hydraulic materials do not react as quickly as portland cement, and as a result they contribute to the later developed cement strength rather than the earlier. The decreased early activity results in lower heats of hydration, which leads to thermal crack formation. However, the addition of blast furnace slag does not eliminate thermal crack formation.
ASTM C125-99a “Standard Terminology Relating to Concrete and Concrete Aggregates” defines a number of terms that apply to hydraulic cement. It is well known in the prior art, that the hydraulic properties of blast furnace slag vary greatly upon the chemical nature of the blast furnace slag and the way that molten slag is cooled.
Blast furnace slag is classified by performance in the blast furnace slag activity test in three grades, Grade 80, Grade 100, and Grade 120. ASTM specification C989 outlines the strength development of portland cement mixed with the three strength grades of finely ground, granulated blast furnace slag as measured at seven days and twenty-eight days and expresses this as blast furnace slag activity index (SAI). When blast furnace slag is used in concrete with portland cement, the levels and rate of strength development depend on the properties of the blast furnace slag, the portland cement, the relative and total amounts of the blast furnace slag and the cement as well as the cement curing temperatures. Unless the slag is derived from a blast furnace it cannot be marketed as blast furnace slag under the ASTM C989 standards.
ASTM C989 specifies that the reference cement used to test blast furnace slag activity have a minimum 28-day strength of 35 MPa (5,000 psi) and an alkali content between 0.6 and 0.9%. To properly classify a blast furnace slag, the reference portland cement must conform to the limits on strength and alkali content under ASTM specification C989. Test data indicate that concrete compressive strengths at 1, 3 and even 7 days tend to be lower using blast furnace slag cement combinations. Generally a higher numerical grade of blast furnace slag can be used in larger amounts and will provide improved early strength performance, but tests must be made using job materials under job conditions to properly access the performance of a blast furnace slag cement.
Blast furnace slag has latent hydraulic properties that require an activator to realize these hydraulic properties. One way for slag to acquire hydraulic properties is to rapidly quench the slag to preserve the molten slag in a vitreous state. Two processes that are commonly used to activate the slag's hydraulic properties are granulation and pelletization. In the granulation process, slag is quenched by the injection of a large quantity of water under pressure into the slag. If the temperature of the slag is above its melting point prior to quenching, then quenching produces a wet sand-like material with a high degree of vitrification. But if the slag is permitted to cool slowly, it crystallizes and exhibits reduced hydraulic properties. To achieve the desired fineness, the granulated slag is dried and ground. Blast furnace slags are typically ground to a specific surface area of 5,000 to 6,500 cm 2 /g. A fineness of greater than 6,500 cm 2 /g requires additional steps and is more difficult to achieve on a large industrial scale under dry conditions. Another measure of specific surface area is the Blaine air permeability method. The Blaine Fineness test is described in ASTM C204 “Standard Test Method of Hydraulic Cement by Air Permeability Apparatus.” There, blast furnace slags are described as having a specific surface area of 5,000 to 6,500 cm 2 /g. The early development of high strength is a characteristic of cements comprising blast furnace slag ground to a fineness of 7,500 cm 2 /g. As the fineness increases so does the rate of the hardening reaction. As ground granulated blast furnace slag typically has a fineness of about 5,000-6,500 cm 2 /g, an extra grinding step is required to achieve a fineness of 7,500 cm 2 /g. There is an energy cost for the extra grinding step, but it substantially improves the mechanical strength of the resulting cement. Greater specific surface areas generally result in greater initial strengths.
Cupola furnace slag can be granulated by the process of slag quenching. Molten cupola furnace slag is granulated by the injection into the slag of a large quantity of water under pressure, producing a wet sand like material with a high degree of vitrification. The degree of vitrification depends on the slag temperature prior to injection and the temperature of the water under pressure. Because cupola slag has a lower sulfate and magnesium content and a higher silica and iron oxide content there is a decrease in the heat generated, which is advantageous for increasing setting time and slowing the initial strength gain of the concrete. The lower sulfate and magnesia content coupled with a higher silica and iron oxide content also leads to a reduction in the expansions due to heat of hydration and alkali silica reaction.
For the purpose of illustrating the advantages obtained by the practice of the present invention, plain concrete mixes were prepared and compared to similar mixes containing cupola slag. The following example is illustrative and is not intended to be limiting. The methods and details were in accordance with current applicable ASTM standards.
EXAMPLE 1
Cupola furnace slag useful in cement compositions of the present invention desirably shows the following components upon analysis: Table 1. Composition of Cupola Slag
TABLE 1
Composition of Cupola Slag
Component
Proportion (wt. %)
SiO 2
43.87
Al 2 O 3
8.5
Fe 2 O 3
1.93
CaO
33.3
MgO
3.38
SO 3
0.30
Na 2 O
0.10
K 2 O
0.30
TiO 2
0.34
P 2 O 5
<0.01
Mn 2 O 3
1.18
SrO
0.08
L.O.I. (950° C.)
4.34
Total
97.84
Alkalies as Na 2 O
0.30
Although only applicable to blast furnace slag, the Slag Activity Index test as described in ASTM C989 “Standard Specification for Ground Granulated Blast Furnace Slag for Use in Concrete” was performed on the cupola furnace slag as well as a Blaine Fineness test as described in ASTM C204 “Standard Test Method of Hydraulic Cement by Air Permeability Apparatus.” Table 2 shows the results of these two tests for two different cupola slag samples ground using a 40-lb mill to two different fineness values similar to those of commercially available blast furnace slags.
TABLE 2
Fineness and Slag Activity Index data
Ground
Cupola
ASTM C989
Slag Sample
Requirement for:
Grade
Grade
No. 1
No. 2
80 min
100 min
Fineness, cm 2 /g
4240
6530
—
—
Slag Activity
At 7 days
61
73
—
70
Index, % of
At 28 days
98
124
70
90
control
As evident from Table 2, both samples exceeded the ASTM C989 SAI requirements for Grade 80 and Grade 100 blast furnace slag at 28 days. Sample 2 met the SAI 7 day requirements for Grade 100 as well. Based on this test, all additional tests were preformed on Sample 2.
Conduction calorimetry tests were conducted on neat cement pastes made with the control cement and with cupola furnace slag blend by injection-mixing of 2 grams of cement with water inside a calorimeter cell. The slag used in this test was Sample 2 as it met the ASTM C989 Blast Furnace Slag Activity Index requirement for 7-day and 28-day of commercially available blast furnace slag Grade 100. The heat of hydration was recorded over a 72 hour period. The first peak represents the heat reaction as the cement comes into contact with the mix water. After the initial peak there is a period of relative inactivity during which the paste remains plastic. The second peak indicates an accelerated reaction during which the alite in the cement hydrates rapidly and heat is generated. The initial setting of the paste occurs soon after the beginning of the acceleration period and the final setting occurs towards the end of the acceleration period. A maximum in heat evolution is reached soon after the final set, after which the heat evolution declines to a steady state. The heat of hydration is a function of both the chemical and the physical properties of the cement. Table 3 shows the results of the calorimetry tests.
TABLE 3
Heat Generation Data for Portland Cement and Cupola Furnace Slag Blended Cement
Control
Cupola Slag Blend
Rate of heat
Rate of heat
generation
Total Heat
generation
Total Heat
Description
Time
J/Kg/sec
J/g
Time
J/Kg/sec
J/g
Initial
2.28
min
48.74
3.35
3.48
23.55
2.51
Hydration Peak
Total Heat at:
0.5
hr
15.43
0.5
hr
11.07
Onset of Alite
2.15
hr
0.59
20.15
3.09
hr
0.51
17.26
Hydration
Peak of Alite
11.20
hr
2.91
71.17
15.30
hr
2.70
89.28
Hydration
Total Heat at:
24
hr
169.61
24
hr
140.91
Total Heat at:
48
hr
235.70
48
hr
193.40
Total Heat at:
72
hr
264.33
72
hr
223.19
Table 3 indicates that the initial hydration peak for cupola slag cement occurs later in time than that of the control cement and generates heat at a much slower rate and generates a lot less heat. Total heat one half hour after hydration is considerably lower for cupola furnace slag as well. Another major difference between the control cement and the cupola furnace slag cement is that the onset of alite hydration and the peak of hydration are both much later in the cupola slag cement than in the control. Initially the total heat released for alite hydration is lower for the cupola slag cement but by the time the peak of alite hydration occurs, the total heat generated is higher for the cupola slag cement than the control cement. Total heat released overall remains lower for the cupola slag cement at each of the time periods measured. It is anticipated that the surprising low-heat properties of the cupola slag cement will make it particularly useful in making concrete that is adapted for mass concrete pours such as raft foundations, bridge decks, piers, and dams.
Resistance to sulfate attack on Sample 2 was tested in accordance with ASTM C1012 “Standard Test Method for Length Change of Hydraulic-Cement Mortars Exposed to a Sulfate Solution”. The expansion of the control and the blended cupola furnace slag cement at 15 weeks was 0.026 and 0.015% respectively.
The potential for the cupola slag to modify alkali reactivity was determined using ASTM C1260 “Standard Test Method for Potential Alkali Reactivity of Aggregates (Mortar Bar Method)”. The cement used in this test was the cupola furnace slag bend of sample 2, and the aggregate was a highly reactive graded Albuquerque sand. Table 4 shows the results.
TABLE 4
Expansion of Bars Due to Alkali Silica Reaction
Expansion, %
Age, Days
Control
Cupola Slag Blend
0
0.000
0.000
5
0.009
0.013
11
0.349
0.77
14
0.580
0.195
Table 4 indicates that the potential of cupola slag to modify alkali reactivity is considerably lower for cupola slag at days 11 and 14 than the control.
Compression and flexural strengths of a blended cement containing 35% cupola furnace slag (Sample 2) was measured at day 3, day 7, day 28, day 56 and day 90 and compared to a control cement measured with the same age in days. No chemical additives were added to either mix and the mixes were made with the same cementitious content as well as the same water to cementitious ratio. The mix portions of the two cements are shown in Table 5 while the results of the compression and flexural tests are shown in Table 6.
TABLE 5
Concrete Mix Proportions
Mix Proportions
Material
Control
Cupola Slag Blend
Portland Cement, pcy*
654
426
Slag, pcy
0
229
Eau Claire sand, pcy
1,342
1,336
Eau Claire ¾″ stone, pcy
1,847
1,849
Water, pcy
266
267
Slump, inches
5
7
(*pounds per cubic yard)
TABLE 6
Compressive and Flexural Strength Results
Compressive Strength
Flexural Strength
(ASTM C39), psi
(ASTM C78), psi
Cupola Slag
Cupola Slag
Age, Days
Control
Blend
Control
Blend
3
4,410
2,570
—
—
7
5,530
4,320
785
490
28
7,150
7,780
750
755
56
7,530
8,740
770
750
90
7,710
8,630
—
—
Table 6 demonstrates that the cupola slag blended cement at days 3 and 7 displays a lower compressive strength when measured using the ASTM C29 method. By day 28, however, the compressive strength of the cupola slag has surpassed that of the control cement, a totally unexpected result. Additionally, the compressive strength of the cupola slag blended cement unexpectedly continued to increase until after day 56 where it begins to level off. At day 56 the compressive strength of the cupola slag blended cement is more that 1,200 psi greater than the control cement. These tests indicate the surprising result that the cupola slag blended cement makes superior concrete over that made with conventional cements. Table 6 demonstrates that the flexural strength of the cupola slag blended cement as measured by the ASTM C78 method develops at a slower rate than that of the control but after 28 days is approximately equal to that of the control cement.
X-Ray Diffraction Analysis
X-ray diffraction may be used to identify and quantify crystalline materials. Crystalline materials consist of ordered arrangements of atoms in three-dimensional arrays. Such arrays have characteristic spacings between the layers of closely packed atoms. The length of the spacings vary by atom size and the three dimensional arrays.
When a powdered sample is subjected to a beam of radiation from an X-ray source a diffraction pattern is created. The X-ray beam penetrates the powder a short distance and diffracts from the most densely packed layers of the atoms within the powdered sample. The X-ray beam is rotated through a series of angles relative to the surface of the powdered sample. When the signal from the diffracted beam is particularly strong, the distances between layers of atoms (the d-spacings) can be calculated as multiples of the wavelengths of the incident radiation and the incident angle.
A crystalline material has a characteristic pattern of relative peak heights at given angles. Mixtures of crystalline materials display combinations of these patterns and the relative peak heights from various materials can be used to quantify the relative concentration of each crystalline material. X-ray diffraction may also be used to identify cracks in concrete. The detection limit for X-ray will depend on the type of material analyzed and it can be as high as 5 to 10%.
A ground granulated cupola furnace slag sample was finely powdered and subjected to XRD analysis on a Philips PW 1720 X-ray diffractometer (CuKO) equipped with a θ-compensating slit, graphite monochromator, gas proportional counter detector, pulse height selector and a strip chart recorder. A commercial granulated blast furnace slag sample was also finely powdered and analyzed as a control. Each sample was scanned from 65°2θ to 6°2θ at a rate of 1°2θ per minute. Table 7 is a summary of the phases detected by XRD.
TABLE 7
X-ray Diffraction Analysis
Sample
Largest Phase Detected
Crystalline material
Cupola Furnace Slag
Amorphous material with a
SiO 2 (α-quartz)
peak at 29.8° 2θ
Blast Furnace Slag
Amorphous material with a
CaCO 3 (calcite)
peak at 31° 2θ
As can be seen from Table 7, the two slag samples vary in their crystalline composition as well as their non-crystalline or glassy composition. The cupola slag sample has an amorphous phase peak at 29.8°2θ (lower angle) indicating a larger d-spacing than that of the blast furnace slag. The XRD analysis also shows that crystalline SiO 2 is present in the cupola slag which suggests a more acidic form of the amorphous phase. The amorphous phase of the cupola slag probably contains of higher amounts of not only SiO 2 but also Al 2 O 3 and Fe 3 O 3 than the blast furnace slag.
All references and standards cited herein are incorporated in their entireties. | A slag cement mixture and process of making the same is disclosed. The slag cement mixture is composed of cupola slag and portland cement. The cupola slag is optionally ground granulated. One embodiment of the process includes rapidly quenching the slag by submersion into water or by spraying water onto it, and grinding the resulting product to achieve a fineness of at least 6,000 cm 2 /g. The process also includes the addition of 35% ground granulated cupola slag to portland cement to achieve a stronger and harder cement than portland cement alone. | 8 |
REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to U.S. Provisional Patent Application Ser. No. 60/889,355 entitled “Method for Increasing Production of Adult Stem Cells In Vivo” filed Feb. 12, 2007, which is incorporated herein by reference.
FIELD OF INVENTION
[0002] This invention relates to methodologies for stimulating the production of adult stem cells in living organisms without chemical or physical invasion into the organism and, more particularly, to a method and device for using topical application of acoustic vibrations to stimulate the production of adult stem cells in living organisms.
BACKGROUND OF THE INVENTION
[0003] An adult stem cell is an undifferentiated cell found among differentiated cells in a tissue or organ that is capable of renewing itself and differentiating to yield the major specialized cell types of the tissue or organ. The primary roles of adult stem cells in a living organism are to maintain and repair the tissue in which they are found. Scientists have found adult stem cells in many more tissues than they once thought possible. This finding has led scientists to ask whether adult stem cells could be used for transplants.
[0004] Hematopoietic cell transplantation is the gold standard for cell-based therapy and is routinely used to treat a wide variety of blood disorders and cancer. A major limitation exists, however, in finding donors whose immune systems are compatible with those of the patients requiring transplantation. Therefore, there is a continuing need for techniques for stimulating the production of adult stem cells in living organisms.
[0005] Certain kinds of adult stem cells seem to have the multipotent hematopoietic ability to differentiate into a number of different cell types, given the right conditions. If this differentiation of adult stem cells can be controlled in the laboratory, these cells may become the basis of therapies for many serious common diseases. Scientists in many laboratories are trying to find ways to grow adult stem cells in cell cultures and manipulate them to generate specific cell types so they can be used to treat injury or disease. Some examples of potential treatments include replacing the dopamine-producing cells in the brains of Parkinson's patients, developing insulin-producing cells for type I diabetes, and repairing damaged heart muscle following a heart attack with cardiac muscle cells. One population, known as hematopoietic stem cells, forms all the types of blood cells in the body. A second population, known as bone marrow stromal cells, was discovered a few years later. Stromal cells are a mixed cell population that generate bone, cartilage, fat, and fibrous connective tissue.
[0006] One important point to understand about adult stem cells is that there are a very small number of stem cells in each tissue. Stem cells are thought to reside in a specific area of each tissue where they may remain quiescent (non-dividing) for many years until they are activated by disease or tissue injury. The adult tissues reported to contain stem cells include the brain, bone marrow, peripheral blood, blood vessels, skeletal muscle, skin and liver. In particular, bone marrow stromal cells (mesenchymal stem cells) give rise to a variety of cell types: bone cells (osteocytes), cartilage cells (chondrocytes), fat cells (adipocytes), and other kinds of connective tissue cells such as those in tendons.
[0007] Stem cells differ from other kinds of cells in the body. All stem cells, regardless of their source, have three general properties: they are capable of dividing and renewing themselves for long periods; they are unspecialized; and they can give rise to specialized cell types. Stem cells have two important characteristics that distinguish them from other types of cells. First, they are unspecialized cells that renew themselves for long periods through cell division. The second is that under certain physiologic or experimental conditions, they can be induced to differentiate into cells with special functions, such as the beating cells of the heart muscle or the insulin-producing cells of the pancreas. Until now, the differentiation of adult stem cells controlled in the laboratory has been the only technique for developing adult stem cells for therapeutic uses for many serious common diseases.
[0008] Many serious diseases and disorders, and some therapies, involve damage to body tissues and/or insufficient natural repair of damaged body tissues. For example, cancer chemotherapy and radiation therapy destroy many other non-cancerous cells in the body, including those of the immune system. Disorders or cancers of the blood often involve abnormal growth and/or destruction of certain types of blood cells. Heart failure, which is currently incurable, often involves damage to heart muscle, which the body cannot repair. Liver failure often involves progressive destruction of liver cells. Stroke often involves irreversible damage and/or death of brain cells resulting from a lack of oxygen and nutrient-carrying blood to the affected portion of the brain. Type 2 diabetes, the most common form of the endocrine disorder, involves a progressive decrease in the ability of the pancreas to produce insulin, and its complications are due to progressive destruction of tissues in the eye (diabetic retinopathy, which can lead to blindness), kidney (diabetic nephropathy, which can lead to kidney failure), and nerves (diabetic neuropathy, which can lead to decreased sensation in the limbs and limb amputation as well as dysfunction of stomach, bladder). Osteoarthritis involves destruction of cartilage tissue in the joints. Parkinson's disease, Alzheimer's disease and other central nervous system disorders involve destruction of certain neurons in the brain. Various autoimmune disorders involve immune system attack and destruction of the lining around nerves (multiple sclerosis), the cell lining of the intestine (ulcerative colitis), cartilage in joints (rheumatoid arthritis), and other specific tissues for specific diseases. Spinal cord injuries involve trauma and destruction of nerve tissue in the spinal cord. Aging itself involves a general deterioration throughout the body's tissues.
[0009] Importantly, stem cell therapy offers the potential to help repair and renew the damaged tissues associated with these and other diseases, disorders and therapies. At present, it has been established that adult stem cells typically generate the cell types of tissue in which they reside. A blood-forming adult stem cell in the bone marrow, for example, normally gives rise to the many types of blood cells such as red blood cells, white blood cells and platelets. Until recently, it had been thought that a blood-forming cell in the bone marrow—which is called a hematopoietic stem cell—could not give rise to the cells of a very different tissue, such as nerve cells in the brain. However, a number of experiments over the last several years have raised the possibility that stem cells from one tissue may be able to give rise to cell types of a completely different tissue, a phenomenon known as “stem cell plasticity.” Examples of stem cell plasticity include blood stem cells differentiating to become neurons, liver stem cells differentiating to produce insulin, and hematopoietic stem cells differentiating to become heart muscle. Therefore, exploring the possibility of using adult stem cells for cell-based therapies has become a very active area of investigation by researchers.
[0010] Csete, et al., U.S. Pat. No. 6,759,242 issued Jul. 6, 2004 relates to the growth of cells in culture under conditions that promote cell survival, proliferation, and/or cellular differentiation. This patent contends that proliferation was promoted and apoptosis reduced when cells were grown in lowered oxygen as compared to environmental oxygen conditions traditionally employed in cell culture techniques.
[0011] Csete, et al., U.S. Pat. No. 6,610,540 issued Aug. 26, 2003 relates to the growth of cells in culture under conditions that promote cell survival, proliferation, and/or cellular differentiation. Again, this patent contends that proliferation was promoted and apoptosis reduced when cells were grown in lowered oxygen as compared to environmental oxygen conditions traditionally employed in cell culture techniques.
[0012] Csete, et al., U.S. Pat. No. 6,589,728 issued Jul. 8, 2003 describes a method of isolating, maintaining, and/or enriching stem or progenitor cells derived from diverse organ or tissue sources. This patent specifically teaches that these objectives can be accomplished by the controlled use of subatmospheric oxygen culture, and that the precise oxygen level or levels must be determined empirically and/or by reference to physiologic levels within intact functioning organ or tissue.
[0013] Shutko et al., Russian Patent No. 2,166,924 issued May 20, 2001 describes the application of micro-vibration treatment to eight to ten points located on central line of the vertebral column to mobilize existing adult stem cells in the blood, and thereby increase the presence adult stem cells in peripheral circulation. The micro-vibration frequencies applied to these areas is smoothly changed within a particular acoustic bandwidth, the treatment duration is ten to fifteen minutes, and the increase in the presence of the adult stem cells in the peripheral circulation is expected to occur within three to four hours after application.
[0014] Gillis, U.S. Pat. No. 5,199,942 issued Apr. 6, 1993 relates generally to methods for autologous hematopoietic cell transplantation in patients undergoing cytoreductive therapies, and particularly to methods in which bone marrow or peripheral blood progenitor cells are removed from a patient prior to myelosuppressive cytoreductive therapy, expanded in ex-vivo culture in the presence of a growth factor, and then readministered to the patient concurrent with or following cytoreductive therapy to counteract the myelosuppressive effects of such therapy. The patent also describes a culture media containing one or more growth factors for expanding progenitor cells in ex-vivo culture.
[0015] Emerson, et al., U.S. Pat. No. 5,646,043 issued Jul. 8, 1997 describes methods, including culture media conditions, which provide for ex-vivo human stem cell division and/or the optimization of human hematopoietic progenitor cell cultures and/or increasing the metabolism or GM-CSF secretion or IL-6 secretion of human stromal cells are disclosed.
[0016] Bachovchin, et al., U.S. Pat. No. 6,258,597 issued Jul. 10, 2001 describes methods, compositions, and devices for chemically stimulating the number and/or differentiation of hematopoietic cells in living organisms. The methods involve contacting the hematopoietic cells with an inhibitor of dipeptidyl peptidase (DPIV) in the absence of exogenously provided cytokines.
[0017] Buck, et al., U.S. Pat. No. 7,037,719 issued May 2, 2006 describes enriched neural stem and progenitor cell populations, and methods for identifying, isolating and enriching for neural stem cells using reagent that bind to cell surface markers.
[0018] Saito, et al., U.S. Pat. No. 7,037,892 issued May 2, 2006 describes a method for chemically stimulating the proliferation a hematopoietic stem cells in a living organism.
[0019] More particularly, the invention relates to a hematopoietic stem cell proliferating agent comprising insulin-like growth factor, either alone or in combination with some or other colony-stimulating factors and/or growth factors and to a method for proliferating.
[0020] Yang, U.S. Pat. No. 7,048,922 issued May 23, 2006 describes the stimulation of hematopoiesis by ex-vivo activated immune cells including a protocol for activating and administering human blood cells so that bone marrow histology and/or blood cell counts of patients suffering from aplastic anemia approach normal. The protocol includes culturing the blood cells in the presence of a cytokine and an ionophore.
[0021] Wallner, et al., U.S. Pat. No. 7,067,489 issued Jun. 27, 2006 describes methods and products for stimulating hematopoiesis, preventing low levels of hematopoietic cells and producing increased numbers of hematopoietic and mature blood cells both in-vivo and in-vitro.
[0022] Although these references indicate a high level of interest in in-vivo and in-vitro techniques for stimulating the production of stem cells, only Shutko et al., Russian Patent No. 2,166,924, describes the topical use of acoustical vibrations for stimulating the production of adult stem cells. However, the techniques described in this application are directed to mobilizing existing adult stem cells in the blood to increase the presence adult stem cell in peripheral circulation. The effect of the acoustical vibration treatment is expected to occur within about three to four hours after application. Therefore, Shutko et al. is directed to mobilizing existing adult stem cells, and does not describe a technique for stimulating the production of new adult stem cells in a living organism.
[0023] In view of the foregoing, it will be appreciated none of the conventional technologies provide a non-invasive technique for stimulating the production of adult stem cells in living organisms. Accordingly, there remains a need in the art for techniques for stimulating the production of adult stem cells in living organisms. There remains a further need for non-invasive techniques for stimulating the production of adult stem cells in living organisms, in particular without introducing chemicals or physically invading the organisms.
SUMMARY OF THE INVENTION
[0024] The present invention meets the needs described above through a method and device for using topically applied acoustical vibrations to stimulate the production of adult stem cells in living organisms. This approach is non-invasive, and more specifically does not involve introducing chemicals or physically invading the organisms. More specifically, one or more acoustical transducers are placed directly on the skin of the organism in certain locations, and selected vibration profiles are applied to the organism through the transducers. A regimen of regular application of the selected vibration profiles to the specified locations stimulates the production of adult stem cells in the organism.
[0025] In a particular embodiment, acoustical vibrations are applied to specific areas of the body in specified pulse profiles that generally include sequences of pulses ranging from one-half second to three seconds, modulated with an oscillatory signal in the frequency range of 1 Hz to 1500 Hz, and having pulse amplitude in the range of range from about 20 to 5000 microns. The number of application points may vary from one to about thirty, and treatments may be applied once or twice daily over an extended period of weeks, months or years. For example, the acoustical micro-vibration treatments of this type may be applied to the spine, skull, back, pelvis, abdomen, and the upper and low extremities.
BRIEF DESCRIPTION OF THE DRAWING
[0026] FIG. 1 is a front view of a micro-vibration unit suitable for implementing the present invention.
[0027] FIG. 2 is a graphical representation of a first micro-vibration profile that may be applied through the micro-vibration unit to a living organism to stimulate the production of adult stem cells in the organism.
[0028] FIG. 3 is a graphical representation of a second micro-vibration profile that may be applied through the micro-vibration unit to a living organism to stimulate the production of adult stem cells in the organism.
[0029] FIG. 4 is a graphical representation of a third micro-vibration profile that may be applied through the micro-vibration unit to a living organism to stimulate the production of adult stem cells in the organism.
[0030] FIG. 5 is a graphical representation of a fourth micro-vibration profile that may be applied through the micro-vibration unit to a living organism to stimulate the production of adult stem cells in the organism.
[0031] FIG. 6 is a graphical representation of a fifth micro-vibration profile that may be applied through the micro-vibration unit to a living organism to stimulate the production of adult stem cells in the organism.
[0032] FIG. 7A is a graphical representation of an area overlying the thoracic spine of a human selected for micro-vibration treatment.
[0033] FIG. 7B is a graphical representation of specific points within the area of FIG. 7A for applying micro-vibration treatments to stimulate the production of adult stem cells.
[0034] FIG. 8A is a graphical representation of an area overlying the front portion of the cranium of a human selected for micro-vibration treatment.
[0035] FIG. 8B is a graphical representation of specific points within the area of FIG. 8A for applying micro-vibration treatments to stimulate the production of adult stem cells.
[0036] FIG. 9A is a graphical representation of an area overlying the rear portion of the cranium of a human selected for micro-vibration treatment.
[0037] FIG. 9B is a graphical representation of specific points within the area of FIG. 9A for applying micro-vibration treatments to stimulate the production of adult stem cells.
[0038] FIG. 10A is a graphical representation of an area overlying the lower spine of a human selected for micro-vibration treatment.
[0039] FIG. 10B is a graphical representation of specific points within the area of FIG. 10A for applying micro-vibration treatments to stimulate the production of adult stem cells.
[0040] FIG. 11A is a graphical representation of areas overlying the shoulder blades of a human selected for micro-vibration treatment.
[0041] FIG. 11B is a graphical representation of specific points within the areas of FIG. 11A for applying micro-vibration treatments to stimulate the production of adult stem cells.
[0042] FIG. 12A is a graphical representation of areas overlying the lower back of a human selected for micro-vibration treatment.
[0043] FIG. 12B is a graphical representation of specific points within the areas of FIG. 12A for applying micro-vibration treatments to stimulate the production of adult stem cells.
[0044] FIG. 13A is a graphical representation of an area overlying a front portion of the abdomen of a human selected for micro-vibration treatment.
[0045] FIG. 13B is a graphical representation of specific points within the area of FIG. 13A for applying micro-vibration treatments to stimulate the production of adult stem cells.
[0046] FIG. 14A is a graphical representation of an area overlying a rear portion of the abdomen of a human selected for micro-vibration treatment.
[0047] FIG. 14B is a graphical representation of specific points within the area of FIG. 14A for applying micro-vibration treatments to stimulate the production of adult stem cells.
[0048] FIG. 15A is a graphical representation of areas overlying the leg muscles of a human selected for micro-vibration treatment.
[0049] FIG. 15B is a graphical representation of specific points within the area of FIG. 15A for applying micro-vibration treatments to stimulate the production of adult stem cells.
[0050] FIG. 16A is a graphical representation of areas overlying the inner arm muscles of a human selected for micro-vibration treatment.
[0051] FIG. 16B is a graphical representation of specific points within the area of FIG. 16A for applying micro-vibration treatments to stimulate the production of adult stem cells.
[0052] FIG. 17A is a graphical representation of areas overlying the outer arm muscles of a human selected for micro-vibration treatment.
[0053] FIG. 17B is a graphical representation of specific points within the area of FIG. 17A for applying micro-vibration treatments to stimulate the production of adult stem cells.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0054] Mechano-transduction is the process by which cells in living organisms convert mechanical stimuli into biochemical signals. The inventors have discovered that cells react to acoustical micro-vibration stimuli by trying to protect tissue integrity, which stimulates the production of adult stem cells in the tissue. For example, it is believed sound energy stimulates chondrocyte, which leads to enhanced proteoglycan synthesis, and ultimately results in augment synovial fluid production and cartilage repair. It is also believed that acoustical micro-vibrational stimulation enhances chondrocyte proliferation in living tissue, especially through the application of repetitive pulses with oscillatory waveform in the frequency range from 1 Hz to 1500 Hz. Analysis of the test data further suggests that genetically coded chondral growth is up-regulated by these mechanical signals. Other cell types that are believed to respond to this type of mechanical stimuli with increased production of adult stem cells include osteocyte, myocardiocyte, monocyte, endothelium.
[0055] Adult stem cells can differentiate in all of above mentioned cell types and serve as the precursors for tissue repair. The primary function of adult stem cells is to maintain and repair tissues wherever it is found. The proliferation of adult stem cells increases when tissue is damaged or stimulated in a manner that mimics the effect of damaged. Known factors that increase adult stem cell production include chemical substances (such as growth factors) and hypoxemia (decreased concentration of oxygen in the tissue). In accordance with the present invention, adult stem cell production is stimulated by mechanical stimuli in the form of acoustical micovibrations. The adult stem cells respond to the micovibration treatment by multiplying faster in the area where the treatment is applied. This action is similar to chondrocyte response to increase synthesis of proteoglycan to protect cartilage or osteocyte to produce more bone in response to mechanical stress.
[0056] FIG. 1 is a front view of a micro-vibration unit 100 suitable for implementing the present invention. The micro-vibration unit includes a control unit 102 and a plurality of transducers 104 a - d that convert electric drive signals into acoustical pulse waves. The transducers are configured to be applies directly to the skin, for example with tape, elastic straps or other suitable attachment devices. A prior but similar micro-vibration unit is described in commonly owned U.S. patent application Ser. No. 10/761,726 (Publication No. 2004-0167446), which is incorporated herein by reference. The micro-vibration unit 100 is different from the prior unit in that the new unit 100 is configured to produce the pulse wave profiles described below, which have been found to be effective for stimulating adult stem cell production in living organism.
[0057] FIG. 2 is a graphical representation of an illustrative portion of a micro-vibration profile 120 that may be applied through the micro-vibration unit 100 to a living organism to stimulate the production of adult stem cells in the organism. The pulse wave profile 120 includes three pulses indicated as pulse 1 , pulse 2 and pulse 3 . Although only three pulses are shown, the full pulse wave profile 120 may include many more pulses, such as tens or even hundreds of pulses depending on the length of the treatment. Each pulse (illustrated by pulses 1 , 2 , and 3 ) is typically in the range of one-half to ten seconds in duration, and the time between pulses (illustrated by pulse separation periods 5 and 7 ) and 3 ) is typically in the range of one-tenth to three seconds. In addition, the modulation frequency of the pulses typically varies from pulse to pulse within the range of 1500 Hz to 100 Hz. As shown conceptually in FIG. 2 , the modulation frequency may decrease with each successive pulse. For example, the pulse profile may begin at 1500 Hz, step down with pulse-to-pulse increments of 100 Hz, and end with a final pulse 100 Hz. Of course, this is relatively simple pulse profile provided to illustrate the technique, and many variations may be implemented.
[0058] The inventors believe that the leading edges 4 , 6 and 8 of micro-vibration pulses within the indicated frequency range have the effect of expanding capillaries in the tissues underlying the area of the treatment, and the cessation of the pulses relaxes the capillaries. Therefore, repeated application of the pulse illustrated by pulses 1 , 2 , and 3 has the effect of repeatedly expanding and relaxing the capillaries. The repeated expansion and contraction of the capillaries is believed to have the effect of increasing the delivery of nutrition and oxygen, which has the effect of stimulating the production of adult stem cells in the affected tissue.
[0059] FIG. 3 is a graphical representation of a micro-vibration profile 122 that is similar to the profile 120 , except that it starts at the low frequency end of the range at about 100 Hz, increases in increments of about 100 Hz up to the upper end of the range at about 1500 Hz. Again, each pulses typically has a duration in the range of one-half to ten seconds, and the pulse separation time is typically in the range of one-tenth of a second to three seconds.
[0060] FIG. 4 is a graphical representation of a micro-vibration pulse profile 124 that may be applied through the micro-vibration unit 100 to a living organism to stimulate the production of adult stem cells in the organism. This micro-vibration profile 124 begins with at a very low frequency of about 1 Hz and builds up to about 120 Hz. The duration of the pulse profile 124 can vary from about 30 second to 30 minutes, and can be applied repetitively, as desired. This type of ultra-low frequency treatment is typically applied for three minutes to one hour, and has been found to be suitable for stimulating the production of adult stem cells in muscle and tendon tissue.
[0061] FIG. 6 is a graphical representation of a micro-vibration profile 126 that is similar to the profile 124 , except that starts with at the high frequency end of the range at about 120 Hz, decreases down to the lower end of the range at about 1 Hz. Like the profile 124 , the profile 126 can vary from about 30 second to 30 minutes, and can be applied repetitively, as desired.
[0062] FIG. 7 is a graphical representation of a micro-vibration profile 128 that is a combination of the profiles 120 , 122 , 124 and 126 described above. The inventors have found that a consistent regimen of applying this type of profile once or twice daily over an extended period, such as several months, has the desired effect of stimulating the production of adult stem cells in the a range of tissues, such as muscle, tendon, fat, liver and bone marrow. Of course, the particular profile 128 shown in merely illustrative, and alternative pulse shapes, frequencies, durations and combinations can be applied using the present invention. Nevertheless, it should be appreciated that the profile 128 within the parameters described above has been found to be effective profile for practicing the present invention.
[0063] FIG. 7A is a graphical representation of an area 130 overlying the thoracic spine of a human, and FIG. 7B shows specific points 132 for applying micro-vibration treatments to stimulate the production of adult stem cells within the tissues underlying area 130 . The tissues underlying area 130 include a large portion of the spinal cord, bone marrow, skeletal muscles and fat tissue located along vertebral column staring from C1 vertebra down to the L1 vertebra, and approximately three inches wide along both sides of the vertebral midline.
[0064] FIG. 8A is a graphical representation of an area 140 overlying the front portion of the cranium of a human, and FIG. 8B shows specific points 142 for applying micro-vibration treatments to stimulate the production of adult stem cells within the tissues underlying area 140 . FIG. 9A is a graphical representation of an area 150 overlying the front portion of the cranium of a human, and FIG. 9B shows specific points 152 for applying micro-vibration treatments to stimulate the production of adult stem cells within the tissues underlying area 150 . The tissues underlying the areas 140 and 150 include the brain and bone marrow located on the skull.
[0065] FIG. 10A is a graphical representation of an area 160 overlying the lower spinal area of a human, and FIG. 10B shows specific points 162 for applying micro-vibration treatments to stimulate the production of adult stem cells within the tissues underlying area 160 . The tissues underlying the area 160 includes the spine, bone morrow, skeletal muscles and fat tissue located along vertebral column staring from L1 vertebral body down to S5 vertebral body and approximately three inches to both sides of the vertebral midline.
[0066] FIG. 11A is a graphical representation of an area 170 overlying the lower back area of a human, and FIG. 11B shows specific points 172 for applying micro-vibration treatments to stimulate the production of adult stem cells within the tissues underlying area 170 . The tissues underlying the area 170 includes the bone morrow, skeletal muscles and fat tissue located in the region of both scapulas.
[0067] FIG. 12A is a graphical representation of an area 180 overlying the lower back area of a human, and FIG. 12B shows specific points 182 for applying micro-vibration treatments to stimulate the production of adult stem cells within the tissues underlying area 180 . The tissues underlying the area 180 include the bone morrow, skeletal muscles and fat tissue located in region of the flat bones of pelvis.
[0068] FIG. 13A is a graphical representation of an area 190 overlying a front portion of the abdomen of a human, and FIG. 13B shows specific points 192 for applying micro-vibration treatments to stimulate the production of adult stem cells within the tissues underlying area 190 . FIG. 14A is a graphical representation of an area 194 overlying a rear portion of the abdomen of a human, and FIG. 14B shows specific points 196 for applying micro-vibration treatments to stimulate the production of adult stem cells within the tissues underlying area 194 . The tissues underlying the areas 190 and 194 include the liver, the skeletal muscles and fat tissue in the region of the liver.
[0069] FIG. 15A is a graphical representation of an area 200 overlying the leg area of a human, and FIG. 15B shows specific points 202 for applying micro-vibration treatments to stimulate the production of adult stem cells within the tissues underlying area 200 . The tissues underlying the area 180 include the bone morrow, skeletal muscles and fat tissue located in region of the leg muscles.
[0070] FIG. 16A is a graphical representation of an area 210 overlying the inner arm area of a human, and FIG. 16B shows specific points 212 for applying micro-vibration treatments to stimulate the production of adult stem cells within the tissues underlying area 210 . FIG. 17A is a graphical representation of an area 220 overlying outer arm of a human, and FIG. 17B shows specific points 222 for applying micro-vibration treatments to stimulate the production of adult stem cells within the tissues underlying area 220 . The tissues underlying the areas 210 and 220 include the bone morrow, skeletal muscles and fat tissue located in region of the arm muscles.
[0071] The term “frequency pass” refers to a number of modulated or non-modulated pulses applied by the vibroacoustic device. A modulated pulse is a low frequency pulse filled with higher frequency pulses. The pulses may have any desired shape, such as sinusoidal, rectangular, triangular, and so forth. The modulation frequency may be constant during a pulse (i.e., constant frequency pulse) or the frequency may vary during a pulse (i.e., variable frequency pulse). The modulation frequency may be the same for every pulse (i.e., constant frequency pulse sequence) or the modulation frequency may vary from pulse to pulse (i.e., variable frequency pulse sequence). The amplitude of the micro-vibration signal may also vary within a pulse or from pulse to pulse. A non-modulated pulse is a pulse in which a constant DC value is applied by the vibroacoustic transducer. A rest period is a time between pulses when the vibroacoustic transducers apply no stimulation.
[0072] During a pulse sequence, the pulses may have the same duration (i.e., constant duration pulses) or the duration may vary from pulse to pulse (i.e., variable duration pulses). In addition, the rest period between pulses may remain constant or it may vary from rest period to rest period. A pulse sequence in which the duration of the pulses and the rest periods between the pulses remains the same is referred to as a constant pulse.
[0073] The parameters of a pulse sequence, such as the frequency, amplitude, duration, and number of pulses of the modulated or non-modulated pulses can all be varied to produce different pulse sequences. The term High Frequency (HF) pass refers to a pulse sequence that includes a number of modulated pulses. Unless otherwise notes, the HF pass includes pulses with constant pulse duration and amplitude, where frequency and amplitude change from pulse to pulse within the pass. For example, if modulated frequency starts from 1200 Hz in the pulse # 1 and duration of that pulse is 2 seconds the next pulse # 2 may have modulated frequency of 1995 Hz and duration of that pulse can be 2.01 seconds to keep same number of cycles for each HF pulse. The amplitude of each pulse in a HF pass may also vary from maximum to minimum during the HF pass, typically from 50 to 1000 microns. The rest time between pulses during the HF pass ranges from 0.01 to 0.1 seconds unless a different value is specified.
[0074] The term Low Frequency (LF) pass refers to a pulse sequence that includes non-modulated pulses where frequency and amplitude of the stimulation change smoothly from the beginning to the end of the LF pass. The duration the LF pass varies from 0.5 second to 5 seconds. The frequency applied during the LF pass typically varies from 0.5 Hz to 120 Hz. The term Fixed Frequency (FF) pass or period refers to a period during which the vibroacoustic transducer applies a constant frequency.
[0075] Specific micro-vibration treatment regimen have been developed to reduce symptoms, repair tissue and effect cures for a number of diseases and conditions. The specific treatment regimens can be applied daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0076] Multiple sclerosis. Today, multiple sclerosis is recognized as a chronic, inflammatory, demyelinating autoimmune disease of the Central nervous system (CNS). The disease is characterized by damage to the myelin covering nerve cells and damage to the underlying nerve cell fibers, which leads to slowed or blocked transmission of signals by the nerve cells. The nerve damage causes reduced or lost muscle function. Vibroacoustic stimulation helps to repair the nerve damage caused by multiple sclerosis by stimulating the production of adult stem cells, which repair the nerve cells and the myelin covering nerve cells. The stem cells repair oligodenrocytes, improve nerve cell conduction, open capillaries to provide better blood circulation, and produce an anti-inflammatory effect.
[0077] The vibroacoustic treatment regimen for multiple sclerosis includes a first application applied to the spinal cord, followed by a rest period, followed by a second application applied to the head. The spinal cord application includes a number HF passes, LF passes and FF periods applied to the spinal cord lasting from 30 to 60 minutes. After a rest period of 60 minutes, the second application lasting from 2 to 3 minutes is applied to the head.
[0078] The spinal cord application uses vibroacoustic stimulation for treatment of multiple sclerosis lesions located in spinal cord to achieve micro-vibration in the sound frequencies to the spinal cord. The transducers are placed along the vertebral column staring from C1 vertebral body down to L1 vertebral body and 3 inches wide to the right and 3 inches wide to the left from vertebral midline as shown in FIG. 7B .
[0079] The spinal cord application includes a number of HF and LF passes followed by a 3-minute FF period during which a constant frequency in the range of 350 and 450 Hz is applied. The spinal cord application begins with two HF passes, followed by one LF pass, followed by two more HF passes, and concludes with one FF period. This sequence of passes can be repeated, as desired. The spinal cord application typically includes one sequence (2 HF passes, LF pass, 2 HF passes, one FF period) lasting about 30 minutes, which can be repeated to produce a total first application lasting 60 minutes.
[0080] During the HF pass, each pulse has a duration ranging from 2 to 5 seconds and typically applies a constant frequency during each pulse. The frequency and amplitude typically varies from pulse to pulse during the HF pass. The modulation frequency changes from pulse to pulse from 1100 Hz to 800 Hz or from 800 Hz to 1100 Hz over the pulse sequence. The pulse-to-pulse change in frequency can be selected produce the desired duration for the HF pass. There are a number of parameters that can be changed from pulse to pulse, as desired, including the pulse duration, rest time, and modulation frequency. The duration of the HF pass last from 3 to 5 minutes. The duration of the LF pass is typically from 1 to 5 minutes. During the LF pass, the signal applied by the vibroacoustical transducer varies from smoothly from 1 Hz to 120 Hz or from 120 Hz to 1 Hz over the course of the pass. The total number of HF and LF passes during the first application ranges from 5 to 10 (average 3 min per pass) plus the fixed frequency (FF) interval. The duration of the entire application should not be less than 30 minutes or longer than 60 minutes. The recommended duration for the application is from 30 to 60 minutes
[0081] After a rest period of about an hour, the second application is applied to the head as shown in FIGA. 8 B and 9 B. The head application includes one HF pass in which the frequency varies from pulse to pulse starting from 1100 Hz and ending with 900 Hz or in reverse order from 900 Hz to 1100 Hz. The duration of each pulse can vary from 1.5 seconds to 2 seconds. The rest time between each modulated pulse during the HF pass can vary and should not be not less than about 0.2 seconds. The number of modulated pulses is from 30 to 60 pulses. The duration of the head application is from 2 to 3 minutes.
[0082] Migraine headache. Researchers believe that migraine headaches may be caused by functional changes in the trigeminal nerve system, which is a major pain pathway in your nervous system, and by imbalances in brain chemicals, including serotonin, which plays a regulatory role for pain messages going through this pathway. During a migraine headache, serotonin levels drop. Researchers believe this causes the trigeminal nerve to release substances called neuropeptides, which travel to the brain's outer covering known as the meninges. There the neuropeptides cause blood vessels to become dilated and inflamed. The result is a migraine headache pain.
[0083] The Vibroacoustic stimulation for treatment for migraine headache involves transmitting micro-vibration in the sound frequencies to the brain and meningeal membranes. The vibroacoustic treatment stimulate the production of adult stem cells that repair never cells, improve nerve cell fiber conduction, and provide better blood circulation in the trigeminal nerve system.
[0084] The treatment regimen for migraine headache includes one HF pass applied to the head as shown in FIGS. 8B and 9B . During the HF pass, this modulation frequencies applied start from 1100 Hz and end with frequency of 700 Hz or in reverse order from 700 Hz to 1100 Hz. The duration of each pulse can vary from 1 seconds to 2 seconds. The number of modulated pulses is from 30 to 60 pulses. The duration of the application is from 1 to 2 minutes. This treatment regimen can be applied daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0085] Benign Prostatic Hypertrophy (BPH). It is common for the prostate gland to become enlarged as a man ages. Doctors call this condition benign prostatic hyperplasia (BPH), or benign prostatic hypertrophy. The micro-vibration treatment regimen for BPH includes vibroacoustic stimulation to suppress alpha-sympathetic nervous system to cause bladder neck relaxation to improve urea flow and decrease prostate volume by improving blood circulation in the relevant area. Vibroacoustic stimulation for treatment of BPH is designed to achieve transmission of micro-vibration in the sound frequencies to the prostate. The vibroacoustic transducers are located in a first area about 5 inches above ramie pubis (pelvic bone in front) and 8 inches wide to the right and 8 inches wide to the left from abdominal midline. Additional transducers can also be placed in a second area from the base of the penis to the anus about two inches wide to the right and 2 inches wide to the left from pelvic midline. The treatment regimen can be applied simultaneously to the first and second areas, or it can be applied to each area in separate treatments.
[0086] The treatment regimen for BPH includes a number HF passes, LF passes and a FF period with modulation at 400 Hz at the end of application. The total application time from 30 to 35 minutes. The application starts with three LF passes 3 to 5 minutes long separated by rest periods of 10 seconds. The LF passes are followed by two HF passes 3 to 5 minutes long separated by a rest period of 10 seconds. This is followed by another LF pass 3 to 5 minutes in duration, followed by 5 to 10 pulses about one second in duration each with modulation frequency of 400 Hz. Each frequency of the vibroacoustic stimulation applied during the LF pass varies from 3 Hz to 100 Hz. The duration of each LF pass is no less than 3 minutes. The frequency of LF smoothly changes from 3 Hz to 100 Hz.
[0087] The High frequency pass consists of pulses with duration of 2 seconds and modulation starting at 1200 Hz and change to conclude the HF pass at 600 Hz.
[0088] Spinal cord injury. The treatment regimen for spinal cord injury will use vibroacoustic stimulation to increase the production of adult stem cells to repair glial cells and neurons in the spinal cord and improve nerve cell fiber conduction. The transducers are placed near the spinal cord in the area of the injury, for example as shown in FIG. 10B . The application can also be applied along vertebral column staring from C1 vertebral body down to L1 vertebral body and 3 inches wide to the right and to the left from vertebral midline or direct on the vertebral column as shown in FIG. 7B . The treatment regimen consists of number HF and LF passes followed by 5 one-second FF periods with modulation at 400 Hz at the end of application. The sequence of HF and LF passes is as follows: 2 HF passes followed by 2 LF passes. After those four passes, there will be a 10 second rest period. After the rest period, 3 HF passes followed by 1 LF pass. Thereafter there will be an additional 5-second FF period with modulation at 400 Hz at the end of application. During the HF pass, each pulse has constant frequency and amplitude, and the frequency and amplitude vary from pulse to pulse. The duration of each HF pass is from 3 to 5 minutes, the duration of each HF pulse varies from 1 to 2 seconds, and the modulation frequency varies from 1200 Hz to the 400 Hz or from 400 HZ to the 1200 Hz over the course of the HF pass. The rest time between HF modulated pulses is from 0.1 to 0.2 seconds. The amplitude of the micro-vibration varies from 50 microns to 1000 microns. The amplitude of LF non-modulated pulses varies from 300 to 2000 microns. The total application time from 24 to 28 minutes.
[0089] Peripheral neuropathy. Peripheral neuropathy is a problem with the nerves that carry information to and from the brain and spinal cord. This produces pain, loss of sensation, and inability to control muscles. The treatment regimen for peripheral neuropathy uses vibroacoustic stimulation to increase the production of adult stem cell to repair myelin, repair nerve cells, improve nerve fiber conduction, and provide better blood circulation in the treatment area. The treatment area includes the location where an affected peripheral nerve originates and along the length of the nerve.
[0090] The treatment regimen for peripheral neuropathy consists of number (typically 5) of HF passes followed by a number of LF passes (typically 2), followed by 5 one-second FF periods with modulation at 400 Hz at the end of application. The HF pass includes constant amplitude and frequency pulses that vary in frequency from pulse to pulse. The modulation frequency ranges from 1400 Hz to minimum 100 Hz per during the HF pass. The frequency applied during the LF pass varies from 4 Hz to 30 Hz. The application concludes with 5 one-second 5 periods modulated at 400 Hz. There is a rest period of at least 5 seconds between each HF pass.
[0091] The amplitude of HF modulated pulses is constant during each pulse and varies from pulse to pulse from 200 to 1000 microns. The amplitude of stimulation during the LF pass varies from 500 to 2000 microns. The total application time from 18 to 20 minutes.
[0092] Parkinson's disease. Parkinson's disease (PD) belongs to a group of conditions called motor system disorders, which are the result of the loss of dopamine-producing brain cells. The four primary symptoms of PD are tremor, or trembling in hands, arms, legs, jaw, and face; rigidity, or stiffness of the limbs and trunk; bradykinesia, or slowness of movement; and postural instability, or impaired balance and coordination.
[0093] The treatment regimen for Parkinson's disease will use vibroacoustic stimulation to increase adult stem cell production to improve function of dopamine-producing neurons, improve nerve cell conduction and increase blood circulation in the treatment area.
[0094] The treatment regimen includes two applications. The first application is applied along vertebral column staring from C1 vertebral body down to L1 vertebral body and 3 inches wide to the right and to the left from vertebral midline or direct on the vertebral column as shown in FIG. 7B . The first application includes a number passes of HF passes, a number of LF passes, and 5 one-second pulses with fixed frequency (FF) modulation of 400 Hz at the end of application. The sequence of HF and LF passes is as follows: 2 passes of HF followed by 1 pass of LF. After those four passes, there will be a 30 second rest period. Then 1 pass of HF followed by five one-second pulses with fixed frequency (FF) modulation of 400 Hz at the end of application. The duration per application should not exceed 15 minutes. The amplitude of micro-vibration varies from 200 microns to 1000 microns.
[0095] The second application consists of one or two HF passes applied to the head as shown in FIGS. 8B and 9B . The HF pass includes constant frequency pulses that vary in frequency from pulse to pulse. The modulation frequency starts at 1100 Hz and ends at 800 Hz or in reverse order from 800 Hz to 1100 Hz. The duration of each pulse can vary from 2 seconds to 3 seconds. The number of modulated pulses is from 30 to 60 pulses. The duration of the second application is from 1 to 3 minutes. The amplitude of HF modulated pulses varies from 50 to 200 microns.
[0096] Functional Constipation. Constipation is defined as having a bowel movement fewer than three times per week. Functional constipation means that the bowel is healthy but not working properly. Colonic inertia, delayed transit, and pelvic floor dysfunction are three types of functional constipation. Colonic inertia and delayed transit are caused by a decrease in muscle activity in the colon. These syndromes may affect the entire colon or may be confined to the lower, or sigmoid, colon. Pelvic floor dysfunctions are caused by a weakness of the muscles in the pelvis surrounding the anus and rectum. However, because this group of muscles is voluntarily controlled to some extent, biofeedback training is somewhat successful in retraining the muscles to function normally and improving the ability to have a bowel movement.
[0097] Functional constipation that stems from problems in the structure of the anus and rectum is known as anorectal dysfunction, or anismus. These abnormalities result in an inability to relax the rectal and anal muscles that allow stool to exit.
[0098] The treatment regimen #1 for colonic inertia uses vibroacoustic stimulation to stimulate autonomous and somatic nervous system to cause colonic muscle activation. Treatment regimen #2 for pelvic floor dysfunction uses vibroacoustic stimulation to stimulate somatic nervous system to cause pelvic muscle activation Treatment regimen #3 for anorectal dysfunction, or anismus uses vibroacoustic stimulation to stimulate autonomous and somatic nervous system to cause colonic muscle and pelvic muscle relaxation.
[0099] Treatment regiment #1 consists of 4 or 5 HF passes with modulated frequency starting from 1300 Hz and ending with frequency of 600 Hz or in reverse order from 600 Hz to 1300 Hz. The duration of each pulse can vary from 1 seconds to 2 seconds. The duration for application between 12 and 15 minutes. The transducers are placed 8 inches above ramie pubis (pelvic bone in front) and 8 inches wide to the left from abdominal midline. Additional transducers can be placed in the area from the base of the crotch to the anus 2 inches wide to the right and 2 inches wide to the left from pelvic midline. This regimen can be applied to both areas simultaneously or with separate treatments.
[0100] Treatment regiment #2 consists of a number of HF passes of pulses modulated by High Frequency (HF) and Low Frequency (LF) without modulation, and ending application with 5 pulses of fixed frequency modulation of 400 Hz. The duration of each pulse during the HF pass is approximately 1 second. The sequence order of HF and LF passes is as follows: 1 LF pass starting at 3 Hz and ending at 100 Hz or in reverse order from 100 Hz to 3 Hz. The duration of LF passes is approximately 5 minutes. After the LF pass is finished there is a rest period of approximately 10 seconds followed by 3 HF passes. The modulation frequencies for HF pulses starts at 1500 Hz and end at 200 Hz. The duration of each HF pass is from 2.5 to 3 minutes with a rest period of about 10 seconds between passes. The HF passes are followed by another LF pass, followed by 5 one-second FF periods with modulation at 400 Hz at the end of application. The duration for application is between 24 and 26 minutes. The transducers placed in the area from the base of the crotch to the tale bone 2 inches wide to the right and 2 inches wide to the left from pelvic midline.
[0101] Treatment regiment #3 consists of number of HF passes, a number of LF passes, and ends application with 5 one-second FF periods with modulation at 400 Hz. The duration of each pulse during the HF pass is approximately 2 seconds. The sequence order of HF and LF is as follows: 3 HF passes with modulation frequencies ranging from 1500 Hz to 100 Hz or in reverse order from 100 Hz to 1500 Hz. The HF passes are followed by one LF pass in which the frequency ranges from 3 Hz to 100 Hz or in reverse order from 100 Hz to 3 Hz. The duration of the LF pass is approximately 3 to 5 minutes followed by 5 one-second FF periods with modulation at 400 Hz at the end of application. The amplitude of HF modulated pulses varies from 200 to 1000 microns. The amplitude of the stimulation applied during the LF pass varies from 500 to 2000 microns. The application time is from 20 to 22 minutes. The transducers placed in the area from the base of the crotch to the tale bone 2 inches wide to the right and 2 inches wide to the left from pelvic midline.
[0102] Urge incontinence (Over Active bladder). Urge incontinence is a sudden, intense urge to urinate, followed by an involuntary loss of urine. The bladder muscle contracts and may give a warning of only a few seconds to a minute to reach a toilet. With urge incontinence, there may also be a need to urinate often, sometimes several times a night. Some people with urge incontinence have a strong desire to urinate when they hear water running or after they drink only a small amount of liquid. Simply going from sitting to standing may even cause urine to leak. Urge incontinence may be caused by a urinary tract infection or by anything that irritates the bladder. It can also be caused by bowel problems or damage to the nervous system associated with multiple sclerosis, Parkinson's disease, Alzheimer's disease, stroke or injury. In urge incontinence, the bladder is said to be “overactive”—it's contracting even when your bladder isn't full. In fact, urge incontinence is often called an overactive bladder.
[0103] The treatment regimen for urge incontinence uses vibroacoustic stimulation to suppress autonomous nervous system to cause bladder muscle relaxation. The regimen consists of number (approximately 5) LF passes, followed by 1 HF, followed by 5 one-second FF periods with modulation at 400 Hz at the end of application. The LF passes start from 3 Hz and end with 200 Hz or in reverse order from 200 Hz to 3 Hz. The duration of each LF pass is around 3 minutes. The modulation frequencies for the HF pass starts from 1500 Hz and end at 200 Hz. The duration of HF pass is from 3 to 4 minutes follow by 5 one-second pulses with fix frequency modulation of 400 Hz at the end of application. The amplitude of HF modulated pulses varies from 100 to 500 microns. The amplitude of LF modulated pulses varies from 500 to 2000 microns. The duration of the application from 18 to 22 minutes. The transducers are placed 6 inches above ramie pubis (pelvic bone in front) and 6 inches wide to the right and 6 inches wide to the left from abdominal midline.
[0104] Essential tremor. Essential tremor is an unintentional, somewhat rhythmic muscle movement involving to-and-fro movements (oscillations) of one or more parts of the body. Essential tremor (sometimes called benign essential tremor) is the most common of the more than 20 types of tremor. The treatment regimen for essential tremor uses vibroacoustic stimulation to stimulate motor nerve system. The regimen consists of one or two HF passes with modulated frequency starting from 1200 Hz and ending with frequency of 800 Hz or in reverse order from 800 Hz to 1200 Hz. The duration of each pulse can vary from 1.5 seconds to 2 seconds. The number of modulated pulses is from 30 to 60 pulses. The duration of the application is from 2 to 3 minutes. The amplitude of HF modulated pulses varies from 150 to 300 microns. Location is the same as for migraine headache as shown on FIGS. 8B and 9B .
[0105] In addition, micro-vibration treatment regimens have been developed for application to specific areas of the body.
[0106] Micro-vibration Treatment Regimen No. 1. The application area for Micro-vibration Treatment Regimen No. 1 includes the bone marrow and spinal cord located on or along vertebral column staring from C1 vertebral body down to L1 vertebral body and 3 inches wide to the right and to the left from vertebral midline as shown in FIG. 7B .
[0107] The therapeutic effects for Micro-vibration Treatment Regimen No. 1 include decreased mitosis time leading to increased stem cell multiplication in the application area; mobilization of stem cells and migration of stem cells into peripheral circulation in the application area; stem cells reaching peripheral circulation exhibiting less differentiation with more plasticity; and increased conductivity and enhanced signal to noise ratio in neural pathways in the spinal cord.
[0108] The application algorithm for Micro-vibration Treatment Regimen No. 1 includes one or more modulated multi-pulse application cycles referred to as a high frequency pass (HF pass). Each HF pass typically lasts from 1 to 5 minutes with an average of about 3 minutes per HF pass. The total minimum number of HF passes during an application can range from 1 to 12 HF passes with the lengths of the HF passes varying and having an average time of about 3 minutes per pass. The total duration of each application should be in the range of 3 minutes (for one HF pass) and up to about 60 minutes total. The average recommended duration of the application is from 15 to 60 minutes. Applications can be repeated with several hours between applications. Typical regimens include applications daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0109] The frequency range for Micro-vibration Treatment Regimen No. 1 is 1500 Hz to 600 Hz, which may decrease in 100 Hz pulse-to-pulse increments from 1500 HZ to 600 HZ during a HF pass, or it may increase from 600 Hz to 1500 Hz in 100 Hz pulse-to-pulse increments during a HF pass. The amplitude of the excitation ranges from 50 to 1000 microns and may change with frequency. For example, the amplitude may ramp from 100 microns at 1500 Hz to 1000 microns at 600 Hz, or the amplitude may ramp from 1000 microns at 600 Hz to 100 microns at 1500 Hz. The pulse width duration is typically from 0.1 to 5 seconds for each pulse, and the rest time between pulses is typically from 0.01 sec to 0.1 seconds.
[0110] Micro-vibration Treatment Regimen No. 2. The application area for Micro-vibration Treatment Regimen No. 2 includes the bone marrow and spinal cord located on or along vertebral column staring from C1 vertebral body down to L1 vertebral body and 3 inches wide to the right and to the left from vertebral midline as shown in FIG. 7B .
[0111] The therapeutic effects for Micro-vibration Treatment Regimen No. 2 include stem cells mobilization and forced to peripheral circulation and decreased conductivity of neural pathways in spinal cord depending on application duration.
[0112] The application algorithm for Micro-vibration Treatment Regimen No. 2 includes the application of pulses with or without modulation from 1.0 seconds to 0.008 seconds and from 0.008 seconds to 1.0 seconds. Each pass duration is from 1 to 5 minutes. The Low Frequencies (LF) pass consist of from 1 Hz to 120 Hz and from 120 Hz to 1 Hz. Total minimum number of LF passes 1 to 12, where is low frequencies smoothly changed from 1 Hz to 120 Hz or from 120 Hz to 1 Hz. The duration each LF pass no less than 1 minute and no more than 5 minutes. Application should not be less when 1 minutes and no longer than 60 minutes. Typical regimens include applications daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0113] The frequency range for Micro-vibration Treatment Regimen No. 2 is 1 Hz to 120 Hz or 120 Hz to 1 Hz non-modulated low frequency. The amplitude of the micro-vibration in microns range from about 10 up to 1000 Microns in the sweep from 1 Hz to 120 Hz or from 120 Hz to 1 Hz non-modulated. Pulse Width during Sweep range from 1 sec to 0.008 sec for sweep from 1 Hz to 120 Hz and from 0.008 sec to 1 sec for a sweep from 120 Hz to 1 Hz.
[0114] Micro-vibration Treatment Regimen No. 3. The application area for Micro-vibration Treatment Regimen No. 3 includes the bone marrow n and spinal cord located on or along vertebral column staring from C1 vertebral body down to L1 vertebral body and 3 inches wide to the right and to the left from vertebral midline as shown in FIG. 7B .
[0115] The therapeutic effects for Micro-vibration Treatment Regimen No. 3 include decreased mitosis time leading to increase stem cell multiplication in the application area; stem cell mobilization and migration of stem cells into peripheral circulation; stem cells entering peripheral circulation that are less differentiated with more plasticity; and increased conductivity and enhanced signal to noise ratio in neural pathways in spinal cord or decrease conductivity of neural pathways in spinal cord depending on preponderance of duration and quantity of HF and LF passes.
[0116] The application algorithm for Micro-vibration Treatment Regimen No. 3 consists of a mix of regimens described in Micro-vibration Treatment Regimen Nos. 1 and 2 in any order. Typical regimens include applications daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0117] The frequency range for Micro-vibration Treatment Regimen No. 3 is 1500 to 600 Hz or 600 to 1500 Hz Modulated (High Frequency) and 1 Hz to 120 Hz or 120 Hz to 1 Hz non-modulated. The amplitude of micro-vibration in microns range from 50 to 1000 microns change with frequency from 100 microns at 1500 Hz and 1000 microns at 600 Hz. Pulse width during the sweep include a combination of pulse duration from 0.1 to 5 seconds for each pulse at modulated sweep (HF) and 1 sec to 0.008 sec for sweep from 1 Hz to 120 Hz and from 0.008 sec to 1 sec for a sweep from 120 Hz to 1 Hz (LF). Rest time between modulated pulses during HF pass (sweep) width minimum is 0.01 sec and max 0.1 sec. Typical regimens include applications daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0118] Micro-vibration Treatment Regimen No. 4. The application area for Micro-vibration Treatment Regimen No. 4 includes the bone marrow and spinal cord located on or along vertebral column staring from C1 vertebral body down to L1 vertebral body and 3 inches wide to the right and to the left from vertebral midline as shown in FIG. 7B .
[0119] The therapeutic effects for Micro-vibration Treatment Regimen No. 4 includes decreased mitosis time leading to increase stem cell multiplication. Simultaneously stem cell located in bone marrow of the spinal cord experience faster mobilization and migrate into peripheral circulation less differentiated with more plasticity without stimulating nerve pathways in the application area.
[0120] The application algorithm for Micro-vibration Treatment Regimen No. 4 includes pulse widths from 1 to 5 seconds with modulation frequency from 1200 Hz to 800 Hz in desired increments to fit pulse width, where pulse duration can be change from pulse to pulse. This is referred to as the High Frequency (HF) pass. The time between each pulse inside HF has a pause from 0.1 sec to 2 seconds. Each pass from 2 to 4 minutes long. Total minimum number of passes 5 (average 3 to 4 minutes per pass). The duration of the entire application should not be less when 2 minutes (for one pass) and not longer than 120 minutes. Average recommended duration for application from 15 to 30 minutes. Typical regimens include applications daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0121] The frequency range for Micro-vibration Treatment Regimen No. 4 is 1200-800 modulated or 800 Hz to 1200 Hz (HF pass) and 2 to 120 Hz or 120 to 2 Hz (LF pass) non-modulated. Amplitude of micro-vibration in microns range from 50 to 1000 microns change with frequency from 100 microns at 1200 Hz and 1000 microns at 800 Hz and up to 2000 Microns in the sweep from 2 Hz to 120 Hz non-modulated. Pulse width during the pass is from 0.1 to 5 seconds for each pulse at modulated HF sweep and for LF sweep from 0.5 to 0.008 seconds. Rest time between modulated pulses during HF pass ranges from 0.1 to 2.0 seconds between pulses with modulation during HF sweep and no pause during LF sweep from 2 Hz to 120 Hz non-modulated. The Algorithm consists of mix of regimen described in Micro-vibration Treatment Regimen Nos. 1 and 2 in any order.
[0122] Micro-vibration Treatment Regimen No. 5. The application area for Micro-vibration Treatment Regimen No. 5 includes bone marrow located on the skull and brain as shown in FIGS. 8B and 9B .
[0123] The therapeutic effects for Micro-vibration Treatment Regimen No. 5 include vibroacoustic stimulation of stem cells located in bone marrow causing decreased mitosis time leading to increased stem cell multiplication. This regimen can also be used to stimulate adult neural stem cells to decrease the occurrence and severity of headaches.
[0124] The application algorithm for Micro-vibration Treatment Regimen No. 5 includes a HF pass with pulse width 1 to 5 seconds with modulation frequency from 1100 Hz to 600 Hz in desired increments to fit the pulse width, where the pulse duration can be changed from pulse to pulse. The time between each pulse inside HF has a pause from 0.1 sec to 2 seconds. Each HF pass from 0.5 to 4 minutes long for a minimum number of 1 or 2 passes. The duration of the entire application should not be less than 0.5 minutes (for one pass) and not longer than 10 minutes. Typical regimens include applications daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0125] The frequency range for Micro-vibration Treatment Regimen No. 5 is 1100-600 or 600 to 1100 Hz modulated. The amplitude of the micro-vibration in microns range from 10 to 200 microns and change with frequency. The pulse width ranges from 0.1 to 3 seconds for each pulse at modulated HF pulses. Rest time between modulated pulses during HF pass ranges from 0.1 to 3.0 seconds.
[0126] Micro-vibration Treatment Regimen No. 6 The application area for Micro-vibration Treatment Regimen No. 6 includes bone marrow located in the skull and brain as shown in FIGS. 8B and 9B .
[0127] The therapeutic effects for Micro-vibration Treatment Regimen No. 6 include vibroacoustic stimulation of stem cells located in bone marrow resulting in decreased mitosis time leading to increased stem cell multiplication. This regimen can also be used to help dissolve a cerebral hematoma.
[0128] The application algorithm for Micro-vibration Treatment Regimen No. 6 includes a HF pass with pulse width ranging from 1 to 5 seconds with modulation frequency ranging from 1500 Hz to 200 Hz in desired increments to fit pulse width, where pulse duration can be changed from pulse to pulse. The rest time between each pulse during the HF pass ranges from 0.1 sec to 2 seconds. The duration of each pass ranges from 2 to 4 minutes with a minimum number of 4 passes 4 (average 2 to 4 minutes per pass). The duration of entire application should not be less than 6 minutes (for one pass) and not longer than 15 minutes per application. Typical regimens include applications daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0129] The frequency range for Micro-vibration Treatment Regimen No. 6 ranges from 1500 to 100 Hz or 100 to 1500 Hz modulated (HF pass). The amplitude of micro-vibration in microns range from 100 microns at frequency 1500 Hz and 300 Microns at frequency 100 Hz. The pulse width ranges from 0.1 to 2 seconds for each pulse. The rest time between modulated pulses ranges from 0.1 to 3.0 seconds between pulses.
[0130] Micro-vibration Treatment Regimen No. 7. The application area for Micro-vibration Treatment Regimen No. 7 includes bone marrow located along vertebral column staring from L1 vertebral body down to S5 vertebral body and 3 inches wide to the right and to the left from vertebral midline as shown in FIG. 10B .
[0131] The therapeutic effects for Micro-vibration Treatment Regimen No. 7 include decreased mitosis time leading to increased stem cell multiplication; simultaneously stem cells located in bone marrow experience increased mobilization and migration into peripheral circulation less differentiated with more plasticity; improvement of blood circulation in application area.
[0132] The application algorithm for Micro-vibration Treatment Regimen No. 7 includes a HF pass with pulse width ranging from 1 to 5 seconds with modulation frequency ranging from 1200 Hz to 100 Hz in desire increment to fit pulse width, where the pulse duration can change from pulse to pulse. The time between each pulse of the HF pass should not be less than 0.01 seconds. Each pass extends from 2 to 4 minutes with a minimum number of 5 passes (average 3 min per pass). The duration of the entire application should not be less than 3 minutes (for one pass) and not longer than 120 minutes. The average recommended duration for the application is 15 to 30 minutes. Typical regimens include applications daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0133] The frequency range for Micro-vibration Treatment Regimen No. 1 is 1200-100 Hz or 100-1200 Hz modulated. The amplitude of micro-vibration in microns range from 100 microns to 1000—at frequency 1200 Hz and up to 2000 Microns at frequency 100 Hz. The pulse width ranges from 0.1 to 7 seconds. The rest time between modulated pulses ranges from 0.1 to 1.0 seconds between pulses.
[0134] Micro-vibration Treatment Regimen No. 8. The application area for Micro-vibration Treatment Regimen No. 8 includes bone marrow located along vertebral column staring from L1 vertebral body down to S5 vertebral body and 3 inches wide to the right and to the left from vertebral midline as shown in FIG. 10B .
[0135] The therapeutic effects for Micro-vibration Treatment Regimen No. 8 include stem cells mobilization and migration into peripheral circulation. Pain is reduced in application area.
[0136] The application algorithm for Micro-vibration Treatment Regimen No. 8 includes LF pass ranging from 1 Hz smoothly changing up to 100 Hz. The amplitude of micro-vibration can vary from 100 microns to 2000 microns and may depend on the type of transducer used. The pulse duration ranges from 1 second to 0.1 second with rest time between pulses ranging from 0.01 to 0.1 seconds. Typical regimens include applications daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0137] The frequency range for Micro-vibration Treatment Regimen No. 8 is 1 to 100 Hz or 1 to 100 Hz non-modulated (LF pass). The amplitude of micro-vibration in microns ranges from 100 to 2000 microns during LF sweep from 1 Hz to 100 Hz or 100 Hz to 1 Hz. The pulse width during ranges from 0.01 to 0.1 sec between pulses without modulation during (LF) sweep. Rest time between modulated pulses during HF pass (sweep) Width From 0.01 to 0.1 seconds between pulses without modulation during (LF) sweep.
[0138] Micro-vibration Treatment Regimen No. 9. The application area for Micro-vibration Treatment Regimen No. 9 includes bone marrow located along vertebral column staring from L1 vertebral body down to S5 vertebral body and 3 inches wide to the right and to the left from vertebral midline as shown in FIG. 10B .
[0139] The therapeutic effects for Micro-vibration Treatment Regimen No. 9 include stem cells mobilization and migration into peripheral circulation and reduced pain in application area.
[0140] The application algorithm for Micro-vibration Treatment Regimen No. 9 includes a combination of HF and LF passes. The duration of the HF modulated pulses can range from 0.1 sec to 7 seconds with a total duration of the HF sweep ranging from 3 to 10 minutes. The duration of the HF sweep may be altered depending on the type of application and weight of the person receiving the treatment. Persons having lower weight typically receive treatments with shorter duration. The rest time between pulses ranges from 0.01 to 1 second. The rest time should be sufficient to allow reduced polarization during stimulated chemical reaction inside the scull and a release of stem cells into the peripheral circulation. Typical regimens include applications daily or several times per day for as long as the therapeutic effect is desired, typically an extended period of weeks, months or years.
[0141] The frequency range for Micro-vibration Treatment Regimen No. 9 ranges from 2000 to 100 modulated or 100 to 2000 Hz (HF pass) and 1 to 100 Hz or 1 to 100 Hz (LF pass) non-modulated. The amplitude of micro-vibration in microns ranges from 100 to 2000 microns during LF pass 1 to 100 Hz or 1 to 100 Hz non-modulated and 100 to 1000 on HF pass 2000 to 100 or 100 to 2000 Hz modulated. The pulse width during the HF sweep ranges from 0.1 to 7 seconds and from 1 second to 0.01 second during the LF pass. The rest time between modulated pulses during HF pass ranges from 0.1 to 1 second between pulses during the HF pass and 0.1 to 0.2 sec for the LF pass.
[0142] It should be understood that the preceding regimens are illustrative of the types of treatments that have been found to be therapeutic, but that the specific parameters of the treatment may be varied within the scope of the invention as defined by the following claims. In view of the foregoing, it will be appreciated that present invention provides significant improvements for stimulating the growth of adult stem cells for a variety of therapeutic purposes. | A method and device for using topically applied acoustical vibrations to stimulate the production of adult stem cells in living organisms. This approach is non-invasive, and more specifically does not involve introducing chemicals or physically invading the organisms. One or more acoustical transducers are placed directly on the skin of the organism in certain locations, and selected vibration profiles are applied to the organism through the transducers. The treatment includes the regular application of various vibration pulse profiles that generally include sequences of pulses in which each pulse has a duration in the range of one-half to ten seconds, is separated by rest periods in the range of one-tenth to three seconds, is modulated with an oscillatory signal in the frequency range of 1 Hz to 1,500 Hz, and has a pulse amplitude in the range of range from about 20 to 5000 microns. | 0 |
BACKGROUND OF THE INVENTION
1. Field of the Invention. The present invention relates generally to deburring tools, more specifically to deburring tools capable of deburring the outer edge and the inner edge of a cylindrically shaped object, and more particularly to deburring tools which can be utilized to deburr the inner and outer edges of hollow tubing such as a cartridge shell.
2. Description of the Prior Art. Previous inventors have directed their efforts toward providing reaming and deburring tools some of which use angular deburring tools, some of which are known as chasers and reamers, hand reamers, tube working tools for deburring the ends of tubes, and special manual reamers for thin-wall tubing. While each of the tools just mentioned includes angled reaming devices, each of the tools is either quite limited in its use or so complex as to make use by a layperson difficult. None of the prior art of which applicant is aware has taught a deburring tool having the unique features, capabilities and construction of the present invention which allow its use in deburring simultaneously both the inner and the outer edges of the end of hollow tubing such as that used in cartridge shells.
SUMMARY OF THE INVENTION
The present invention consists of a double deburring tool which can be used in simultaneously deburring the inner and outer edges of a cartridge shell, including a cleaning device for cleaning the cap recess of the cartridge shell and the firing hole through which the cap ignites powder in the cartridge shell, and further including means for cleaning the interior of the cartridge shell. The device in one embodiment includes a base which can be clamped to a bench and a rotatable head having blades properly positioned so that, as the rotatable head is turned, the blades deburr the inner and outer edges of a properly positioned cartridge shell. The device further includes adjusting means whereby the deburring tool can be adjusted to deburr simultaneously the inner and outer edges of tubing and/or cartridge shells of different sizes.
One of the objects of the present invention is to provide a deburring tool capable of simultaneously deburring the inner and outer edges of hollow tubing such as a cartridge shell or the like.
Another object of the present invention is to provide a deburring tool having an adjustment capability to allow its use in deburring the inner and outer edges of tubing of different sizes by adjustment of the deburring tool.
A further object of the present invention is to provide a deburring tool specifically for use in deburring cartridge shells for reloading purposes.
Another object of the present invention is to provide a deburring tool which includes an adaptor capable of cleaning out the cap recess of a cartridge shell.
A further object of the present invention is to provide a deburring tool which includes an adaptor for cleaning the interior of tubing and/or cartridge shells.
Another object of the present invention is to provide a versatile deburring tool which can be constructed to be portable in nature and adapted to a multitude of circumstances.
The foregoing objects, as well as other objects and benefits of the present invention, are made more apparent by the descriptions and claims which follow.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view showing the construction of the deburring tool showing it in position to deburr the end of a cartridge shell.
FIG. 2 is an expanded section view showing the specific structure of the section of the deburring tool utilized in deburring the cartridge shell or hollow tubing.
FIG. 2A is a cross-sectional view taken along lines 2A--2A of FIG. 2 showing the construction of the inner deburring blade.
FIG. 2B is a cross-sectional view taken along lines 2B--2B of FIG. 2 showing the construction of the outer deburring blade.
FIG. 3 is an assembly view showing the adaptor utilized for cleaning a cap recess positioned on the end of the deburring tool.
FIG. 4 is a side view showing a brush which is adaptable for use with the deburring tool in cleaning the interior of a piece of tubing or cartridge shell.
FIG. 5 is an assembly view showing the structure and use of the adaptor for cleaning the cap recess of a cartridge shell.
FIG. 6 is a side view showing the structure of the deburring tool.
FIG. 7 is an end view of the deburring tool cone showing the positioning of the blades involved in deburring the outer edge and the blades involved in deburring the inner edge of a shell or piece of tubing simultaneously.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 of the drawings is a perspective view showing the deburring tool 10 positioned to deburr the end of a cartridge shell 29. The deburring tool 10 has a base 11 together with a deburring cone 22. Base 11 is provided with a clamp consisting of a relieved section 18 with a rigidly positioned jaw 19 at one end and an adjustable jaw 17 positioned at the other end. Adjustable jaw 17 is attached to threaded rod 15, and threaded rod 15 extends through a threaded hole in wall 53 so that, as threaded rod 15 is turned, adjustable jaw 17 moves toward or away from jaw 19 along arrow D. Threaded rod 15 has a handle 16 enabling it to be turned easily as shown by arrow C. Deburring cone 22 includes a rod 20 which is substantially rigidly attached thereto. Rod 20 passes through a hole 21 in base 11 as shown and attaches to arm 12 by means of a screw or other appropriate attaching means. Arm 12 has a handle 13 pivotally attached thereto by means of a screw or pin 14. When arm 12 is turned along arrow A, deburring cone 22 turns on axis H as shown by arrow B. Deburring cone 22 includes a cone 42 and multiple outer blades 24, as well as multiple inner blades 34 shown in other views of the drawings. The inner blades 34 are not generally adjustable, but the outer blades 24 are captured in slots within deburring tool 22 and by means of slots in outer blades 24 into which nut 23 fits so that, as nut 23 is turned on threads 52 of deburring cone 22, the outer blades 24 move back and forth along arrow F, thereby changing the point at which they intersect cone 42 of deburring cone 22. For purposes of utilizing deburring cone 22 with deburring tool 10 to deburr a cartridge shell 29 as shown, a positioning tool 25 is provided which consists of a base 26 with an extension 27 attached thereto. Extension 27 has a point 28 positioned thereon so that, as extension 27 is pushed inside of cartridge shell 29 and positioned properly, it will extend through the igniting hole 51 of cartridge shell 29. Deburring cone 22, rod 20 and positioning tool 25 are all substantially concentrically located on axis H so that they turn on axis H.
FIG. 2 of the drawings is an expanded sectional view utilizing a cutaway view of cone 42 of deburring cone 22, together with a cross-sectional view of cartridge shell 29 and base 26 of positioning tool 25. Deburring cone 22 has slots 35 into which blades 24 fit. While only one slot 35 is shown in the cutaway of FIG. 2, such slots are provided for each of the outer blades 24. The method of capturing outer blades 24 in slots 35 is shown in FIG. 2B of the drawings. Outer blades 24 also have slots 36 cut therein so that, if outer blades 24 are positioned in slots 35 of deburring cone 22, threaded nut 23 is positioned so that it captures outer blades 24 in slots 36. Inner blades 34 are also positioned in cone 42 of deburring cone 22 in slots as shown in FIG. 2A of the drawings. Deburring cone 22 further includes a threaded extension 32 at the end of cone 42 and a nut 33. Base 26 of positioning tool 25 has a threaded hole 31 in the end thereof whereby positioning tool 25 is attached to threaded extension 32 of deburring cone 22. The diameter of base 26 of positioning tool 25 is such that it approximates the inner diameter of the end of cartridge shell 29 so that it tends to hold the shell casing in position during deburring. The angles of the cutting edge 30 of outer blades 24 and the cutting edge of inner blades 34 are set to deburr the inner and outer edges of cartridge shell 29 simultaneously. Nut 23 is adjusted to position outer blades 24 against the outer edge of cartridge shell 29 when cartridge shell 29 is pushed in until it contacts inner blades 34. The angle I of cutting edge 30 of blade 24 to the wall of cartridge shell 29 was set at substantially 35 degrees in this embodiment, but any angle sufficient to facilitate deburring of the outer edge of the wall of cartridge shell 29 could be used. The angle J of the cutting edge of blade 34 to the wall of cartridge shell 29 was set at substantially 25 degrees in this embodiment, but any angle sufficient to facilitate deburring of the inner edge of the wall of cartridge shell 29 could be used.
FIG. 2A is a cross-sectional view of cone 42 taken along lines 2A--2A of FIG. 2 showing an inner blade 34 positioned in slot 48 of cone 42. There is an expanded opening 57 at the edge of slot 48 which facilitates insertion of an inner blade 34 with an expanded edge 61. Expanded edge 61 is provided to capture inner blade 34 in slot 48.
FIG. 2B is a cross-sectional view of cone 42 taken along lines 2B--2B of FIG. 2 showing an outer blade 24 positioned in slot 35 of cone 42. There is an expanded opening 59 at the edge of slot 35 which facilitates insertion of outer blade 24 with an expanded edge 60. Expanded edge 60 is provided to capture outer blade 24 in slot 35.
Expanded edges 60 and 61 of outer blade 24 and inner blade 34 respectively are created by pressure applied to the edges of the blades 24 and 34 until they expand or by any other acceptable method of providing an expanded edge.
FIG. 3 of the drawings shows cone 42 of deburring cone 22 together with threaded extension 32 and nut 33. Further shown is a cap recess cleaning tool 37 having a center section 54 with an enlarged section 38 at one end and cleaning blades 40 at the opposite end. An extension 41 which fits inside of igniting hole 51 of a cartridge shell 29 is provided at the end of cleaning blades 40. Cap recess cleaning tool 37 has a threaded hole 37 so that it can be screwed onto threaded extension 32 of deburring tool 22. Once in position, extension 41 may be inserted into igniting hole 51 of a cartridge shell 29. Once in position, blades 40 of cap recess cleaning tool 37 clean the inside of the cap recess when cap recess cleaning tool 37 is turned.
FIG. 4 is a side view showing a brush unit 43 for cleaning the interior of a cartridge shell 29. It includes a base 44 having a threaded hole 45 so that it can be screwed onto extension 32 of deburring cone 22 and an extension 47 to which a brush 46 is attached. When cleaning brush 43 is attached to the threaded extension 32 of deburring tool 22 and handle 13 is turned, brush 46 turns, thereby cleaning the interior of cartridge shell 29 in which it is positioned.
FIG. 5 is an assembly view showing the use of cap recess cleaning tool 37 to clean a cap recess 50 in cartridge shell 29. Extension 41 of cap recess cleaning tool 37 extends through igniting hole 51 of cartridge shell 29, thereby cleaning igniting hole 51 and centering cap recess cleaning tool 37 so that, when cap recess cleaning tool 37 is turned, the blades 40 clean out cap recess 50. Cap recess cleaning tool 37 includes a threaded hole 39 designed to facilitate attachment to threaded extension 32 of deburring cone 22.
FIG. 6 of the drawings is a top view of the body of deburring cone 22 without any blades positioned therein. Slot 35, into which outer blade 24 extends from cone 42 of deburring cone 22, extends well into threads 52 of deburring cone 22. Threaded extension 32 is substantially rigidly attached to cone 42, and a nut 33 is provided to act as a stop for holding positioning tools and other tools on the end of deburring cone 22 as well as preventing inner blades 34 from coming out of slots 48.
FIG. 7 of the drawings is an end view of the cone 42 of deburring cone 22. FIG. 7 particularly shows the positioning of inner blades 34, which deburr the inside edge of a cartridge shell 29, and the positioning of outer blades 24, which deburr the outer edge of a cartridge shell 29, during use. FIG. 7 further shows the layout of slots 48 utilized to hold inner blades 34 in position and slots 35 utilized to capture outer blades 24. Nut 33 is also utilized to hold blades 34 in position as shown in FIGS. 2 and 5 of the drawings. The outer blades 24 are positioned about axis H and threaded extension 32, which is positioned on axis H at substantially 120 degrees from each other, and inner blades 34 are positioned about axis H and threaded extension 32, which is positioned on axis H at substantially 120-degree intervals. All of the blades utilized are positioned substantially equiangularly about axis H so that, when six blades are used as in this embodiment, a blade of one sort or the other is positioned at substantially every 60 degrees about the axis H established by threaded extension 32.
While the foregoing description of the invention has shown a preferred embodiment using specific terms, such description is presented for illustrative purposes only. It is applicant's intention that changes and variations may be made without departure from the spirit or scope of the following claims, and this disclosure is not intended to limit applicant's protection in any way. | A deburring tool is provided having two sets of blades for use in simultaneously deburring the inner and outer edges of a piece of tubing, further including adjustment capability allowing the use of the tool in deburring tubing of different sizes, further including a cap recess cleaning tool, a cleaning brush and a base for mounting the deburring tool on a bench, table or the like. | 8 |
This application is a divisional of 08/761,934 filed Dec. 9, 1996 now U.S. Pat. No. 5,907,039.
FIELD OF THE INVENTION
The present invention relates to a method for preparing 2-acylamino alcohol derivatives which have a function to enhance or inhibit biosynthesis of glycolipids and also have antiviral, antitumor, metastasis inhibition and nerve cell growth enhancing functions. Furthermore, the present invention relates to novel amino alcohol derivatives which are useful in preparing the 2-acylamino alcohol derivatives.
BACKGROUND OF THE INVENTION
A 2-acylamino alcohol derivative, 2-decanoylamino-3-morpholino-1-phenyl-1-propanol (hereinafter referred to as “PDMP”), represented by the following formula:
has an activity to control biosynthesis of glycolipids, but the activity is greatly different among its four stereoisomers. Therefore, separation of its optically active isomers is carried out by a method in which decanoylaminoacetophenone is condensed with morpholine by Mannich reaction and then reduced with sodium borohydride to obtain PDMP as a mixture of four stereoisomers, resolution of the diastereomers is effected by a crystallization method and then optical resolution of the racemic compounds is effected by a crystallization method ( J. Lipid. Res., 28:565-571 (1987), and Advances in Lipid Research, 26:183-213 (1993)).
SUMMARY OF THE INVENTION
An object of the present invention is to provide a process for preparing optically active substances of PDMP having plural asymmetric centers and its analogues using a chiral compound as the starting material at high efficiency, particularly a stereoselective synthesis process which requires no complicated optical resolution step.
Another object of the present invention is to provide novel amino alcohol derivatives which are useful for preparing PDMP and its analogues.
In order to develop a simple and general stereoselective process for preparing PDMP and its analogues, the inventors of the present invention have conducted intensive studies and found as the results that all of the four stereoisomers of PDMP or its analogues can be stereoselectively synthesized by establishing synthetic steps which comprise stereochemically proceeding reactions using, as the main starting material and asymmetric source, an N-protected 2-aminopropanediol which has two asymmetric centers in its molecule in advance and whose amino group is protected with a urethane type protecting group which can be obtained at a reasonable price as a reagent for peptide synthesis use, and have also found novel amino alcohol derivatives as intermediates of the synthetic steps. The present invention has been accomplished based on these findings.
Accordingly, these and other objects of the present invention have been accomplished by a process for preparing a 2-acylamino alcohol derivative which comprises the following steps:
(A) reacting an aminopropanol derivative represented by the following formula (1):
Y—CH 2 —C*H(NHP 1 )—C*H(OH)—R 1 (1)
wherein * represents an asymmetric carbon atom;
P 1 represents an alkyl group or an amino-protecting group;
R 1 represents an alkyl group, a cycloalkyl group or an aryl group; and
Y represents a leaving group,
with an amine represented by R 2 H, wherein R 2 is represented by the following formula (I) to (VI), to synthesize an amino alcohol derivative represented by the following formula (2):
R 2 —CH 2 —C*H(NHP 1 )—C*H(OH)—R 1 (2)
wherein P 1 , R 1 and R 2 each has the same meaning as those defined above,
(B) leaving P 1 from said amino alcohol derivative represented by formula (2) to synthesize an amino alcohol derivative represented by the following formula (3):
R 2 —CH 2 —C*H(NH 2 )—C*H(OH)—R 1 (3)
wherein R 1 and R 2 each has the same meaning as those defined above, and
(C) reacting said amino alcohol derivative represented by formula (3) with a carboxylic acid represented by R 11 COOH or a reactive derivative thereof, wherein R 11 represents an alkyl or alkenyl group having from 3 to 18 carbon atoms which may be substituted with a hydroxyl group, to prepare a 2-acylamino alcohol derivative represented by the following formula (4):
R 2 —CH 2 —C*H(NHCOR 11 )—C*H(OH)—R 1 (4)
wherein R 1 , R 2 and R 11 each has the same meaning as those defined above;
wherein R 3 and R 4 are the same or different and each represents a hydrogen atom, a lower alkyl group, a lower alkenyl group, a hydroxyl-lower-alkyl group, a lower alkoxyalkyl group, an amino-lower-alkyl group, a cycloalkyl group, a hydroxycycloalkyl group, an aralkyl group or a piperazino group which may be substituted with a lower alkyl group;
R 5 represents a hydrogen atom or at least one substituents which are the same or different and are selected from a hydroxyl group, a lower alkyl group, a lower alkoxyl group, a hydroxyl--lower-alkyl group, a carboxyl group, a (lower alkoxyl)carbonyl group, an aralkyl group, a piperidino group, an acyloxy group, an amino group and an amino-lower-alkyl group;
R 6 represents a hydrogen atom or at least one substituents which are the same or different and are selected from the substituents as defined in R 5 ;
R 7 represents a lower alkylene group which may be discontinued by an oxygen atom;
R 8 and R 9 are the same or different and each represents a hydrogen atom, a lower alkyl group or a hydroxyl-lower-alkyl group, or R 8 and R 9 represent, together with a nitrogen atom to which they are bound, a piperidino group or a morpholino group which may be substituted with a lower alkyl group;
m is an integer of 2 to 6;
p is an integer of 2 or 3; and
X represents the following formula (VII) or (VIII):
wherein R 10 represents a hydrogen atom, a lower alkyl group, an acyl group, a (lower alkoxyl)carbonyl group or a pyridyl group.
Furthermore, these and other objects of the present invention have been accomplished by the amino alcohol derivatives represented by formula (2).
Moreover, these and other objects of the present invention have been accomplished by the amino alcohol derivatives represented by formula (3).
DETAILED DESCRIPTION OF THE INVENTION
In the present invention, the term “lower” in the “lower alkyl”, “lower alkoxyl” and the like means that the carbon number thereof is from 1 to 6.
Also, the term “alkylene group which may be discontinued by an oxygen atom” means that at least two alkylene groups are linked to each other via at least one oxygen atom.
PDMP and its analogues, have been discovered as glycolipid biosynthesis controlling substances are interesting compounds which also have physiological functions such as antiviral, antitumor, metastasis inhibition, nerve cell growth enhancing and the like. Structurally, they have 2-amino alcohol as the basic nucleus and at least two asymmetric carbon atoms in the molecule. Since functions of four stereoisomers obtained therefrom are different from each other, it is necessary to develop a means for the stereoselective synthesis of these four isomers in studying relationship between structure and function of PDMP and its analogues and developing high active analogues.
As described above, one aspect of the present invention relates to a process for stereoselectively synthesizing the four stereoisomers of PDMP and its analogues using, as the main starting material, a 2-aminopropanediol derivative which has two asymmetric carbon atoms in its molecule and whose amino group is protected with a urethane type protecting group. This process is based on the following new findings.
That is, the stereoselective synthesis of PDMP and its analogues has been achieved by 1) using a chiral compound having two asymmetric carbon atoms in its molecule as the starting material, 2) introducing a leaving group (a mesyl group or the like) into only primary hydroxyl group among primary and secondary hydroxyl groups, and then substituting the leaving group with a primary or secondary amine and 3) constructing all of the reaction steps as keeping the stereochemistry.
The present invention will be described according to the following synthetic steps.
According to the process of the present invention, an optically active aminopropanol derivative represented by formula (1) is used as the starting material. In formula (1), R 1 is an alkyl group, a cycloalkyl group or an aryl group having from 6 to 15 carbon atoms such as phenyl or the like, preferably a phenyl group which may be substituted with 1 to 3 substituents which are the same or different and are selected from a lower alkyl group, a lower alkoxyl group, a hydroxyl group, a hydroxyl-lower-alkyl group and a nitro group (e.g., a phenyl group, a dimethoxyphenyl group, a dihydroxyphenyl group), and more preferably a phenyl group. P 1 is an alkyl group having from 3 to 18 carbon atoms such as a decyl group or an amino-protecting group (e.g., a benzyloxycarbonyl group which may be substituted with a nitro group, a halogen atom, a lower alkoxyl group, a (lower alkoxyl)phenylazo group or a phenylazo group; an alkoxycarbonyl group containing a straight, branched or cyclic alkyl group having from 1 to 15 carbon atoms which may be substituted with a fluorenyl group or a methylsulfonyl group; or the like). Specific examples thereof include benzyloxycarbonyl groups which may have a substituent(s) (e.g., a benzyloxycarbonyl group, a p-nitrobenzyloxycarbonyl group, a p-bromobenzyloxycarbonyl group, a p-methoxybenzyloxycarbonyl group, a p-methoxyphenylazobenzyloxycarbonyl group and the like), alkoxycarbonyl groups which may have a substituent(s) (e.g., a t-butoxycarbonyl group, a cyclopentyloxycarbonyl group, an octyloxycarbonyl group, a 9-fluorenylmethoxycarbonyl group, a methylsulfonylethoxycarbonyl group and the like) and amino-protecting groups such as a benzenesulfonyl group and the like, Y represents a leaving group such as a methanesulfonyl (mesyl) group, a trihalogenomethanesulfonyl group (e.g., a trifluoromethanesulfonyl group), a p-toluenesulfonyl group, a benzenesulfonyl group, a p-bromobenzenesulfonyl group or the like.
The aminopropanol derivatives represented by formula (1) can be obtained by treating the optically active N-protected-2-aminopropanediol shown in the above synthesis steps as “compound (a)” with methanesulfonyl chloride (Ms-Cl) or the like in a solvent (e.g., pyridine or the like) or in an anhydrous solvent (e.g., dichloromethane or the like) in the presence of pyridine at a range between an ice-cooled temperature and room temperature to effect methanesulfonylation (mesylation) of only primary hydroxyl group of the diol (step 1). The compound represented by formula (2) can be prepared by treating the product obtained in, step 1 after isolation, or without isolation in some cases, with an amine represented by formula R 2 H in an organic solvent (e.g., ethyl alcohol, N,N-dimethylformamide or the like) (step 2). In the amine represented by formula R 2 H, R 2 represents a group represented by formula (I) to (VI) described above and in formula (I) to (VI), carbon numbers of a cycloalkyl group or a hydroxycycloalkyl group are from 3 to 8 and those of an aralkyl group are from 6 to 20. Preferably, R 2 is a morpholino group, a (lower alkyl)amino group, a (morpholino-lower alkyl)amino group, a cycloalkylamino group which may be substituted with a hydroxyl group, a pyrrolidino group which may be substituted with a hydroxyl group or a hydroxyl-lower-alkyl group, a piperazino group which may be substituted with a lower alkyl group, a bis(hydroxyl-lower-alkyl)amino group or a piperidino group which may be substituted with a hydroxyl group or a hydroxyl-lower-alkyl group, and more preferably a group or a pyrrolidino group.
In step 3, the alkyl group or amino protecting group which protects the amino group is removed by a usual method such as catalytic reduction, acid treatment, base treatment or the like to obtain the compound represented by formula (3), Next, the amino group thus formed is acylated with a carboxylic acid represented by formula R 11 COOH or a reactive derivative thereof such as an acid halide or acid anhydride of a carboxylic acid or the like to obtain the 2-acylamino alcohol derivative represented by formula (4) (step 4). In the above formula R 11 COOH, R 11 is an alkyl or alkenyl group having from 3 to 18 carbon atoms which may have a hydroxyl group at the 2- or 3-position. When the acyl group (R 11 CO—) to be introduced has 10 carbon atoms, decanoyl chloride or decanoic anhydride is used as the above-described acylating agent. Alternatively, the objective 2-acylamino alcohol derivative represented by formula (4) can be obtained by reacting the compound represented by formula (3) with a carboxylic acid (R 11 COOH) having from 8 to 16 carbon atoms and a condensing agent usually used in an amido bonding reaction (step 4). Examples of the carboxylic acid include fatty acids and hydroxyl-substituted fatty acids such as octanoic acid, 2-hydroxyoctanoic acid, decanoic acid, 2-hydroxydecanoic acid, dodecanoic acid, 2-hydroxydodecanoic acid, myristic acid, 2-hydroxymyristic acid, palmitic acid, 2-hydroxypalmitic acid and the like. Examples of the condensing agent include dicyclohexylcarbodiimide, water-soluble carbodiimide and the like. Examples of the water-soluble carbodiimide include 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC).
Examples of the amino alcohol derivatives represented by formula (2) include
(a) derivative wherein R 1 is an alkyl group or a cycloalkyl group, or a phenyl group which may be substituted with from 1 to 3 substituents which are the same or different and are selected from a lower alkyl group, a lower alkoxyl group, a hydroxyl group, a hydroxyl-lower-alkyl group and a nitro group; and P 1 is an alkyl group having from 3 to 18 carbon atoms or an amino-protecting group selected from (i) a benzyloxycarbonyl group which may be substituted with a nitro group, a halogen atom, a lower alkoxyl group, a (lower alkoxyl)phenylazo group or a phenylazo group and (ii) an alkoxycarbonyl group containing a straight, branched or cyclic alkyl group which may be substituted with a fluorenyl group or a methylsulfonyl group,
(b) derivatives wherein R 1 is an alkyl group having from 6 to 15 carbon atoms, a cyclohexyl group or a phenyl group; P 1 is a decyl group or an amino-protecting group selected from a benzyloxycarbonyl group, a t-butoxycarbonyl group and an octyloxycarbonyl group; and R 2 is an amino group selected from a morpholino group, a (lower alkyl)amino group, a (morpholino-lower alkyl)amino group, a cycloalkylamino group which may be substituted with a hydroxyl group, a pyrrolidino group which may be substituted with a hydroxyl group- or a hydroxyl-lower-alkyl group, a piperazino group which may be substituted with a lower alkyl group, a bis(hydroxyl-lower-alkyl) amino group and a piperidino group which may be substituted with a hydroxyl group or a hydroxyl-lower-alkyl group,
(c) derivatives wherein R 1 is a phenyl group; P 1 is a benzyloxycarbonyl group; and R 2 is a morpholino group, a pyrrolidino group, a hydroxypyrrolidino group, hydroxypiperidino group, a an N-methylpiperazino group, a diethanolamino group or a hydroxycyclohexylamino group; and wherein their configuration is (1S,2S), and
(d) derivatives wherein R 1 is a phenyl group; P 1 is a benzyloxycarbonyl group; and R 2 is a morpholino group, a pyrrolidino group, a piperidino group, a cyclohexylamino group or a cyclopentylamino group; and wherein their configuration is (1R,2R).
Examples of the amino alcohol derivatives represented by formula (3) include derivatives wherein R 1 is an alkyl group having from 6 to 15 carbon atoms, a cyclohexyl group or a phenyl group; and R 2 is a morpholino group, a (lower alkyl)amino group, a (morpholino-lower alkyl)amino group, a cycloalkylamino group which may be substituted with a hydroxyl group, a pyrrolidino group which may be substituted with a hydroxyl group or a hydroxyl-lower-alkyl group, a piperazino group which may be substituted with a lower alkyl group, a bis(hydroxyl-lower-alkyl) amino group or a piperidino group which may be substituted with a hydroxyl group or a hydroxyl-lower-alkyl group.
According to the present invention, the product of each production step may be isolated. In some cases, the objective 2-acylamino alcohol derivative represented by formula (4) can be obtained by using as the starting material an optically active diol which is the raw material of formula (1), and carrying out the above-described stepwise reactions in succession without isolating the product of each step.
The synthesis methods of N-protected-2-aminopropanediols to be used as the raw material of the amino alcohol derivative represented by formula (1) which is the starting material in the process of the present invention include a method in which an aminoketone is reduced ( J. Org. Chem., 54:1866 (1989)), a method in which an N-(diphenylmethylene)amino acid ester is treated with diisobutylaluminum hydride and then with a Grignard's reagent ( J. Org. Chem., 57:5469 (1992)), a method in which an acid chloride of an N-protected-aminoaldehyde or N-protected-amino acid is treated with an organometallic reagent ( J. Am. Chem. Soc., 95:4098 (1973)), an asymmetric aldol reaction of 2-oxazolidinone with aldehyde ( J. Am, Chem. Soc., 108:6757 (1986)) (Evans method) and an asymmetric aldol reaction of chiral imidazolidinone and oxazolidinone with aldehyde ( Helv. Chem. Acta, 70:237 (1987)).
On the other hand, N-protected-α-aminoketones to be used as the raw material of N-protected-2-aminopropanediols may be synthesized, for example, by a method in which an N-protected-α-amino acid is used as the starting material, and the carboxyl group of the amino acid is converted into an acid chloride and then allowed to undergo Friedel-Crafts' reaction with benzene ( J. Am. Chem. Soc., 103:6157 (1981)) or a method in which the carboxyl group of the amino acid is treated with an alkyl lithium reagent to convert it into a lithium salt and then allowed to react with a Grignard's reagent ( J. Org. Chem., 54:1866 (1989)).
Thus, according to the present invention, optically active substances of PDMP and its analogues having a plurality of asymmetric centers can be synthesized efficiently by using an N-protected-2-aminopropanol derivative as the starting material without requiring complex optical resolution. In other words, the present invention is markedly useful, because all of the four stereoisomers of PDMP and its analogues can be synthesized stereoselectively. In addition, the novel amino alcohol derivatives of the present invention have plural asymmetric centers and therefore are markedly useful as a synthesis intermediate of PDMP and its analogues.
The present invention is now illustrated in greater detail by way of the following examples, but it should be understood that the present invention is not to be construed as being limited thereto. The term “MeOH”, “AcOEt”, “AcOH”and “DMF” as used hereinafter mean “methanol”, “ethyl acetate”, “acetic acid” and “N,N-dimethylformamide”, respectively.
EXAMPLES
Example 1
Synthesis of (1S,2S)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester:
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol (21.2 g, 70.3 mmol) was dissolved in pyridine (350 ml), and methanesulfonyl chloride (5.6 ml, 72.3 mmol) was added dropwise thereto on an ice bath over a period of 5 minutes. The resulting mixture was stirred for 30 minutes on the ice bath and then overnight at room temperature. After confirming completion of the reaction with TLC (chloroform : methanol =20:1), the solvent was removed by evaporation, and ethyl acetate (500 ml) was added thereto. The residue thus obtained was washed with 1 N HCl (250 ml×3 times) and brine (250 ml), and then dried over anhydrous sodium sulfate to evaporate the solvent. The crystals thus precipitated were washed with a mixture of ethyl acetate and n-hexane (1:1) to obtain the objective compound as white crystals (25.3 g, yield: 95.0%).
TLC Rf:
0.55 (CHCl 3 : MeOH =20:1 ), 0.83 (AcOEt), 0.62 )n-Hexane : ACOEt =1:2)
1 H-NMR (CDCl 3 )δ:
7.35-7.26 (10 H, m, aromatic), 5.30 (1 H, d, J=7.81 Hz, NH), 5.02 (2H, s, C H 2 —O—CO), 4.99 (1 H, d, J=3.91 Hz, C H —OH), 4.43-4.39, 4.22-4.12 (3 H , m, N—C H —C H 2 ), 2.98 (3 H, s, SO 3 CH 3 )
Example 2
Synthesis of (1S,2S)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester:
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol (15.4 g, 51.0 mmol) was dissolved in methylene chloride (150 ml), pyridine (12.1 ml, 149.6 mmol) was added thereto, and then methanesulfonyl chloride (4.5 ml, 58.1 mmol) was added dropwise thereto on an ice bath over a period of 5 minutes. The mixture thus prepared was stirred for 30 minutes on the ice bath and then overnight at room temperature. After confirming completion of the reaction with TLC (chloroform methanol =20:1, n-hexane : ethyl acetate =1:1) , water (100 ml) and chloroform (50 ml) were added thereto. The resulting organic layer was washed with each 100 ml of 1 N hydrochloric acid, water, a saturated sodium bicarbonate solution and water in this order, dried over anhydrous sodium sulfate and then filtered. The solvent was removed by evaporation, and 100 ml of a mixture of n-hexane and ethyl acetate (2:1) was added thereto and allowed to stand overnight. The crystals thus precipitated were collected by filtration and washed with a mixture of n-hexane and ethyl acetate (2:1) to obtain the objective compound as white crystals (16.56 g, yield: 85.7%).
Example 3
Synthesis of (1S,2S)-2-benzyloxycarbonylamino-3-morpholino-1-phenyl-1-propanol:
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (9.68 g, 25.5 mmol) was dissolved in ethanol (50 ml), morpholine (9.8 ml, 112.6 mmol) was added thereto at room temperature, and the obtained mixture was stirred at 40° C. for 3 days. After confirming completion of the reaction with TLC (chloroform:methanol=20:1, n-hexane:ethyl acetate=1:2, ethyl acetate), the solvent was removed by evaporation, and then water (50 ml) and ethyl acetate (150 ml) were added thereto. The resulting organic layer was washed with a saturated sodium bicarbonate solution, water and brine in this order, dried over anhydrous sodium sulfate and then filtered. The solvent was removed by evaporation and the resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:2) to obtain the objective compound as a colorless oily material (3.61 g, yield: 38.1%).
TLC Rf: 0.32 (CHCl 3 :MeOH=20:1), 0.12 (n-Hexane:AcOEt=1:2)
1 H-NMR (CDCl 3 ) δ: 7.38-7.26 (10H, m, aromatic), 5.04 (2H, s, CH 2 O—CO), 5.00 (1H, d, J=3.41 Hz, H-1), 4.11 (1H, m, H-2), 3.72 (4H, m, (CH 2 ) 2 O), 2.68-2.47 (6H, m, (CH 2 ) 3 N)
Example 4
Synthesis of (1R,2R)-2-benzyloxycarbonylamino-3-morpholino-1-phenyl-1-propanol:
(1R,2R)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (1.21 g, 3.19 mmol) was dissolved in N,N-dimethylformamide (6 ml), morpholine (1.11 g, 12.8 mmol) was added thereto at room temperature, and the mixture thus obtained was stirred at 40° C. for 24 hours. After confirming almost completion of the reaction with TLC (chloroform:methanol=20:1, n-hexane:ethyl acetate=1:2, ethyl acetate), a saturated sodium bicarbonate solution (70 ml) and ethyl acetate (100 ml) were added thereto, and the resulting organic layer was washed with water and brine in this order, dried over anhydrous sodium sulfate and then filtered. The solvent was removed by evaporation and the resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:2) to obtain the objective compound as a colorless oily material (507.5 mg, yield: 43.0%).
Example 5
Synthesis of (1S,2S)-2-amino-3-morpholino-1-phenyl-1-propanol:
(1S,2S)-2-Benzyloxycarbonylamino-3-morpholino-1-phenyl-1-propanol (438.8 mg, 1.19 mmol) was dissolved in methanol (10 ml), 10% palladium-carbon (126.5 mg, 10.0 mol %) was added thereto, and the mixture thus obtained was stirred overnight at room temperature in an atmosphere of hydrogen. After confirming completion of the reaction with TLC (chloroform:methanol=9:1 and 7:3), palladium-carbon was removed by filtration and the resulting filtrate was concentrated to obtain the objective compound as a colorless oily material (275.6 mg, yield: 98.5%).
TLC Rf: 0.48, 0.24 (CHCl 3 :MeOH=7:3) (tailing), 0.68 (CHCl 3 :MeOH:aqNH 3 =4:1:trace)
1 H-NMR (CD 3 OD) δ: 7.36-7.26 (5H, m, aromatic), 4.47 (1H, d, J=6.60 Hz, H-1), 3.65 (4H, m, (CH 2 ) 2 O), 3.21-3.14 (1H, m, H-2), 2.51-2.43, 2.32-2.24, 2.11-2.05 (6H, m, (CH 2 ) 3 N)
Example 6
Synthesis of (1S,2S)-2-amino-3-morpholino-1-phenyl-1-propanol:
(1S,2S)-2-Benzyloxycarbonylamino-3-morpholino-1-phenyl-1-propanol (3.82 g, 10.3 mmol) was dissolved in methanol (10 ml), ammonium formate (2.6 g, 41.3 mmol) and 10% palladium-carbon (888.5 mg, 8.09 mol %) were added thereto, and the mixture thus obtained was stirred overnight at room temperature. After confirming completion of the reaction with TLC (chloroform:methanol=9:1 and 7:3), palladium-carbon was removed by filtration and the resulting filtrate was concentrated to obtain the objective compound as a colorless oily material (2.34 g, yield: 99.0%).
Example 7
Synthesis of (1S,2S)-2-decanoylamino-3-morpholino-1-phenyl-1-propanol:
(1S,2S)-2-Amino-3-morpholino-1-phenyl-1-propanol (1.33 g, 4.0 mmol) was dissolved in methanol (4 ml), and decanolyl chloride (0.82 ml, 4.0 mmol) was added thereto in the presence of triethylamine (668.0 μl, 4.8 mmol) under ice cooling. Thirty minutes thereafter, almost completion of the reaction was confirmed with TLC (ethyl acetate, chloroform:methanol=20:1, chloroform:methanol=7:3), and then methanol (30 ml) was added thereto allowed to stand for 90 minutes. After concentration of the reaction solution under a reduced pressure, a saturated sodium bicarbonate solution (20 ml) was added thereto, and extraction was conducted with ethyl acetate (50 ml). The resulting organic layer was washed with water (20 ml) and brine (20 ml), dried over anhydrous sodium sulfate and then concentrated under a reduced pressure to obtain an oily material (853.5 mg). The oily material thus obtained was purified by silica gel column chromatography (ethyl acetate) to obtain the objective compound as a colorless oily material (930.5 mg, yield: 59.6%).
TLC Rf: 0.62 (CHCl 3 :MeOH=9:1), 0.26 (AcOEt) 1 H-NMR (CDCl 3 ) δ: 7.38-7.26 (5H, m, aromatic), 5.87 (1H, d, J=7.26 Hz, NH), 4.95 (1H, d, J=3.63 Hz, H-1), 4.28 (1H, m, H-2), 3.72 (4H, m, (CH 2 ) 2 O), 2.63-2.44 (6H, m, (CH 2 ) 3 N), 2.09 (2H, m, CO—C H 2 —CH 2 ), 1.50 (2H, m, CO—CH 2 —C H 2 ), 1.24 (12H, brs, (C H 2 ) 6 CH 3 ), 0.88 (3H, t, CH 3 )
Example 8
Synthesis of (1S,2S)-2-decanoylamino-3-morpholino-1-phenyl-1-propanol:
(1S,2S)-2-Amino-3-morpholino-1-phenyl-1-propanol (84.9 mg, 0.270 mmol) was dissolved in tetrahydrofuran (4 ml), decanoic anhydride (109.2 mg, 0.334 mmol) was added thereto in the presence of triethylamine (80.0 μl, 0.575 mmol) under ice cooling, and the mixture thus obtained was stirred for one day at room temperature. After confirming almost completion of the reaction with TLC (ethyl acetate, chloroform:methanol=20:1, chloroform:methanol=7:3), ethyl acetate (30 ml) and a saturated sodium bicarbonate solution (20 ml) were added thereto, and the resulting organic layer was washed with water (20 ml) and brine (20 ml), dried over anhydrous sodium sulfate and then concentrated under a reduced pressure to obtain an oily material (130.8 mg). The thus obtained oily material was purified by silica gel column chromatography (ethyl acetate) to obtain the objective compound as a colorless oily material (37.2 mg, yield: 40.5%).
Example 9
Synthesis of (1S,2S)-2-decanoylamino-3-morpholino-1-phenyl-1-propanol:
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (9.5 g, 25.1 mmol) was dissolved in ethanol (50 ml) on an oil bath (40° C.), morpholine (8.7 ml, 100 mmol) was added thereto, and the mixture thus obtained was stirred at 40° C. for 3 days. After confirming almost completion of the reaction with TLC (n-hexane:ethyl acetate=1:2), the solvent was removed by evaporation under a reduced pressure. Ethyl acetate (100 ml) was added to the resulting residue, and the crystals thus precipitated were removed by filtration. The resulting filtrate was washed with a saturated sodium bicarbonate solution (50 ml), water (50 ml×2 times) and brine (50 ml) and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under a reduced pressure to obtain an oily material (13.7 g).
Methanol (50 ml) and 10% palladium-carbon (2.3 g, 8.6 mol %) were added to the oily material, and vigorously stirred overnight in a atmosphere of hydrogen. After confirming completion of the reaction with TLC (ethyl acetate, chloroform:methanol=9:1, chloroform:methanol=7:3), palladium-carbon was removed by filtration and the resulting filtrate was concentrated to obtain an oily material (9.33 g).
The oily material thus obtained was dissolved in methanol (25 ml), triethylamine (4.2 ml, 30 mmol) was added thereto, and then decanoyl chloride (5.15 ml, 25 mmol) was added dropwise thereto under ice cooling. Thirty minutes thereafter, it was confirmed that the reaction was almost completed with TLC (ethyl acetate, chloroform:methanol=20:1, chloroform:methanol=7:3), and then methanol (20 ml) was added thereto and allowed to stand for 30 minutes. The reaction solution was concentrated under a reduced pressure, a saturated sodium bicarbonate solution (50 ml) was added thereto, and extraction was conducted with ethyl acetate (150 ml). The resulting organic layer was washed with water (40 ml×3 times) and brine (40 ml), dried over anhydrous sodium sulfate and then concentrated under a reduced pressure to obtain an oily material (9.73 g). Thereafter, the oily material was purified by silica gel column chromatography (ethyl acetate) to obtain the objective compound as a colorless oily material (4.35 g, yield: 44.6%).
Example 10
Synthesis of (1S,2S,2′S)-2-(2′-hydroxydecanoylamino)-3-morpholino-1-phenyl-1-propanol and (1S,2S,2′R)-2-(2′-hydroxydecanoylamino-3-morpholino-1-phenyl-1-propanol:
(1S,2S)-2-Amino-3-morpholino-1-phenyl-1-propanol (141.5 mg, 0.600 mmol) was dissolved in methylene chloride (6 ml), 2-hydroxydecanoic acid (100 mg, 0.531 mmol) and N-hydroxysuccinimide (150.8 mg, 1.131 mmol) were added thereto, and the mixture thus obtained was stirred at room temperature for 15 minutes. 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (134.0 mg, 0.699 mmol) was added thereto on an ice bath and stirred overnight. After confirming almost completion of the reaction with TLC (ethyl acetate, chloroform:methanol=20:1), ethyl acetate (30 ml) was added thereto, the resulting organic layer was washed with a 5% citric acid solution (15 ml), a saturated sodium bicarbonate solution (15 ml) and water (15 ml) in this order and dried over anhydrous sodium sulfate, the solvent was removed by evaporation under a reduced pressure. The crude product thus obtained was purified by silica gel column chromatography (ethyl acetate, chloroform:methanol=20:1) to obtain the objective compounds as colorless oily materials (15.6 mg as the (1S,2S,2′S) compound and 20.0 mg as the (1S,2S,2′R) compound). In this case, absolute configuration of the objective compounds were identified by carrying out the same synthetic procedure using (2)-2-hydroxydecanoic acid as the raw material. (1S,2S,2′S)-2-(2′-Hydroxydecanoylamino)-3-morpholino-1-phenyl-1-propanol:
TLC Rf: 0.38 (AcOEt)
1 H-NMR (CDCl 3 ) δ: 7.36-7.25 (5H, m, aromatic), 6.82 (1H, d, J=7.81 Hz, NH), 4.96 (1H, d, J=3.41 Hz, H-1), 4.3 (1H, m, H-2), 3.99 (1H, dd, J=3.90, 3.91 Hz, H-2′), 3.71 (4H, t, (CH 2 ) 2 O), 2.64-2.49 (6H, m, (CH 2 ) 3 N), 1.70-1.65 (1H, m, CH(OH)—C H 2 (A)), 1.50-1.43 (1H, m, CH(OH)—C H 2 (B)), 1.31-1.20 (12H, m, (C H 2 ) 6 —CH 3 ), 0.88 (3H, t, CH 3 )
13 C-NMR(CDCl 3 ) δ: 174.3 140.8, 128.4, 127.7, 126.0, 75.2, 72.0, 66.9, 59.9, 54.4, 51.0, 34.8, 31.8, 29.4, 29.2, 24.8, 22.6, 14.1
(1S,2S,2′R)-2-(2′-Hydroxydecanoylamino)-3-morpholino-1-phenyl-1-propanol:
TLC Rf: 0.20 (AcOEt)
1 H-NMR (CDCl 3 ) δ: 7.37-7.25 (5H, m, aromatic), 6.88 (1H, d, J=8.3 Hz, NH), 5.00 (1H, d, J=3.41 Hz, H-1), 4.3 (1H, m, H-2), 4.03 (1H, dd, J=3.90, 3.43 Hz, H-2′), 3.72 (4H, t, (CH 2 ) 2 O), 2.67-2.53 (6H, m, (CH 2 ) 3 N), 1.66-1.61 (1H, m, CH(OH)—C H 2 (A)), 1.50-1.45 (1H, m, CH(OH)—C H 2 (B)), 1.32-1.20 (12H, m, (C H 2 ) 6 CH 3 ), 0.88 (3H, t, CH 3 )
13 C-NMR(CDCl 3 ) δ: 174.0, 140.8, 128.4, 127.7, 126.0, 75.2, 72.2, 66.9, 60.1, 54.4, 50.8, 34.8, 31.8, 29.4, 29.3, 29.2, 24.6, 22.6, 14.1
Example 11
Synthesis of (1S,2S)-2-decanoylamino-3-(N-methylpiperazino)-1-phenyl-1-propanol:
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (1.81 g, 4.78 mmol) was dissolved in ethanol, N-methylpiperazine (1.92 g, 19.2 mmol) was added thereto, and the mixture thus obtained was stirred at 40° C. for 3 days. After completion of the reaction, the solvent was removed by evaporation under a reduced pressure, a saturated sodium bicarbonate solution was added thereto, and extraction was conducted with chloroform. The resulting organic layer was dried over anhydrous sodium sulfate and filtered, and then the solvent was removed by evaporation. Next, the extract was dissolved in methanol, 10% palladium-carbon was added thereto and a hydrogen gas was introduced under stirring vigorously. After completion of the reaction, palladium-carbon was removed by filtration, the solvent was removed by evaporation under a reduced pressure, methanol was added to the resulting residue, and decanoyl chloride was further added thereto on an ice bath in the presence of triethylamine. After completion of the reaction, the solvent was removed by evaporation under a reduced pressure, a saturated sodium bicarbonate solution was added thereto, and extraction was conducted with chloroform. The organic layer thus obtained was dried over anhydrous sodium sulfate and filtered, and the solvent was removed by evaporation. The extract was purified by silica gel column chromatography (chloroform:methanol=9:1) to obtain the objective compound as a colorless oily material (10.0 mg). 1 H-NMR (CDCl 3 ) δ: 7.37-7.25 (5H, m, aromatic), 5.91 (1H, d, J=7.3 Hz, NH), 4.95 (1H, d, J=3.4 Hz, H-1), 4.29 (1H, m, H-2), 2.78-2.36 (10H, m, H-3, H-2′, H-3′, H-4′, H-5′), 2.32 (3H, t, N—CH 3 ), 2.30-2.27 (1H, m, COC H 2 (A)), 2.11-2.08 (1H, m, COC H 2 (B)), 1.63-1.60 (1H, m, CO—CH 2 —C H 2 (A)), 1.53-1.48 (1H, m, CO—CH 2 —C H 2 (B)), 1.25 (12H, brs, (C H 2 ) 6 CH 3 ), 0.88 (3H, t, CH 3 )
Example 12
Synthesis of (1S, 2S)-2-decanoylamino-3-((2S)-2-hydroxymethylpyrrolidino)-1-phenyl-1-propanol:
The objective compound (89.6 mg) was prepared as a colorless oily material in the same manner as in Example 11, except that (2S)-2-hydroxymethylpyrrolidine was used in place of N-methylpiperazine.
1 H-NMR (CDCl 3 ) δ: 7.35-7.23 (5H, m, aromatic), 6.13 (1H, d, J=6.3 Hz, NH), 4.99 (1H, d, J=3.4 Hz, H-1), 4.14 (1H, m, H-2), 3.71-3.67 (1H, m, H-6′A), 3.57-3.53 (1H, m, H-6′B), 3.29-3.24 (1H, m, H-5′A), 3.14-3.09 (1H, m, H-3A), 2.83-2.78 (1H, m, H-3B), 2.76 (1H, m, H-2′), 2.38-2.32 (1H, m, H-5′B), 2.14-2.03 (2H, m, COCH 2 ), 1.92-1.83 (1H, m, H-3′A), 1.80-1.73 (2H, m, H-4′), 1.70-1.62 (1H, m, H-3′B), 1.50-1.43 (2H, m, CO—CH 2 —C H 2 ), 1.22 (12H, brs, (C H 2 ) 6 CH 3 ), 0.88 (3H, t, CH 3 )
13 C-NMR(CDCl 3 ) δ: 174.1, 141.1, 128.3, 127.5, 125.7, 75.6, 66.4, 63.6, 57.6, 56.1, 54.1, 36.7, 31.8, 29.4, 29.3, 29.2, 29.0, 27.0, 25.6, 23.9, 22.6, 14.1
Example 13
Synthesis of (1S,2S)-2-decanoylamino-3-(3-hydroxypyrrolidino)-1-phenyl-1-propanol:
The objective compound (a mixture having a diastereomer ratio of 1:1, 88.3 mg) was prepared as a colorless oily material in the same manner as in Example 11, except that 3-hydroxypyrrolidine was used in place of N-methylpiperazine.
1 H-NMR (CDCl 3 ) δ: 7.36-7.24 (5H, m, aromatic), 5.91 (0.5H, d, J=7.3 Hz, NH), 5.88 (0.5H, d, J=7.3 Hz, NH), 5.0 (1H, H-1), 4.40 (1H, m, H-3′), 4.23 (1H, m, H-2), 3.06-3.01 (1H, m, H-5′A), 3.00-2.70 (3H, m, H-3, H-2′A), 2.67-2.63 (1H, m, H-2′B), 2.54-2.45 (1H, m, H-5′B), 2.21-2.12 (1H, m, H-4′A), 2.11-2.00 (2H, m, COC H 2 ), 1.79-1.74 (1H, m, H-4′B), 1.50-1.44 (2H, m, CO—CH 2 —C H 2 ), 1.22 (12H, brs, (C H 2 ) 6 CH 3 ), 0.88 (3H, t, CH 3 )
13 C-NMR(CDCl 3 ) δ: 173.6, 141.0, 140.9, 128.3, 127.5, 127.4, 125.9, 75.3, 75.1, 71.1, 71.0, 63.7, 57.6, 53.6, 53.5, 52.6, 36.7, 34.7, 31.8, 29.4, 29.3, 29.2, 29.0, 25.6, 22.6, 14.0
Example 14
Synthesis of (1S,2S)-2-decanoylamino-3-pyrrolidino-1-phenyl-1-propanol:
The objective compound (92.2 mg) was prepared as a colorless oily material in the same manner as in Example 11, except that pyrrolidine was used in place of N-methylpiperazine.
1 H-NMR (CDCl 3 ) δ: 7.36-7.23 (5H, m, aromatic), 5.91 (1H, d, J=7.8 Hz, NH), 5.05 (1H, d, J=3.4 Hz, H-1), 4.26 (1H, m, H-2), 2.86 (2H, d, J=5.4 Hz, H-3), 2.70 (4H, m, H-2′, H-5′), 2.07 (2H, m, COCH 2 ), 1.81 (4H, m, H-3′, H-4′), 1.47 (2H, m, CO—CH 2 —C H 2 ), 1.3-1.1 (12H, m, (C H 2 ) 6 CH 3 ), 0.88 (3H, t, CH 3 )
13 C-NMR(CDCl 3 ) δ: 173.5, 141.0, 128.2, 127.4, 125.9, 75.4, 57.9, 55.2, 52.3, 36.7, 31.8, 29.3, 29.2, 29.0, 25.6, 23.6, 22.6, 14.0
Example 15
Synthesis of (1S,2S)-2-decanoylamino-3-(3-hydroxymethylpiperidino)-1-phenyl-1-propanol:
The objective compound (a mixture having a diastereomer ratio of 1:1, 246.5 mg) was prepared as a colorless oily material in the same manner as in Example 11, except that 3-hydroxymethylpiperidine was used in place of N-methylpiperazine.
1 H-NMR (CDCl 3 ) δ: 7.36-7.24 (5H, m, aromatic), 5.96 (0.5H, d, J=7.8 Hz, NH), 5.94 (0.5H, d, J=7.8 Hz, NH), 4.96 (0.5H, d, J=3.4 Hz, H-1), 4.94 (0.5H, d, J=3.4 Hz, H-1), 4.33-4.26 (1H, m, H-2), 3.59-3.51 (1H, m), 3.50-3.42 (1H, m), 3.00-2.83 (2H, m), 2.59 (1H, dd, H-3A), 2.48 (1H, dd, H-3B), 2.3-2.0 (2H, m), 2.07 (2H, m, COC H 2 ), 1.9-1.5 (4H, m), 1.48 (2H, m, CO—CH 2 —C H 2 ), 1.4-1.1 (12H, m, (C H 2 ) 6 CH 3 ), 1.10-1.00 (1H, m), 0.88 (3H, t, CH 3 )
Example 16
Synthesis of (1S,2S)-3-cyclohexylamino-2-decanoylamino-1-phenyl-1-propanol
The objective compound (40.6 mg) was prepared as a colorless oily material in the same manner as in Example 11, except that cyclohexylamine was used in place of N-methylpiperazine.
1 H-NMR (CDCl 3 ) δ: 7.4-7.2 (5H, m, aromatic), 6.64 (1H, d, J=7.3 Hz, NH), 5.14 (1H, d, J=2.5 Hz, H-1), 4.37 (1H, m, H-2), 3.34 (1H, dd, J=4.9, 12.7 Hz, H-3A), 3.13 (1H, dd, J=5.4, 16.3 Hz, H-3B), 2.77 (1H, m, (CH 2 ) 2 C H NH), 2.2-2.0 (4H, m), 1.76 (2H, d, J=12.7 Hz), 1.63 (1H, d, J=10.7 Hz), 1.5-1.0 (19H, m), 0.88 (3H, t, J=6.8 Hz, CH 3 )
13 H-NMR (CDCl 3 ) δ: 173.7, 141.1, 128.3, 127.3, 125.5, 75.9, 57.0, 53.2, 49.1, 36.8, 33.2, 33.0, 31.8, 29.4, 29.3, 29.2, 29.0, 25.8, 25.7, 24.8, 22.6, 14.1
Example 17
Synthesis of (1S,2S)-2-decanoylamino-3-(4-hydroxycyclohexylamino)-1-phenyl-1-propanol
The objective compound (12.0 mg) was prepared as a colorless oily material in the same manner as in Example 11, except that 4-hydroxycyclohexylamine was used in place of N-methylpiperazine.
1 H-NMR (CDCl 3 ) δ: 7.4-7.2 (5H, m, aromatic), 6.36 (1H, d, J=6.8 Hz, NH), 5.13 (1H, d, J=2.0 Hz, H-1), 4.31 (1H, m, H-2), 3.61 (1H, m, CH 2 C H OH)), 3.34 (1H, dd, J=4.4, 12.7 Hz, H-3A), 3.06 (1H, dd, J=4.9, 12.7 Hz, H-3B), 2.73 (1H, m, CH 2 C H NH), 2.2-1.9 (6H, m), 1.5-1.0 (18H, m), 0.88 (3H, t, J=6.8 Hz, CH 3 )
Example 18
Synthesis of (1S,2S)-2-decanoylamino-3-(2-(N-morpholino)ethylamino-1-phenyl-1-propanol
The objective compound (91.7 mg) was prepared as a colorless oily material in the same manner as in Example 11, except that 2-(N-morpholino)ethylamine was used in place of N-methylpiperazine.
1 H-NMR (CDCl 3 ) δ: 7.4-7.2 (5H, m, aromatic), 6.02 (1H, d, J=7.3 Hz), NH), 4.64 (1H, d, J=2.4 Hz, H-1), 4.28 (1H, m, H-2), 3.80 (1H, dd, J=9.8, 14.2 Hz), 3.68 (4H, t, J=4.4 Hz, CH 2 —O—CH 2 ), 3.50 (2H, m), 3.30 (1H, dd, J=5.9, 14.2 Hz), 2.7-2.5 (2H, m), 2.48 (4H, t, J=4.4 Hz, CH 2 NCH 2 ), 2.4-2.3 (2H, m), 2.00 (2H, m, COCH 2 ), 1.65 (2H, m), 1.5-1.0 (14H, m, (C H 2 ) 7 CH 3 ), 0.88 (3H, t, J=6.8 Hz, CH 3 )
Example 19
Synthesis of (1S,2S)-2-(2-hydroxy-n-octanoylamino)-3-morpholino-1-phenyl-1-propanol
(1S,2)-2-Amino-3-morpholino-1-phenyl-1-propanol was prepared in the same manner as in Example 11, except that morpholine was used in place of N-methylpiperazine. The compound obtained (99.2 mg, 0.42 mmol) was dissolved in methylene chloride, 2-hydroxy-n-octanoic acid (80.0 mg, 0.50 mmol) and N-hydroxysuccinimide (102.1 mg, 0.42 mmol) were added thereto at room temperature, and then 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (118.1 mg, 0.62 mmol) was added thereto under ice cooling and further stirred. After completion of the reaction, chloroform was added thereto and the resulting organic layer was washed with a 5% citric acid solution, a saturated sodium bicarbonate solution and water in this order, dried over anhydrous sodium sulfate and then filtered. The solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatography (ethyl acetate) to obtain the objective compound as a colorless oily material as one of its diastereomer (15.4 mg), as well as the other diastereomer (16.9 mg).
(One Diastereomer)
TLC Rf: 0.2 (AcOEt)
1 H-NMR (CDCl 3 ) δ: 7.37-7.26 (5H, m, aromatic), 6.75 (1H, d, J=7.3 Hz, NH), 5.00 (1H, d, J=3.4 Hz, H-1), 4.3 (1H, m, H-2), 4.02, 4.01, 4.00, 3.99 (1H, dd, CO—C H —OH), 3.74, 3.73, 3.72 (4H, t, CH 2 OCH 2 ), 2.69-2.52 (6H, m, CH 2 N(CH 2 ) 2 ), 1.72-1.66 (1H, m, CH(OH)C H 2 (A)), 1.51-1.43 (1H, m, CH(OH)C H 2 (B)), 1.30-1.20 (8H, m, (C H 2 ) 4 CH 3 ), 0.87 (3H, t, CH 3 )
13 H-NMR (CDCl 3 ) δ: 174.1, 140.8, 128.4, 127.7, 126.0, 75.3, 72.0, 66.9, 60.0, 54.5, 51.1, 34.9, 31.6, 29.0, 24.7, 22.5, 14.0
(The Other Diastereomer)
TLC Rf: 0.1 (AcOEt)
1 H-NMR (CDCl 3 ) δ: 7.37-7.26 (5H, m, aromatic), 6.85 (1H, d, J=7.8 Hz, NH), 5.01 (1H, d, J=3.4 Hz, H-1), 4.3 (1H, m, H-2), 4.06, 4.05, 4.04, 4.03 (1H, dd, CO—C H —OH), 3.74, 3.73, 3.72 (4H, t, CH 2 OCH 2 ), 2.68-2.51 (6H, m, CH 2 N(CH 2 ) 2 ), 1.68-1.64 (1H, m, CH(OH)C H 2 (A)), 1.51-1.46 (1H, m, CH(OH)C H 2 (B)), 1.30-1.20 (8H, m, (C H 2 ) 4 CH 3 ), 0.88 (3H, t, CH 3 )
13 H-NMR (CDCl 3 ) δ: 173.9, 140.8, 128.4, 127.7, 126.0, 75.2, 72.2, 66.9, 60.1, 54.4, 50.8, 34.8, 31.6, 29.0, 24.5, 22.5, 14.0
Example 20
Synthesis of (1R,2S)-2-decanoylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol
The objective compound (204.2 mg) was prepared as white solid in the same manner as in Example 11, except that (1R,2S)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester was used in place of (1S,2S)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester, and 4-hydroxypiperidine was used in place of N-methylpiperazine.
TLC Rf: 0.24 (CHCl 3 :MeOH:AcOH=9:1:1)
1 H-NMR (CDCl 3 ) δ: 7.37-7.26 (5H, m, aromatic), 6.29 (1H, d, J=4.3 Hz, NH), 4.83 (1H, d, J=5.0 Hz, H-1), 4.25 (1H, m, H-2), 3.76 (1H, m, H-4′), 2.90-2.78 (2H, br, H-2′A), 2.70-2.56 (2H, m, H-3), 2.38-2.35 (2H, br, H-2′B), 2.01-1.91 (2H, br, H-3′A), 2.16-2.10 (2H, m, COCH 2 ), 1.67-1.57 (4H, m, H-3′B, COCH 2 C H 2 ), 1.24 (12H, brs, (C H 2 ) 6 )CH 3 ), 0.88 (3H, t, CH 3 )
MS (FAB): 405 (M+H) +
Example 21
Synthesis of (1S,2R)-2-decanoylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol
The objective compound (160.5 mg) was prepared as a colorless oily material in the same manner as in Example 20, except that (1S,2R)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester was used in place of (1R,2S)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester.
1 H-NMR (CDCl 3 ) δ: Coincided with the data of Example 20.
Example 22
Synthesis of (1R,2R)-2-decanoylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol
The objective compound (184.2 mg) was prepared as a colorless oily material in the same manner as in Example 20, except that (1R,2R)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester was used in place of (1R,2S)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester.
TLC Rf: 0.20 (CHCl 3 :MeOH:AcOH=9:1:1)
1 H-NMR (CDCl 3 ) δ: 7.37-7.23 (5H, m, aromatic), 6.77 (1H, d, J=7.6 Hz, NH), 4.95 (1H, d, J=3.6 Hz, H-1), 4.41 (1H, m, H-2), 3.78 (1H, m, H-4′), 3.06-3.03 (2H, br, H-2′A), 2.86 (2H, m, H-3), 2.80-2.70 (2H, br, H-2′B), 2.10-2.00 (4H, m, H-3′A, COCH 2 ), 1.76 (2H, m, H-3′B), 1.45 (2H, m, COCH 2 C H 2 ), 1.24 (12H, brs, (C H 2 ) 6 CH 3 ), 0.88 (3H, t, CH 3 )
13 H-NMR (CDCl 3 ) δ: 174.8, 141.0, 128.8, 128.1, 126.4, 74.5, 65.1, 58.2, 51.2, 50.9, 50.7, 36.9, 32.6, 32.3, 29.9, 29.8, 29.7, 29.6, 26.0, 23.0, 14.6
MS (FAB): 450 (M+H) +
Example 23
Synthesis of (1R,2S)-2-decanoylamino-3-diethylamino-1-phenyl-1-propanol
The objective compound (L-erythro compound) was prepared in the same manner as in Example 11, except that (1R,1S)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester was used in place of (1S,2S)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester, and diethylamine was used in place of N-methylpiperazine.
TLC Rf: 0.59 (CHCl 3 :MeOH:AcOH=9:1:1), 0.32 (CHCl 3 :MeOH:AcOH=95:5:10)
1 H-NMR (CDCl 3 ) δ: 7.38-7.23 (5H, m, aromatic), 5.87 (1H, d, J=4.0 Hz, NH), 4.75 (1H, d, J=6.3 Hz, H-1), 4.17 (1H, m, H-2), 2.97-2.50 (6H, m, CH 2 N(CH 2 ) 2 ), 2.04 (2H, m, COCH 2 ), 1.45 (2H, COCH 2 C H 2 ), 1.24 (12H, brs, (C H 2 ) 6 CH 3 ), 1.05 (6H, brt, N(CH 2 C H 3 ) 2 ), 0.88 (3H, t, (CH 2 ) 6 C H 3 )
MS (FAB): 377 (M+H) +
Example 24
Synthesis of (1S,2R)-2-decanoylamino-3-diethylamino-1-phenyl-1-propanol
The objective compound (D-erythro compound) was prepared in the same manner as in Example 11, except that (1S,2R)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester was used in place of (1S,2S)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester, and diethylamine was used in place of N-methylpiperazine.
1 H-NMR (CDCl 3 ) δ: Coincided with the data of Example 23.
Example 25
Synthesis of (1R,2S)-2-hexanoylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol
The objective compound (250.5 mg) was prepared as white solid in the same manner as in Example 20, except that hexanoyl chloride was used in place of decanoyl chloride.
1 H-NMR (CDCl 3 ) δ: 7.36-7.26 (5H, m, aromatic), 5.95 (1H, d, J=4.3 Hz, NH), 4.80 (1H, d, J=5.0 Hz, H-1), 4.22 (1H, m, H-2), 3.72 (1H, m, H-4′), 2.90-2.78 (2H, br, H-2′A), 2.70-2.56 (2H, m, H-3), 2.38-2.35 (2H, br, H-2′B), 2.01-1.91 (2H, br, H-3′A), 2.16-2.10 (2H, m, COCH 2 ), 1.67-1.57 (4H, m, H-3′B, COCH 2 C H 2 ), 1.24 (4H, brs, (C H 2 ) 2 CH 3 ), 0.88 (3H, t, CH 3 )
Example 26
Synthesis of (1R,2S)-2-octanoylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol
The objective compound (230.2 mg) was prepared as white solid in the same manner as in Example 20, except that octanoyl chloride was used in place of decanoyl chloride.
1 H-NMR (CDCl 3 ) δ: 7.36-7.26 (5H, m, aromatic), 6.09 (1H, d, J=4.3 Hz, NH), 4.80 (1H, d, J=5.0 Hz, H-1), 4.21 (1H, m, H-2), 3.70 (1H, m, H-4′), 2.90-2.78 (2H, br, H-2′A), 2.70-2.56 (2H, m, H-3), 2.38-2.35 (2H, br, H-2′B), 2.01-1.91 (2H, br, H-3′A), 2.16-2.10 (2H, m, COCH 2 ), 1.67-1.57 (4H, m, H-3′B, COCH 2 C H 2 ), 1.24 (8H, brs, (C H 2 ) 4 CH 3 ), 0.88 (3H, t, CH 3 )
Example 27
Synthesis of (1R,2S)-2-dodecanoylamino-3-(4-hydroxypiperidino-1-phenyl-1-propanol
The objective compound (265.0 mg) was prepared as white solid in the same manner as in Example 20, except that dodecanoyl chloride was used in place of decanoyl chloride.
1 H-NMR (CDCl 3 ) δ: 7.36-7.26 (5H, m, aromatic), 5.97 (1H, d, J=4.3 Hz, NH), 4.80 (1H, d, J=5.0 Hz, H-1), 4.22 (1H, m, H-2), 3.72 (1H, m, H-4′), 2.90-2.78 (2H, br, H-2′A), 2.70-2.56 (2H, m, H-3), 2.38-2.35 (2H, br, H-2′B), 2.01-1.91 (2H, br, H-3′A), 2.16-2.10 (2H, m, COCH 2 ), 1.67-1.57 (4H, m, H-3′B, COCH 2 C H 2 ), 1.24 (16h, brs, (C H 2 ) 8 CH 3 ), 0.88 (3H, t, CH 3 )
Examples 28 to 30
The following stereoisomers were prepared in the same manner as in Examples 25 to 27. The yield amounts were as follows.
Example 28
(1S,2R)-2-hexanoylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol; yield amount: 245.0 mg
Example 29
(1S,2R)-2-octanoylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol; yield amount: 233.5 mg
Example 30
(1S,2R)-2-dodecanoylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol; yield amount 215.0 mg
Example 31
Synthesis of (1R,2R)-2-benzyloxycarbonylamino-3-pyrrolidino-1-phenyl-1-propanol
(1R,2R)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (1.52 g, 4.01 mmol) was dissolved in DMF (8 ml), pyrrolidine (1.14 g, 16.03 mmol) was added thereto, and the mixture thus obtained was stirred at 40 to 50° C. for 18 hours. Ethyl acetate (100 ml) was added thereto, and the resulting organic layer was washed with a saturated sodium bicarbonate solution (70 ml), water (70 ml) and brine (70 ml) in this order and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under a reduced pressure, and the crude product thus obtained was purified by silica gel column chromatography (chloroform:methanol=20:1) to obtain the objective compound as a colorless oily material (1.21 g, yield: 85.5%).
TLC Rf: 0.20 (CHCl 3 :MeOH=20:1), 0.20 (AcOEt)
1 H-NMR (CDCl 3 ) δ: 7.39-7.24 (10H, m, aromatic), 5.06-5.02 (2H, m, CH 2 —O—CO), 4.99 (1H, d, J=3.91 Hz, H-1), 4.07 (1H, m, H-2), 2.9-2.6 (6H, m, (CH 2 ) 3 N), 1.83-1.74 (4H, m, H-3′, H-4′)
13 H-NMR (CDCl 3 ) δ: 156.0, 140.8, 136.5, 128.4, 128.2, 128.0, 127.8, 127.4, 126.1, 75.7, 66.6, 58.1, 55.2, 53.4, 23.6
Example 32
Synthesis of (1R,2R)-2-benzyloxycarbonylamino-3-cyclopentylamino-1-phenyl-1-propanol
(1R,2R)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (1.21 g, 3.19 mmol) was dissolved in DMF (6 ml), cyclopentylamine (1.09 g, 12.8 mmol) was added thereto, and the mixture thus obtained was stirred at 40 to 50° C. for 32 hours. Further, cyclopentylamine (0.51 g, 5.99 mmol) was added thereto, and the obtained mixture was stirred overnight at 40 to 50° C. After confirming almost completion of the reaction with TLC (ethyl acetate), the reaction solution was mixed with ethyl acetate (100 ml) and the resulting organic layer was washed with a saturated sodium bicarbonate solution (70 ml), water (70 ml) and brine (70 ml) in this order and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under a reduced pressure, and the crude product thus obtained was purified by silica gel column chromatography (chloroform:methanol=20:1) to obtain the objective compound as a colorless oily material (534.4 mg, yield: 45.7%).
TLC Rf: 0.17 (CHCl 3 :MeOH=20:1), 0.10 (AcOEt)
1 H-NMR (CDCl 3 ) δ: 7.35-7.23 (10H, m, aromatic), 5.34 (1H, d, CONH), 5.08 (1H, s, H-1), 4.98 (2H, m, CH 2 —O—CO), 3.94 (1H, m, H-2), 3.24 (1H, m, H-3A), 3.08 (1H, m, H-2′), 2.85 (1H, dd, J=2.93, 12.21 Hz, H-3B), 2.04-1.93, 1.87-1.79, 1.73-1.55, 1.51-1.30 (8H, m, H-3′, H-4′, H-5′, H-6′)
13 H-NMR (CDCl 3 ) δ: 160.7, 141.0, 136.4, 128.4, 128.2, 128.0, 127.8, 127.3, 125.6, 76.3, 66.6, 59.9, 54.7, 53.5, 49.9, 34.1, 33.2, 33.1, 32.7, 23.8, 23.6, 23.4
Example 33
Synthesis of (1R,2R)-2-benzyloxycarbonylamino-3-piperidino-1-phenyl-1-propanol
(1R,2R)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (1.21 g, 3.19 mmol) was dissolved in DMF (6 ml), piperidine (1.09 g, 12.8 mmol) was added thereto, and the mixture thus obtained was stirred at 40 to 50° C. for 24 hours. After confirming almost completion of the reaction with TLC (ethyl acetate, chloroform:methanol=20:1), ethyl acetate (100 ml) was added thereto, and the resulting organic layer was washed with a saturated sodium bicarbonate solution (70 ml), water (70 ml) and brine (70 ml) in this order and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under a reduced pressure, and the crude product thus obtained was purified by silica gel column chromatography (ethyl acetate) to obtain the objective compound as a colorles oily material (795.4 mg, yield: 68.0%).
TLC Rf:
0.20 (CHCl 3 :MeOH=20:1), 0.17 (AcOEt)
1 H-NMR (CDCl 3 ) δ:
7.36-7.25 (10H, m, aromatic), 5.04 (2H, s, CH 2 —O—CO), 5.01 (1H, d, J=3.42 Hz, H−1), 4.94 (1H, d, J=7.33 Hz, NH), 4.15 (1H, m, H-2), 2.64-2.45 (6H, m, (CH 2 ) 3 N), 1.68-1.54 (4H, m, H-3′, H-5′), 1.5-1.4 (2H, m, H-4′)
13 C-NMR (CDCl 3 ) δ: 155.9, 140.8, 136.4, 128.5, 128.3, 128.1, 127.9, 127.4, 126.3, 75.7, 66.7, 60.5, 55.8, 51.7, 26.1, 23.9
Example 34
Synthesis of (1R,2R)-2-benzyloxycarbonylamino-3-cyclohexylamino-1-phenyl-1-propanol
(1R,2R)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (1.21 g, 3.19 mmol) was dissolved in DMF (6 ml), cyclohexylamine (1.29 g, 13.0 mmol) was added thereto, and the mixture thus obtained was stirred at 40 to 50° C. for 2 days. Further, cyclohexylamine (0.62 g, 6.25 mmol) was added thereto, and the obtained mixture was stirred overnight at 40 to 50° C. After confirming almost completion of the reaction with TLC (ethyl acetate, chloroform:methanol=20:1), ethyl acetate (100 ml) was added thereto, and the resulting organic layer was washed with a saturated sodium bicarbonate solution (70 ml), water (70 ml) and brine (70 ml) in this order and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under a reduced pressure, and the thus obtained crude product was purified by silica gel column chromatorgraphy (ethyl acetate) to obtain the objective compound as a colorless oily material (750.0 mg, yield: 61.5%).
TCL Rf:
0.19 (CHCl 3 :MeOH=20:1), 0.12 (AcOEt)
1 H-NMR (CDCl 3 ) δ:
7.35-7.22 (10H, m, aromatic), 5.32 (1H, d, J=7.32 Hz, CONH), 5.07 (1H, s, H-1), 4.98 (2H, m, CH 2 —O—CO), 3.94 (1H, m, H-2), 3.26 (1H, m, H-3A), 2.88 (1H, dd, J=2.44, 12.69 Hz, H-3B), 2.44 (1H, m, H-2′), 1.95-1.86, 1.77-1.68, 1.63-1.60, 1.42-1.02 (10H, m, H-3′, H-4′, H-5′, H-6′, H-7′)
13 C-NMR(CDCl 3 ) δ: 156.2, 141.0, 136.4, 128.4, 128.2, 128.0, 127.8, 127.3, 125.7, 76.3, 66.6, 56.8, 54.7, 49.6, 47.0, 34.7, 33.5, 33.3, 33.0, 25.9, 25.4, 25.0, 24.8, 24.7
Example 35
Synthesis of (1S,2S)-2-t-butyoxycarbonylamino-3-morpholino-1-phenyl-1-propanol
(1S,2S)-2-t-Butoxycarbonylamino-1-phenyl-1,3-propanediol was mesylated in the same manner as in Example 1 and a morpholine substitution reaction was conducted in the same manner as in Example 3 to obtain the objective compound as a colorless oily material (yield: 63%).
TLC Rf:
0.36 (CHCl 3 :MeOH=20:1)
1 H-NMR (CDCl 1 ) δ:
7.38-7.26 (5H, m, aromatic), 4.98 (1H, d, J=3.91 Hz, H-1), 4.05 (1H, m, H-2), 3.74 (4H, m, (CH 2 ) 2 O), 2.64-2.59 (5H, m, H-2′, H-6′, H-3A), 2.46 (1H, dd, J=4.89, 13.19 Hz, H-3B), 1.38 (9H, s, (CH 3 ) 3 )
Example 36
Synthesis of (1S,2S)-2-decanoylamino-3-morpholino-1-phenyl-1-propanol using (1S,2S)-2-t-butoxycarbonylamino-3-morpholino-1-phenyl-1-propanol as the raw material
(1S,2S)-2-t-Butoxycarbonylamino-3-morpholino-1-phenyl-1-propanol (49.9 mg, 0.149 mmol) was dissolved in methylene chloride (1 ml), and trifluroacetic acid (1 ml) was added thereto under ice cooling. Thirty minutes thereafter, completion of the raction was confirmed with TLC (chloroform:methanol=9:1), ether (3 ml) was added thereto, and the solvent was removed by evaporation under a reduced pressure. The colorless oily material thus obtained was acylated in the same manner as in Exampl e7 to obtain the objective compound as a colorless oily material (48.8 mg, yield: 82.2%).
Example 37
Synthesis of (1S,2S)-2-benzylorxycaronylamino-3-(N-methylpiperazino)-1-phenyl-1-propanol
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (1.81 g, 4.78 mmol) was dissolved in ethanol (40 ml), sodium iodide (712.8 mg, 4.75 mmol) and N-methylpiperazine (1.92 g, 19.2 mmol) were added thereto, and the mixture thus obtained was stired at 50° C. for 5 days. After confirming almost completion of the reaciton with TLC (chloroform:methanol=9:1), the solvent was removed by evaporation, water (50 ml) and ethyl acetate (100 ml) were added thereto, and the resulting organic layer wa s washed with water and brine in this order, dried over anhydrous sodium sulfate and then filtered. The solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatogaphy (chloroform:methanol=10:1) to obtain the objective compound as a colorless oily material (242.2 mg, yield: 13.2%).
TLC Rf:
0.38 (CHCl 3 :MeOH=9:1)
1 H-NMR (CDCl 3 ) δ:
7.36-7.26 (10H, m, aromatic), 5.04 (2H, s, CH 2 —O—CO), 5.00 (1H, d, J=3.41 Hz, H-1), 4.97 (1H, d, NH), 4.12 (1H, m, H-2), 2.70-2.49 (10H, m, (CH 2 ) 3 N, (CH 2 ) 2 N), 2.28 (3H, s, CH 3 —N)
13 C-NMR(CDCl 3 ) δ: 156.0, 140.7, 136.4, 128.5, 128.3, 128.1, 127.9, 127.5, 126.2, 75.3, 66.8, 59.6, 55.1, 54.1, 52.1, 45.9
Example 38
Synthesis of (1S,2S)-2-benzyloxycarbonylamino-3-((2S)-2-hydroxymethylpyrrolidino)-1-phenyl-1-propanol
(2S)-2-Hydroxymethylpyrrolidine (323.3 mg), 3.20 mmol) was dissolved in ethanol (12 ml), and the obtained mixture was added dropwise to a methylene chlordie solution (3 ml) of (1S,2S)-2-benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-p-bromobenzenesulfonyl ester (872 mg, 1.50 mmol). Two days after stirring at 45° C., almost completion of the reaciton was confirmed with TLC (chloroform:methanol=9:1, ethyl acetate:2-propanol=2:1), the solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatography (ethyl acetate:2-propanol=7:3) to obtain the objective compound as a colorless oily materail (79.5 mg, yield: 13.8%).
TLC Rf:
0.25 (CHCl 3 :MeOH=9:1), 0.39 (AcOEt:(CH 3 ) 2 CHOH=2:1)
1 H-NMR (CDCl 3 ) δ:
7.51-7.23 (10H, m, aromatic), 5.32 (1H, br, NH), 4.99 (3H, m, H-1, CH 2 —O—CO), 3.93 (1H, m, H-2), 3.67, 3.66, 3.64, 3.63 (1H, dd, C H 2 (A)—OH), 3.51 (1H, dd, J=4.40, 11.23 Hz, C H 2 (B)—OH), 3.28-3.23 (1H, m, H-5′A), 3.08 (1H, dd, J=5.86, 13.19 Hz, H-3A), 2.81 (1H, dd, J=2.93, 13.18 Hz, H-3B), 2.71 (1H, m, H-2′), 2.34-2.28 (1H, m, H-5′B), 1.90-1.59 (4H, m, H-3′, J-4′)
13 C-NMR (CDCl 3 ) δ: 156.5, 141.0, 136.5, 128.4, 128.3, 128.0, 127.8, 125.5, 125.8, 75.4, 66.6, 66.4, 63.7, 58.0, 56.2, 55.4, 27.0, 23.8
Example 39
Synethesis of (1S,2S)-2-benzyloxycarbonylamino-3-(3-hydroxypyrrolidino)-1-phenyl-1-propanol
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (2.60 g, 6.86 mmol) was dissolved in ethanol (20 ml), 3-hydroxypyrrolidine (1.19 g, 13.68 mmol) was added thereto, and the mixture thus obtained was stirred at 45° C. for 5 days. After confirming almost completion of the reaciton with TLC (chloroform:methanol=9:1), the solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatography (chloroform:methano=9:1, ethayl acetate:methanol=9:1) to obtain the objective compound as a colorless oily materail (527.1 mg, yield: 20.8%).
TLC Rf:
0.25 (CHCl 3 :MeOH=9:1), 0.35 (AcOEt:MeOH=4:1)
1 H-NMR (CDCl 3 ) δ:
7.41-7.24 (10H, m, aromatic), 5.26 (0.7H, d, J=7.82 Hz, NH, originated from one diastereomer), 5.20 (0.3H, d, NH, originated from the other diastereomer), 5.00 (3H, s, H-1, CH 2 —O—CO), 4.34 (0.7H, m, H-3′, originated from one diastereomer), 4.28 (0.3H, m, H-3′, originated from the other diasteremer), 4.02 (1H, m, H-2), 3.04-2.99, 2.89-2.42 (6H, m, (CH 2 ) 3 N), 2.20-2.07 (1H, m, H-4′A), 1.80-1.68 (1H, m, H-4′B)
13 C-NMR(CDCl 3 ) δ: 156.5, 141.2, 141.1, 136.7, 128.8, 128.6, 128.3, 128.2, 127.8, 126.4, 75.4, 75.2, 71.3, 67.0, 64.0, 58.0, 54.2, 54.1, 53.8, 34.9
Example 40
Synthesis of (1S,2S)-2-benzyloxycarbonylamino-3-pyrrolidino-1-phenyl-1-propanol
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (1.21 g, 3.19 mmol) was dissolved in DMF (6 ml), pyrrolidine (0.91 g, 12.8 mmol) was added thereto, and theobtianed mixture was stirred at 40° C. for 24 hours. Ethyl acetate (100 ml) was added thereto, and the resulting organic layer was washed with a saturated sodium bicarbonate solution (70 ml), water (70 ml) and brine (80 ml) in this order and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under a reduced pressure, and the crude product thus obtained was purified by silica gel column chromatography (chloroform:methanol=20:1) to obtain the objective compound as a colorless oily material (983.1 mg, yield: 87.0%).
TLC Rf:
0.20-(CHCl 3 :MeOH=20:1), 0.20 (AcOEt)
1 H-NMR (CDCl 3 ) δ:
Coincided with the data of Example 31.
13 C-NMR(CDCl 3 ) δ:
Coincided with the data of Example 31.
Example 41
Synthesis of (1S,2S)-2-benzyloxycarbonylamino-3-(3-hydroxymethylpuperidino)-1-phenyl-1-propanol
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (2.43 g, 6.41 mmol) was dissolved in ethanol (20 ml), 3-hydroxymethylpiperidine (1.47 g, 12.78 mmol) was added thereto, and the mixture thus obtained was stirred at 45° C. for 5 days. After confirming almost completion of the reaciton with TLC (chloroform:methanol=9:1), the solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1, ethyl acetate:methanol=20:1) to obtain the objective compound as a colorless oily material (293.3 mg, yield: 11.5%).
TLC Rf:
0.42 (CHCl 3 :MeOH=9:1), 0.16 (AcOEt:MeOH=20:1)
1 H-NMR (CDCl 3 ) δ:
7.35-7.26 (10H, m, aromatic), 5.03 (2H, s, CH 2 —O—CO), 4.994 (0.5H, d, J=7.81 Hz, H-1, originated from one diastereomer), 4.986 (0.5H, d, J=8.30 Hz, H-1, originated from the other idastereomer), 4.15-4.09 (1H, m, H-2), 3.56-3.45 (2H, m, C H 2 —OH), 3.00-2.91, 2.75, 2.25-2.00 (4H, m, H-2′, H-6′), 2.65-2.59 (1H, m, H-3A), 2.49-2.45 (1H, m, H-3B), 1.82 (1H, m, H-3′), 1.75-1.65, 1.63-1.53, 1.09-1.04 (4H, m, H-4′, H-5′)
13 C-NMR(CDCl 3 ) δ: 156.2, 156.1, 140.7, 136.4, 128.5, 128.3, 128.1, 127.9, 127.5, 126.2, 75.4, 75.3, 66.7, 65.7, 65.6, 60.4, 60.3, 60.2, 58.2, 57.5, 55.7, 55.1, 52.0, 38.8, 38.7, 26.6, 24.7, 14.2
Example 42
Synthesis of (1S,2S)-2-benzyloxycarbonylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (273.6 mg, 0.722 mmol) was dissolved in ethanol (3ml), sodium iodide (119.2 mg, 0.795 mmol) and 4-hydroxypiperidine (171.5 mg, 1.70 mmol) were added thereto, adn the mixture thus obtained was stirred at room temperature for 4 days. After confirming almost completion of the reaction with TLC (chloroform:methanol=9:1), 4-hydroxypiperidine (157.0 mg, 1.55 mmol) was added thereto, and the obtained mixture was stirred at 45° C. for 2 days. The solvent was removed by evaporation, and the resulting residue was purified-by silica gel column chromatography (chloroform:methanol=20:1) to obtain the objective compound as a colorless oily material (112.6 mg, yield: 40.6%).
TLC Rf:
0.24 (CHCl 3 :MeOH=9:1)
1 H-NMR (CDCl 3 ) δ:
7.36-7.25 (10H, m, aromatic), 5.03 (3H, m, CH 2 —O—CO, NH), 5.00 (1H, d, J=2.93 Hz, H-1), 4.11 (1H, m, H-2), 3.71 (1H, m, H-4′), 2.91, 2.82, 2.64, 2.48, 2.32, (6H, m, (CH 2 ) 3 N), 1.89 (2H, m, H-3′A, H-5′A), 1.64-1.56 (2H, m, H-3′B, H-5′B)
13 C-NMR(CDCl 3 ) δ: 156.1, 140.7, 136.4, 128.5, 128.3, 128.1, 127.9, 127.5, 126.2, 75.4, 66.9, 66.8, 66.7, 59.5, 52.2, 51.9, 34.4
Example 43
Synthesis of (1S,2S)-2-benzyloxycarbonylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol
(1S,2S)-2-Benzyloxycarboylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (270.0 mg, 0.712 mmol) was dissolved in ethanol (3 ml), 4-hydroxypiperidine (287.8 mg, 2.85 mmol) was added thereto, and the mixture thus obtained was stirred at 45° C. for 2 days. After confirming almost completion of the reaction with TLC (chloroform:methanol=9:1), the solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1) to obtain the objective compound as a colorless oily material (170.9 mg, yield: 62.5%).
TLC Rf:
0.24 (CHCl 3 :MeOH=9:1)
Example 44
Synthesis of (1R,2S)-2-benzyloxycarbonylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol
(1R,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (273.6 mg, 0.722 mmol) was dissolved in ethanol (3 ml), 4-hydroxypiperidine (291.7 mg, 2.89 mmol) was added thereto, and the mixture thus obtained wa s stirred at 45° C. for 2 days. After confirming almost completion of the reaction with TLC (chloroform:methanol=9:1), the solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1) to obtain the objective compound as a colorless oily material (184.3 mg, yield: 66.5%).
TLC Rf:
0.24 (CHCl 3 :MeOH=9:1)
Example 45
Synthesis of (1R,2S)-2-benzyloxycarbonylamino-3-(4-hydroxypiperidino)-1-phenyl-1-propanol
(1R,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (295.6 mg, 0.780 mmol) was dissolved in ethanol (3ml), 4-hydroxypiperidine (315.1 mg, 3.12 mmol) was added thereto, and the mixture thus obtained was stirred at 45° C. for 2 days. After confirming almost completion of the reaction with TLC (chloroform:methanol=9:1), the solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1) to obtain the objective compound as a colorless oily material (179.7 mg, yield: 60.0%).
TLC Rf:
0.24 (CHCl 3 ):MeOH=9:1)
1 H-NMR (CDCl 3 ) δ:
7.36-7.25 (10H, m, aromatic), 5.03 (3H, m, CH 2 —O—CO, NH), 5.00 (1H, d, J=2.93 Hz, H-1), 4.11 (1H, m, H-2), 3.71 (1H, m, H-4′), 2.91, 2.82, 2.64, 2.32, (6H, m, (CH 2 ) 3 N), 1.89 (2H, m, H-3′A, H-5′A), 1.64-1.56 (2H, m, H-3′B, H-5′B)
13 C-NMR(CDCl 3 ) δ: 156.1, 140.7, 136.4, 128.5, 128.3, 128.1, 127.9, 127.5, 126.2, 75.4, 66.9, 66.8, 66.7, 59.5, 52.2, 51.9, 34.3
Example 46
Synthesis of (1S,2S)-2-benzyloxycarbonylamino-3-diethanolamino-1-phenyl-1-propanol
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (1.50 g, 3.96 mmol) was dissolved in ethanol (30 ml), diethanolamine (1.69 g, 16.1 mmol) was added thereto, and the mixture thus obtained was stirred at 45° C. for 5 days. After confirming almost completion of the reaction with TLC (chloroform:methanol=9:1), the solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatography (chloroform:methanol=9:1) to obtain the objective compound as a colorless oily material (81.1 mg, yield: 5.3%).
TLC Rf: 0.38 (CHCl 3 :MeOH=9:1)
1 H-NMR (CDCl 3 ) δ: 7.31-7.21 (10H, m, aromatic), 5.48 (1H, d, J=8.79 Hz, NH), 5.04 (1H, d, J=2.44, H-1), 4.95 (2H, m, CH 2 —O—CO), 3.89 (1H, m, H-2), 3.64-3.54 (4H, m, N(CH 2 —CH 2 —OH) 2 ), 2.79, 2.71-2.53 (6H, m, (CH 2 ) 3 N)
13 C-NMR(CDCl 3 ) δ: 156.9, 141.5, 136.4, 128.4, 128.3, 128.0, 127.8, 127.4, 125.9, 72.6, 66.7, 59.9, 57.5, 57.3, 55.5
Example 47
Synthesis of (1S,2S)-2-benzyloxycarbonylamino-3-(4-hydroxycyclohexylamino)-1-phenyl-1-propanol
(1S,2S)-2-Benzyloxycarbonylamino-1-phenyl-1,3-propanediol-3-methanesulfonyl ester (1.21 g, 3.19 mmol) was dissolved in DMF (6 ml), trans-4-aminocyclohexanol (1.47 g, 12.76 mmol) was added thereto, and the mixture thus obtained was stirred at 50° C. for 3 days. After confirming almost completion of the reaction with TLC (chloroform:methanol=9:1), ethyl acetate (100 ml) was added thereto, and the resulting organic layer was washed with a saturated sodium bicarbonate solution (70 ml), water (70 ml) and brine (70 ml) in this order and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under a reduced pressure, the crude product thus obtained was purified by silica gel column chromatography (chloroform:methanol=9:1) to obtain the objective compound as white crystals (571.5 mg, yield: 45.0%).
TLC Rf: 0.18 (CHCl 3 :MeOH=4:1), 0.16 (AcOEt:MeOH=4:1)
1 H-NMR (CDCl 3 ) δ: 7.34-7.23 (10H, m, aromatic), 5.33 (1H, d, NH), 5.07 (1H, s, H-1), 4.98 (2H, m, CH 2 —O—CO), 3.96 (1H, m, H-2), 3.60 (1H, m, H-4′), 3.25 (1H, m, H-3A), 2.89 (1H, m, H-3B), 2.48 (1H, m, H-1′), 1.97 (4H, m, H-2′A, H-3′A, H-5′A, H-6′A), 1.33-1.14 (4H, m, H-2′B, H-3′B, H-5′B, H-6′B)
13 C-NMR(CDCl 3 ) δ: 156.2, 140.8, 136.3, 128.5, 128.3, 128.1, 127.8, 127.4, 125.6, 75.8, 70.0, 66.7, 56.2, 54.7, 49.7, 33.7, 30.9, 30.7
Example 48
Synthesis of (1S,2S)-2-octyloxycarbonylamino-3-morpholino-1-phenyl-1-propanol
(1S,2S)-2-Amino-3-morpholino-1-phenyl-1-propanol (627.7 mg, 2.66 mmol) was dissolved in methanol (10 ml), triethylamine (0.518 ml, 3.723 mmol) was added thereto at room temperature, chloroformic acid n-octyl ester (0.625 ml, 3.192 mmol) was further added thereto on an ice bath, and the mixture thus obtained was stirred at room temperature for 15 hours. After completion of the reaction, methanol (5 ml) was added thereto, the obtained mixture was stirred for 20 minutes, and then the solvent was removed by evaporation under a reduced pressure. Ethyl acetate (100 ml) was added thereto, and the organic layer thus obtained was washed with each 70 ml of a saturated sodium bicarbonate solution, water and brine in this order. The resulting organic layer was dried over anhydrous sodium sulfate, and then filtered, and the solvent was removed by evaporation under a reduced pressure. The crude product thus obtained was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:2) to obtain the objective compound as a colorless oily material (814.5 mg, yield: 78.1%).
TLC Rf: 0.21 (n-Hexane:AcOEt=1:2), 0.32 (CHCl 3 :MeOH=20:1), 0.36 (AcOEt)
1 H-NMR (CDCl 3 ) δ: 7.38-7.26 (5H, m, aromatic), 4.99 (1H, d, J=3.42 Hz, H-1), 4.08 (1H, m, H-2), 3.98 (2H, m, COOCH 2 ), 3.73 (4H, m, (CH 2 ) 2 O), 2.66-2.45 (6H, m, CH 2 N(CH 2 ) 2 ), 1.54 (2H, m, COOCH 2 CH 2 ), 1.27 (10H, m, (CH 2 ) 5 CH 3 ), 0.88 (3H, t, CH 2 CH 3 )
13 C-NMR (CDCl 3 ) δ: 156.5, 140.7, 128.3, 127.6, 126.2, 75.4, 66.9, 65.3, 60.1, 54.4, 52.0, 31.7, 29.2, 29.0, 28.9, 25.7, 22.6, 14.0
Example 49
Synthesis of (1R,2R)-2-octyloxycarbonylamino-3-pyrrolidino-1-phenyl-1-propanol
(1R,2R)-2-Amino-3-pyrrolidino-1-phenyl-1-propanol (250.2 mg, 1.11 mmol) was dissolved in methanol (5 ml), triethylamine (0.186 ml, 1.337 mmol) was added thereto at room temperature, and chloroformic acid n-octyl ester (0.240 ml, 1.226 mmol) was added thereto on an ice bath, and the mixture thus obtained was stirred at room temperature. Ninety minutes thereafter, triethylamine (0.186 ml, 1.337 mmol) and chloroformic acid n-octyl ester (0.240 ml, 1.226 mmol) were added thereto, and the obtained mixture was stirred at room temperature. Twenty hours thereafter, the solvent was removed by evaporation under a reduced pressure, ethyl acetate (100 ml) was added thereto, and the organic layer thus obtained was washed with each 70 ml of a saturated sodium bicarbonate solution, water and brine in this order, dried over anhydrous sodium sulfate, and then filtered. The solvent was removed by evaporation under a reduced pressure, and the crude product thus obtained was purified by silica gel column chromatography (chloroform:methanol=20:1) to obtain the objective compound as a colorless oily material (99.5 mg, yield: 23.8%).
TLC Rf: 0.28 (AcOEt:MeOH=4:1), 0.30 (CHCl 3 :MeOH=9:1)
1 H-NMR (CDCl 3 ) δ: 7.36-7.24 (5H, m, aromatic), 5.05 (1H, d, J=2.93 Hz, H-1), 4.9 (1 H, d, NH), 4.04 (1H, m, H-2), 3.96 (2H, m, COOCH 2 ), 2.91-2.68 (6H, m, CH 2 N(CH 2 ) 2 ), 1.80 (4H, m, H-3′, H-4′), 1.52 (2H, m, COOCH 2 CH 2 ), 1.26 (10H, m, (CH 2 ) 5 CH 3 ), 0.88 (3H, t, CH 2 CH 3 )
13 C-NMR (CDCl 3 ) δ: 156.4, 140.9, 128.2, 127.3, 126.1, 75.6, 65.1, 58.1, 55.2, 53.3, 31.7, 29.1, 28.9, 25.7, 23.6, 22.6, 14.0
Example 50
Synthesis of (1R,2R)-2-decylamino-3-pyrrolidino-1-phenyl-1-propanol
(1R,2R)-2-Decanoylamino-3-pyrrolidino-1-phenyl-1-propanol (181.8 mg, 0.486 mmol) was dissolved in methylene chloride (5 ml), lithium aluminum hydride (153.0 mg, 4.032 mmol) was added thereto at room temperature, and the mixture thus obtained was subjected to reflux at 35 to 40° C. for 2.5 hours. Hydrochloride (1N, 15 ml) was added thereto on an ice bath, and the obtained mixture was stirred for 30 minutes. Further, a saturated sodium bicarbonate solution (70 ml) and chloroform (100 ml) were added thereto, and the organic layer thus obtained was washed with each 70 ml of water and brine in this order, dried over anhydrous sodium sulfate and then filtered. The solvent was removed by evaporation under a reduced pressure, and the crude product thus obtained was purified by silica gel column chromatography (chloroform:methanol=20:1, ethyl acetate:methanol=2:1) to obtain the objective compound as a colorless oily material (121.2 mg, yield: 69.3%).
TLC Rf: 0.39 (CHCl 3 :MeOH=9:1), 0.19 (AcOEt:MeOH=2:1)
1 H-NMR (CDCl 3 ) δ: 7.37-7.22 (5H, m, aromatic), 4.68 (1H, d, J=3.90 Hz, H-1), 2.99 (1H, m, H-2), 2.63-2.42 (8H, m, CH 2 N(CH 2 ) 2 , NHCH 2 ), 1.77 (4H, m, H-3′, H-4′), 1.41-1.24 (16H, m, (CH 2 ) 8 CH 3 ), 0.88 (3H, t, CH 3 )
13 C-NMR (CDCl 3 ) δ: 143.1, 128.1, 127.0, 126.2, 73.9, 61.2, 57.6, 54.5, 48.5, 31.9, 30.2, 29.7, 29.6, 29.4, 29.3, 27.1, 23.6, 22.7, 14.1
Example 51
Synthesis of (1S,2S)-2-benzyloxycarbonylamino-3-morpholino-1-cyclohexyl-1-propanol
(1S,2S)-2-Benzyloxycarbonylamino-1-cyclohexyl-1,3-propanediol-3-methanesulfonyl ester (369.0 mg, 0.958 mmol) was dissolved in a mixture of methylene chloride and methanol (2:1, 5 ml), morpholine (0.25 ml, 2.88 mmol) was added thereto at room temperature, and the mixture thus obtained was stirred at 40° C. Twenty hours thereafter, morpholine (0.083 ml, 0.958 mmol) was further added thereto, and the obtained mixture was stirred at 40° C. for 2 days. After confirming completion of the reaction with TLC (n-hexane:ethyl acetate=1:2), the solvent was removed by evaporation under a reduced pressure, a saturated sodium bicarbonate solution (20 ml) was added thereto, and extraction was conducted with chloroform (30 ml×3 time). The resulting organic layer was dried over anhydrous sodium sulfate and then filtered. The solvent was removed by evaporation under a reduced pressure and the resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:2) to obtain the objective compound as a colorless oily material (61.1 mg, yield: 17.0%).
TLC Rf: 0.36 (CHCl 3 :MeOH=20:1), 0.18 (n-Hexane:AcOEt=1:2)
1 H-NMR (CDCl 3 ) δ: 7.39-7.26 (5H, m, aromatic), 5.11 (2H, m, CH 2 O—CO), 4.98 (1H, br, NH), 3.85 (1H, m, H-2), 3.67 (4H, m, (CH 2 ) 2 O), 3.44 (1H, m, H-1), 2.67-2.48 (6H, m, (CH 2 ) 3 N), 1.86, 1.75, 1.66, 1.53, 1.38, 1.29-1.11 (11H, m)
13 C-NMR (CDCl 3 ) δ: 155.8, 136.4, 128.5, 128.2, 128.0, 127.9, 79.6, 67.0, 66.8, 66.3, 60.9, 54.2, 47.9, 40.6, 29.5, 27.1, 26.4, 26.0, 25.8
Example 52
Synthesis of (1S,2S)-2-decanoylamino-3-morpholino-1-cyclohexyl-1-propanol
(1S,2S)-2-Benzyloxycarbonylamino-3-morpholino-1-cyclohexyl-1-propanol (62.9 mg, 0.167 mmol) was dissolved in methanol (2 ml), 10% palladium-carbon (17.5 mg, 9.83 mol %) was added thereto, and the mixture thus obtained was stirred overnight in an atmosphere of hydrogen at room temperature. After confirming completion of the reaction with TLC (chloroform:methanol=9:1, n-hexane:ethyl acetate=1:3), palladium-carbon was removed by filtration, and the filtrate was concentrated to obtain a oily material (45.0 mg). The oily material was dissolved in methanol (1 ml), triethylamine (34.8 μl, 0.250 mmol) was added thereto, and decanoyl chloride (41.0 μl, 0.200 mmol) was added dropwise thereto under ice cooling. Two hours thereafter, completion of the reaction was confirmed with TLC (ethyl acetate, ethyl acetate:methanol=20:1), and then methanol (5 ml) was added thereto and allowed to stand for 20 minutes. The obtained reaction solution was concentrated under a reduced pressure, and then purified by silica gel column chromatography (ethyl acetate:methanol=40:1) to obtain the objective compound as a colorless oily material (25.3 mg, yield: 38.3%).
TLC Rf: 0.32 (CHCl 3 :MeOH=20:1), 0.28 (Toluene:Acetone=3:1)
1 H-NMR (CDCl 3 ) δ: 5.63 (1H, d, J=8.30 Hz, NH), 4.13 (1H, m, H-2), 3.69 (4H, m, (CH 2 ) 2 O), 3.44 (1H, m, H-1), 2.66-2.49 (6H, m, (CH 2 ) 3 N), 2.20-2.14 (2H, m, CO—CH 2 ), 1.88-1.56, 1.34-1.11 (25H, m), 0.88 (3H, t, CH 3 )
13 C-NMR(CDCl 3 ) δ: 172.7, 77.6, 66.9, 60.6, 54.3, 46.5, 40.9, 36.9, 31.8, 29.5, 29.4, 29.3, 26.4, 26.1, 25.8, 22.6, 14.1
Example 53
Synthesis of (2S,3S)-2-benzyloxycarbonylamino-1-morpholino-3-octadecanol
(2S,3S)-2-Benzyloxycarbonylamino-1,3-octadecanediol-1-methanesulfonyl ester (514.4 mg, 1.003 mmol) was dissolved in a mixture of methylene chloride and methanol (2:1, 5 ml), morpholino (348 μl, 4.00 mmol) was added thereto at room temperature, and the mixture thus obtained was stirred at 40° C. Three days thereafter, morpholine (100 μl, 1.15 mmol) was further added thereto, and the obtained mixture was stirred at 40° C. for 3 days. The solvent was removed by evaporation under a reduced pressure, a saturated sodium bicarbonate solution (20 ml) was added thereto, and extraction was conducted with chloroform (30 ml). The resulting organic layer was dried over anhydrous sodium sulfate and then filtered. The solvent was removed by evaporation under a reduced pressure and the resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:3) to obtain the objective compound as a colorless oily material (50.7 mg, yield: 10.1%).
TLC Rf: 0.35 (n-Hexane:AcOEt=1:3)
1 H-NMR (CDCl 3 ) δ: 7.39-7.26 (5H, m, aromatic), 5.11 (2H, m, CH 2 O—CO), 4.99 (1H, br, NH), 4.46-4.11 (1H, m, H-4A), 3.68 (6H, m, (CH 2 ) 2 O, H-4B, OH), 3.38 (1H, m, H-3), 2.66-2.54 (6H, m, (CH 2 ) 3 N), 1.50, 1.25 (26H, m, (CH 2 ) 13 CH 3 ), 0.88 (3H, t, CH 3 )
Example 54
Synthesis of (2S,3S)-2-decanoylamino-1-morpholino-3-octadecanol
(2S,3S)-2-Benzyloxycarbonylamino-1-morpholino-3-octadecanol (59.2 mg, 0.117 mmol) was dissolved in a mixture of methylene chloride and methanol (1:1, 2 ml), 10% palladium-carbon (21.3 mg, 17.0 mol %) was added thereto, and the mixture thus obtained was stirred in an atmosphere of hydrogen. Three hours thereafter, palladium-carbon was removed by filtration, and the filtrate was concentrated to obtain white crystals (39.7 mg). The white crystals (39.7 mg, 0.107 mmol) was dissolved in a mixture of methylene chloride and methanol (1:1, 2 ml), triethylamine (39.0 μl, 0.280 mmol) was added thereto, decanoyl chloride (48.0 μl, 0.234 mmol) was added dropwise thereto under ice cooling, and the mixture thus obtained was stirred at room temperature for 20 hours. The solvent was removed by evaporation under a reduced pressure, and the obtained residue was purified by silica gel column chromatography (ethyl acetate:methanol=40:1) to obtain the objective compound as a colorless oily material (13.9 mg, yield: 22.6%).
TLC Rf: 0.44 (CHCl 3 :MeOH=20:1), 0.36 (AcOEt:MeOH=40:1)
1 H-NMR (CDCl 3 ) δ: 5.80 (1H, d, J=6.84 Hz, NH), 3.95 (1H, m, H-2), 3.69 (4H, m, (CH 2 ) 2 O), 3.58 (1H, m, H-3), 2.55 (6H, m, (CH 2 ) 3 N), 2.19 (2H, m, CO—CH 2 ), 1.62, 1.41, 1.25 (42H, m), 0.88 (6H, m, CH 3 )
13 C-NMR (CDCl 3 ) δ: 173.5, 74.9, 66.8, 60.1, 54.0, 50.4, 36.8, 34.0, 31.9, 31.8, 29.7, 29.6, 29.4, 29.3, 29.2, 25.8, 22.7, 14.1
Example 55
Synthesis of (2S,3S)-2-benzyloxycarbonylamino-1-morpholino-3-tridecanol
(2S,3S)-2-Benzyloxycarbonylamino-1,3-tridecanediol-1-methanesulfonyl ester (556.2 mg, 1.256 mmol) was dissolved in a mixture of tetrahydrofuran and ethanol (1:1, 4 ml), morpholine (330 μl, 3.79 mmol) was added thereto at room temperature, and the mixture thus obtained was stirred at 40° C. Three days thereafter, morpholine (165 μl, 1.90 mmol) was further added thereto, and the obtained mixture was stirred at 40° C. for 3 days. The solvent was removed by evaporation under a reduced pressure, a saturated sodium bicarbonate solution (20 ml) was added thereto, and extraction was conducted with chloroform (30 ml×3 times). The resulting organic layer was dried over anhydrous sodium sulfate and then filtered. The solvent was removed by evaporation under a reduced pressure and the resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:2) to obtain the objective compound as a colorless oily material (27.1 mg, yield: 5.0%).
TLC Rf: 0.29 (CHCl 3 :MeOH=20:1), 0.28 (n-Hexane:AcOEt=1:2)
1 H-NMR (CDCl 3 ) δ: 7.39-7.25 (5H, m, aromatic), 5.11 (2H, m, CH 2 O—CO), 4.95 (1H, br, NH), 4.47-4.16 (1H, m, H-4A), 3.85-3.62 (6H, m, (CH 2 ) 2 O, H-4B, OH), 3.41 (1H, m, H-3), 2.63-2.41 (6H, m, (CH 2 ) 3 N), 1.52-1.42, 1.26 (16H, m, (C H 2 ) 8 CH 3 ), 0.88 (3H, t, CH 3 )
Example 56
Synthesis of (2S,3S)-2-decanoylamino-1-morpholino-3-tridecanol
(2S,3S)-2-Benzyloxycarbonylamino-1-morpholino-3-tridecanol (25.0 mg, 57.6 μmol) was dissolved in methanol (1 ml), 10% palladium-carbon (16.5 mg, 26.9 mol %) was added thereto, and the mixture thus obtained was stirred in an atmosphere of hydrogen. Two hours thereafter, palladium-carbon was removed by filtration, and the filtrate was concentrated to obtain white crystals (18.4 mg). The white crystals (17.3 mg, 57.6 μmol) were dissolved in methanol (0.5 ml), triethylamine (20.0 μl, 0.143 mmol) was added thereto, and decanoyl chloride (24.0 μl, 0.117 mmol) was added dropwise thereto under ice cooling. One hour thereafter, methanol was added thereto and allowed to stand for 15 hours, the solvent was removed by evaporation under a reduced pressure, and the obtained residue was then purified by silica gel column chromatography (ethyl acetate) to obtain the objective compound as a colorless oily material (10.4 mg, yield: 39.8%).
TLC Rf: 0.41 (CHCl 3 :MeOH=20:1), 0.29 (AcOEt:MeOH=40:1)
1 H-NMR (CDCl 3 ) δ: 5.80 (1H, d, J=6.34 Hz, NH), 3.95 (1H, m, H-2), 3.69 (4H, m, (CH 2 ) 2 O), 3.58 (1H, m, H-3), 2.60-2.55 (6H, m, (CH 2 ) 3 N), 2.19 (2H, m, CO—CH 2 ), 1.62, 1.41, 1.26 (32H, m), 0.88 (6H, m, CH 3 )
13 C-NMR (CDCl 3 ) δ: 173.5, 74.9, 66.8, 60.1, 54.0, 50.4, 36.8, 34.0, 31.9, 31.8, 29.7, 29.6, 29.5, 29.3, 25.8, 22.7, 14.1
Example 57
Synthesis of (2S,3S)-2-benzyloxycarbonylamino-1-morpholino-3-nonanol
(2S,3S)-2-Benzyloxycarbonylamino-1,3-nonanediol-1-methanesulfonyl ester (715.7 mg, 1.850 mmol) was dissolved in a mixture of methyl chloride and methanol (2:1, 10 ml), morpholine (480 μl, 5.51 mmol) was added thereto at room temperature, and the mixture thus obtained was stirred at 40° C. Two days thereafter, morpholine (160 μl, 1.84 mmol) was further added thereto, and the obtained mixture was stirred at 40° C. for 2 days. The solvent was removed by evaporation under a reduced pressure, a saturated sodium bicarbonate solution (20 ml) was added thereto, and extraction was conducted with chloroform (30 ml×3 times). The resulting organic layer was dried over anhydrous sodium sulfate and then filtered. The solvent was removed by evaporation under a reduced pressure and the resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:2) to obtain the objective compound as a colorless oily material (76.1 mg, yield: 10.9%).
TLC Rf: 0.53 (CHCl 3 :MeOH=20:1), 0.29 (n-Hexane:AcOEt=1:2)
Example 58
Synthesis of (2S,3S)-2-decanoylamino-1-morpholino-3-nonanol
(2S,3S)-2-Benzyloxycarbonylamino-1-morpholino-3-nonanol (68.1 mg, 0.180 mmol) was dissolved in methanol (2 ml), 10% palladium-carbon (36.8 mg, 19.2 mol %) was added thereto, and the mixture thus obtained was stirred in an atmosphere of hydrogen. Fifteen hours thereafter, palladium-carbon was removed by filtration, and the filtrate was concentrated to obtain a colorless oily material (55.9 mg). The colorless oily material (43.9 mg, 0.180 mmol) was dissolved in methanol (1 ml), triethylamine (37.6 μl, 0.270 mmol) was added thereto, decanoyl chloride (48.0 μl, 0.234 mmol) was added dropwise thereto under ice cooling, and the mixture thus obtained was stirred at room temperature for 18 hours. The solvent was removed by evaporation under a reduced pressure, and the obtained residue was purified by silica gel column chromatography (ethyl acetate:methanol=20:1) to obtain the objective compound as a colorless oily material (6.0 mg, yield: 8.4%).
TLC Rf: 0.42 (CHCl 3 :MeOH=20:1), 0.44 (AcOEt:MeOH=20:1)
1 H-NMR (CDCl 3 ) δ: 5.80 (1H, d, J=6.35 Hz, NH), 3.95 (1H, m, H-2), 3.69 (4H, m, (CH 2 ) 2 O), 3.59 (1H, m, H-3), 2.55 (6H, m, (CH 2 ) 3 N), 2.19 (2H, m, CO—CH 2 ), 1.62, 1.41, 1.29, 1.28, 1.26 (24H, m), 0.88 (6H, m, CH 3 )
13 C-NMR (CDCl 3 ) δ: 173.5, 74.9, 66.9, 60.1, 54.0, 50.4, 36.8, 34.0, 31.8, 29.5, 29.4, 29.3, 25.8, 25.7, 22.6, 14.1
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
This application is based on application No. Hei 7-345080 filed in Japan, the content of which is incorporated hereinto by reference. | A process for preparing a 2-acylamino alcohol derivative which comprises (A) reacting an aminopropanol derivative represented by the following formula (1):
Y—CH 2 —C*H (NHP 1 )—C*H(OH)—R 1 (1)
with an amine represented by R 2 H to synthesize an amino alcohol derivative represented by the following formula (2):
R 2 —CH 2 —C*H(NHP 1 )—C*H(OH)—R 1 (2)
(B) leaving P 1 from said amino alcohol derivative represented by formula (2) to synthesize an amino alcohol derivative represented by the following formula (3):
R 2 —CH 2 —C*H(NH 2 )—C*H(OH)—R 1 (3)
(C) reacting said amino alcohol derivative represented by formula (3) with a carboxylic acid represented by R 11 COOH or a reactive derivative thereof to prepare a 2-acylamino alcohol derivative represented by the following formula (4):
R 2 —CH 2 —C*H(NHCOR 11 )—C*H(OH)—R 1 (4 )
wherein * represents an asymmetric carbon atom, and P 1 , R 1 , R 2 and R 11 are defined in the specification. A process for preparing alcohol derivatives having an acylamino group through several steps from amino group-protected 2-aminopropanol derivatives, and novel amino alcohols useful as intermediates in the process for preparing the alcohol derivative. | 2 |
BACKGROUND OF THE INVENTION
[0001] The present invention relates to a device that can replace the power supply, control module and foot pedal operational switch that is used to operate a conventional tattoo gun. More particularly, to a battery powered portable system of operating a tattoo gun that can be worn on the user's arm, offers fingertip control of the machine's speed and ON/OFF functions, and can be directly substituted in place of the detachable power cord found in the industry standardized tattoo machines.
[0002] A conventional, prior art tattoo machine has four major components; a tattoo gun, an operational foot switch, a connector cable, and a control unit. The control unit is a bulky enclosure that is connected to an AC power source and has an AC/DC transformer that outputs DC power to a small DC oscillating motor located on the tattoo gun that rapidly strokes the inking needle. The voltage of the DC power output is manually adjusted on the control unit to change the speed of the motor. The operational foot switch allows DC power to the tattoo gun through the connector cable. In operation, the tattoo artist has to go back and forth between the control unit to adjust the needle speed and has to start and stop the needle with the foot pedal. This is awkward to operate and the artist is somewhat constrained by the length of the connector cable.
[0003] There are newer DC operated portable tattoo machines available but these have problems. They are sold as complete units that are very expensive. Additionally, most tattoo artists work and develop their artistic skills with the same tattoo guns for years and are accustomed to the weight, balance, feel and response of that gun. They are not inclined to change. The retrofit control system and power supply is an electronic DC power supply unit with interchangeable batteries that has an LCD visual interface, a spring loaded tattoo gun connection clip with a speed adjustment means thereon, and a fingertip microswitch that can be removably mounted on the tattoo gun where the artist prefers. It is small and light enough to be worn on the arm of the tattoo artist in an elastic pouch.
[0004] The retrofit control system and power supply fulfills a long felt need in the field of tattoo machines. It allows tattoo artists freedom of movement, portability, fingertip control of the gun's operation and speed, and a visual status of battery condition and operating parameters. This new invention utilizes and combines known and new technologies in a unique and novel configuration to overcome the aforementioned problems of the prior art.
SUMMARY OF THE INVENTION
[0005] The general purpose of the present invention, which will be described subsequently in greater detail, is to provide a retrofit control and DC power supply system that is able to connect to existing tattoo guns without any modifications. It has many of the advantages mentioned heretofore and many novel features that result in a new invention which is not anticipated, rendered obvious, suggested, or even implied by any of the prior art, either alone or in any combination thereof.
[0006] In accordance with the invention, an object of the present invention is to provide an improved retrofit control and DC power supply system for a tattoo gun that is small and light enough to be worn on the arm or clipped to a belt.
[0007] It is another object of this invention to provide an improved retrofit control and DC power supply system for a tattoo gun capable of uninterrupted operation through the use of multiple rechargeable, replaceable batteries.
[0008] It is a further object of this invention to provide a retrofit control and DC power supply system for a tattoo gun that gives the artist a visual status of the battery condition and the tattoo gun speed setting.
[0009] It is still a further object of this invention to provide for a retrofit control and DC power supply system for a tattoo gun that incorporates an ON/OFF switch that may be removably mounted on the barrel of the gun.
[0010] The subject matter of the present invention is particularly pointed out and distinctly claimed in the concluding portion of this specification. However, both the organization and method of operation, together with further advantages and objects thereof, may best be understood by reference to the following description taken in connection with accompanying drawings wherein like reference characters refer to like elements. Other objects, features and aspects of the present invention are discussed in greater detail below.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is a top view of the retrofit control and DC power supply system connected to a tattoo gun in the conventional configuration showing the general arrangement of all components;
[0012] FIG. 2 is a top view of the retrofit control and DC power supply connected to a tattoo gun in the preferred configuration showing the general arrangement of all components;
[0013] FIG. 3 is a side view of the retrofit control and DC power supply system control unit and removable battery;
[0014] FIG. 4 is a perspective view of the retrofit control and DC power supply system control unit with installed battery and the elastic arm strap;
[0015] FIG. 5 is the electrical schematic for the retrofit control and DC power supply system;
[0016] FIG. 6 illustrates the alternate embodiment retrofit control system and power supply for a tattoo gun with the side cover plate on;
[0017] FIG. 7 illustrates the alternate embodiment retrofit control system and power supply for a tattoo gun with the side cover plate removed; and
[0018] FIG. 8 illustrate the alternate embodiment retrofit control system and power supply for a tattoo gun prior to installation on a tattoo gun.
DETAILED DESCRIPTION
[0019] There has thus been outlined, rather broadly, the more important features of the invention in order that the detailed description thereof that follows may be better understood and in order that the present contribution to the art may be better appreciated. There are, of course, additional features of the invention that will be described hereinafter and which will form the subject matter of the claims appended hereto.
[0020] 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 other embodiments and of being practiced and carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein are for the purpose of descriptions and should not be regarded as limiting.
[0021] The retrofit control and DC power supply system (system) is configured in a conventional embodiment 4 ( FIG. 1 ) and a preferred embodiment 2 ( FIG. 2 ). Each of these embodiments utilize the same control unit 6 and the same tattoo gun 8 but differ in the components connected to these. The conventional system 4 has a jack connectable foot switch 10 and a jack connectable first spring clip power cable 12 . Although each of these are shown connecting to the control unit 6 with input jack connectors 14 it is well known in the art that there is a plethora of electrical connectors or hard wiring that would accomplish the same task. The preferred embodiment system 2 has only a pin connector attached second spring clip power cable 13 connected to a spring clip power connector 40 with a removably connected tactile remote switch 15 attached thereto.
[0022] The control unit 6 utilized in each of the embodiments has an outer casing that houses the printed circuit board with the operational circuit components thereon, a battery 16 , the first spring clip power control cable pin connector 20 , the second spring clip power cable jack connector 24 , the foot switch cable jack connector 22 , the display interface 26 , the power button 30 , the battery status indicator button 31 and the speed (tattoo gun voltage) control buttons 32 . The outer casing has a belt clip 28 affixed to its bottom face. The operational circuit 34 ( FIG. 5 ) that is used in both embodiments is identical although different electrical pathways are utilized for the operation of the foot switch 10 and the speed control buttons 32 versus the tactile switch 15 and the speed adjustment potentiometer 35 .
[0023] Looking at FIG. 3 it can be seen that the replaceable, rechargeable battery 16 slideably engages into control unit 6 so as to matingly connect their electrical contacts as is well known in the industry and not illustrated. When the electrical contacts are engaged fully the battery 16 and control unit 6 are a mechanically interlocked solid unit. This is accomplished through the use of physically engageable configurations which require the depression of unlock buttons 18 on the battery 16 as is well known in the field of battery powered devices and not discussed or illustrated in detail herein.
[0024] In the preferred embodiment 2 the first spring clip power control cable 13 plugs into spring clip power connector 40 that houses thereon a tactile switch 15 (that is used rather than the foot control switch 10 ) and a speed adjustment potentiometer 35 (that is used rather than speed control buttons 32 .) The first spring clip power control cable 13 has conventional pin connectors on both its distal and proximate ends that connect to the control unit 6 and the spring clip power connector 40 . The spring clip power connector 40 has a pair of spring loaded arms 42 that open and close to engage a pair of matingly conformed contactors 44 that are located on the gun 8 and provide the power to the gun. It also has a speed adjustment potentiometer 35 integrated therein and a detachable tactile switch 15 connected by plug connector halves 46 . The tactile switch 15 switches on and off the power to the gun 8 and is mountable anywhere on the gun 8 by mechanical means such as rubber bands, cable ties, glue or screws, however the likely location for mounting would be the top surface of the tattoo gun's barrel where the artist's index finger could readily access it. When in the preferred configuration, the speed control buttons 32 do not function as this function is now operated through the speed adjustment potentiometer 35 . The preferred embodiment 2 does not have the foot switch 10 or the second spring clip power cable 12 plugged into the control unit 6 .
[0025] The preferred embodiment unit 2 is retrofit onto a conventional tattoo machine by simply disengaging the conventional spring cable and engaging the distal end of the first spring clip power control cable 14 into the spring clip power connector 40 , then manipulating the pair of spring loaded arms 42 to engage the contactors 44 on the tattoo gun 8 the connecting the proximate end of the first spring clip power control cable 14 to a control unit 6 with an operable battery 16 installed. Finally, the tactile switch 15 is coupled to the spring clip power connector 40 via the plug connector halves 46 and mechanically affixed to the tattoo gun 8 .
[0026] In operation, the preferred embodiment 2 once connected is switched on via the power indicator button 30 , and the battery status button 31 is depressed to display the battery voltage, then depressed again to display the tattoo gun voltage in the display interface 26 . The preferred embodiment 2 is slid into the elastic pocket 48 on the elastic arm band 50 such that the display interface 26 is visible, and then the entire unit is slid onto the artist's arm. (Optionally the entire unit may be clipped onto the artist's belt.) The artist adjusts the speed adjustment potentiometer 35 to adjust the voltage to make the tattoo gun 8 operate at the desired speed and then depresses the tactile switch 15 as needed to ink the patron. In this preferred embodiment the speed control buttons 32 are electronically bypassed and the potentiometer 35 handles this function.
[0027] The conventional embodiment unit 4 is retrofit onto a conventional tattoo machine by simply engaging the jack 14 on the first spring clip power cable 12 into the spring clip power cable jack connector 24 , and engaging the jack 14 on the foot switch 10 into the foot switch cable jack connector 22 on control unit 6 since the spring clip 11 is already connected to the conventional tattoo machine it came from.
[0028] In operation, the conventional embodiment 4 once connected is switched on via the power indicator button 30 , and the battery status button 31 is depressed to display the battery voltage, then depressed again to display the tattoo gun voltage in the display interface 26 . The preferred embodiment 2 is slid into the elastic pocket 48 on the elastic arm band 50 such that the display interface 26 is visible, and then the entire unit is slid onto the artist's arm. (Optionally the entire unit may be clipped onto the artist's belt.) The artist adjusts the speed adjustment buttons 32 to make the tattoo gun 8 operate at the desired speed as indicated on the display interface 26 and then depresses the foot switch 10 as needed to ink the patron. In this conventional embodiment 4 the speed control buttons 32 and the foot switch 10 operate to allow the inking of the patron.
[0029] The operational circuit 34 is best described looking at FIG. 5 . Power comes in from the battery source 52 via the main power electronic switch 30 through ON/OFF relay 54 to the first voltage regulator 56 and then to the second voltage regulator 58 . The circuit is completed (energized) to allow power to the spring clip power connector 40 (and tattoo gun 8 ) by either of the grounding out of current through the gun trigger switch 11 or the foot pedal 10 . The first voltage regulator 54 adjusts the operating voltage of the control unit 6 for the operation of the voltmeter 60 and the solid state switches thereon. The second voltage regulator 56 maintains a stable voltage for the operation of the tattoo gun 8 (maintains constant voltage as the battery power is dissipated.) Power taken across voltmeter 60 provides a voltage readout of the battery condition or of the actual output power to the tattoo gun 8 by operation of battery status button 31 . Power then proceeds through a transistorized voltage regulator 62 that adjusts the speed of the gun. This is a three prong regulator that has the middle prong connected to a potentiometer that adjustably bleeds the voltage to ground. (This is the potentiometer that is integrated into the spring clip power connector 40 or the speed adjustment buttons 32 built into the control unit 6 .) Power then proceeds to the switching relay 64 that is energized to allow the circuit to complete through the tattoo gun motor after the ON/OFF power switch 30 or foot pedal 10 is activated.
[0030] The voltage is capped (limited) by the first voltage regulator 56 . An internal voltage regulating potentiometer 63 adjusts the power going to the tattoo gun 8 such that it does not exceed the max voltage needed to run the tattoo gun 8 .
[0031] Eventually it may be possible to mount the control unit/battery assembly to the gun itself as batteries miniaturize and the vibrate coils/relays of the gun become more efficient, requiring less voltage to operate. At this time to accomplish such a task would make a tattoo gun that is too bulky, heavy and unwieldy to work with.
[0032] The conventional method of vibrating the tattoo gun's needle utilizes a rapidly moving coil wrap motor. This coil can be replaced by stacked arrangement of piezoelectric motors 71 (piezo stacker electric motor) or a conventional motor and flywheel assembly that would still vibrate the needles in an up and down motion by the rapid vibration of a moveable bar connected mechanically to the needles.
[0033] FIGS. 6 , 7 and 8 illustrate the alternate embodiment retrofit control system 100 and power supply for a tattoo gun with the side cover plate on, with the side cover plate removed and prior to installation on a tattoo gun 8 . In this embodiment the retrofit system 100 is self contained in case that is directly mounted onto the tattoo gun's 8 main support frame 102 by mechanical fasteners, preferably screws or nuts and bolts. The system case has a support base 73 from which a vertical support 108 extends normally. The system 100 is mounted on the gun 8 in place of the original magnetic coils. A voltage and frequency generator 72 , the battery 16 and the piezo stacker electric motor are mounted in the system case 104 below the drive arm 74 which swings about the pivot 75 on the vertical support 108 . The electronics (which function essentially similar to those of the preferred embodiment described herein and are also mounted onto a printed circuit board) reside on the case panel 110 on the side of the system case 104 . The system electronics include main power electronic switch 30 , display interface 26 , battery status button 31 and needle speed control 32 . Similar to the preferred embodiment, tactile switch 15 switches on and off the power to the gun 8 and is mountable anywhere on the gun 8 by mechanical means such as rubber bands, cable ties, glue or screws, however the likely location for mounting would be the top surface of the tattoo gun's barrel 112 where the artist's index finger could readily access it. A screw adjust means 70 affixed to the support base 73 adjusts the tension on spring 73 that controls the rebound of the drive arm 74 to adjust the force and speed of the needle.
[0034] The mechanical oscillation to drive the tattoo gun needle is generated by voltage coming from the battery 16 that enters the voltage/frequency regulator 72 . There is a DC square wave generated at a frequency and voltage set by the user though needle speed control 32 . This DC square wave of current travels to the piezo stacker motor 71 which expands vertically as the positive voltage is applied, and returns to its neutral (or compressed) thickness when the voltage returns to zero. When the piezo stacker motor 71 expands it pushes on the drive arm 74 with its fulcrum body 118 causing it to swing about pivot 75 . The proximity of the fulcrum body 118 to the pivot 75 multiplies the movement of the piezo motor at the distal end of the drive arm 74 . This oscillating movement is transmitted to the needle by virtue of the connection between the distal end of drive arm 74 and the distal arm of the needle 120 .
[0035] It is to be noted that with this system the piezo stacker motor 71 only withdraws the needle and the screw adjuster means 70 and spring 73 control the insertion of the needle.
[0036] It is well known it the art that the location of the peizo electric motor 71 may be varied to different locations in the case (I.E. above the drive arm 74 to drive the arm down or on an section of the drive arm 74 extending beyond the pivot 75 to pivot it down.) Different spring locations and/or types may be used and batteries may be mounted in different locations depending on weight size and balance.
[0037] The above description will enable any person skilled in the art to make and use this invention. It also sets forth the best modes for carrying out this invention. There are numerous variations and modifications thereof that will also remain readily apparent to others skilled in the art, now that the general principles of the present invention have been disclosed. 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. | A battery powered portable system of operating a tattoo gun that can be worn on the user's arm or clipped to the user's belt. The system directly connects to conventional tattoo guns, and offers the options of utilizing a fingertip control of the machine's speed and ON/OFF functions or the conventional control module and foot pedal controls. | 0 |
RELATED APPLICATIONS
This application claims priority to European Application No. EP 07102250.3, filed Feb. 13, 2007, the teachings and content of which are hereby incorporated by reference herein.
SEQUENCE LISTING
This application contains a sequence listing in computer readable format, the teachings and content of which are hereby incorporated by reference. The sequence listing is identical with that found in European Patent Application No. EP 07102250.3 and in WO06/072065, the teaching and content both of which are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to the use of an immunogenic composition comprising a porcine circovirus type 2 (PCV2) antigen for the prevention and treatment of sub-clinical (chronic) PCV2 infections in animals, preferably in pigs.
2. Description of the Prior Art
Porcine circovirus type 2 (PCV2) is a small (17-22 nm in diameter), icosahedral, non-enveloped DNA virus, which contains a single-stranded circular genome. PCV2 shares approximately 80% sequence identity with porcine circovirus type 1 (PCV1). However, in contrast with PCV1, which is generally non-virulent, infection of swine with PCV2 has recently been associated with a number of disease syndromes which have been collectively named Porcine Circovirus Diseases (PCVD) (also known as Porcine Circovirus associated Diseases (PCVAD)) (Allan et al, 2006, IPVS Congress). Postweaning Multisystemic Wasting Syndrome (PMWS) is generally regarded to be the major clinical manifestation of PCVD (Harding et al., 1997, Swine Health Prod; 5: 201-203; Kennedy et al., 2000, J Comp Pathol; 122: 9-24). Other potentially related conditions reported in the literature include porcine respiratory disease complex (PRDC), porcine dermatopathy and nephropathy syndrome (PDNS), reproductive failure, granulomatous enteritis, and potentially, congenital tremors (CT-AII) and perinatal myocarditis (Chae, Veterinary J., 2005; 169: 326-336).
PCVD affects pigs between 5-22 weeks of age. PCVD is clinically characterized by wasting, paleness of the skin, unthriftiness, respiratory distress, diarrhea, icterus, and jaundice. In some affected swine, a combination of all symptoms will be apparent while other affected swine will only have one or two of these symptoms (Muirhead, 2002, Vet. Rec.; 150: 456). The mortality rate for swine infected with PCV2 can approach 50%. During necropsy, microscopic and macroscopic lesions also appear on multiple tissues and organs, % with lymphoid organs being the most common site for lesions (Allan and Ellis, 2000; J. Vet. Diagn. Invest., 12: 3-14). A strong correlation has been observed between the amount of PCV2 nucleic acid or antigen and the severity of microscopic lymphoid lesions (Brunborg, 2004). In addition, correlation has also been found for the amount of nucleic acid or antigen in blood and the severity of the clinical symptoms (Brunborg, 2004; Liu, 2000; Olvera, 2004). Pigs suffering from PCVD have been shown to have viral loads that are higher than 10 6 genomic equivalents per ml.
In contrast to clinically apparent disease manifestations of PCV2 infection, sub -clinical PCV2 infections are thought to be present in those animals that are infected with PCV2 but are clinically asymptomatic. In general, a relationship exists between these forms of PCV2 infection since sub-clinical infections may easily transition into PCVD, and since convalescent animals may stay persistently (chronically) infected (see FIG. 1 ).
Recent observations have demonstrated that sub-clinical PCV2 infections are frequent events. The existence of sub-clinical infections has been demonstrated by both experimental and field studies. In laboratory studies it could be shown that PCV2 infection in individual pigs is not always associated with clinical signs or lesions (Harms et al., 2001, Vet. Pathol., 38:528-539). In addition, several field studies have shown that the incidence of PCV2 infected, seropositive herds is higher than the incidence of herds affected with PCVD (Olvera et al., 2004, J. Virol. Methods, 117: 75-80). Often, herds that have experienced an acute outbreak of PCVD remain PCV2 infected without showing any apparent clinical signs. According to the literature this form of sub-clinical (persistent) infection within a herd is also called “chronic” infection (Burch D., 2006, Pig International).
The economical impact of PCV2 in sub-clinically infected herds, if any, is unknown and has never been described so far. In particular, it was not known and no indication was ever given whether sub-clinical cases of PCV2 infections have any impact on growth performance of animals or, in general, on the overall health of the affected animals.
Approaches to treat PCV2 infections based on a DNA vaccine are described in U.S. Pat. No. 6,703,023. In WO 03/049703 production of a live chimeric vaccine is described, comprising a PCV1 backbone in which an immunogenic gene of a pathogenic PCV2 strain replaces a gene of the PCV-1 backbone. WO99/18214 has provided several PCV2 strains and procedures for the preparation of a killed PVC2 vaccine. However, no efficacy data have been reported. An effective ORF-2 based subunit vaccine has been reported in WO06/072065. Any of such vaccines are intended to be used for the vaccination/treatment of swine or pigs older than 3 weeks of age. None of these vaccines have ever been described for the prophylaxis or treatment of animals sub-clinically infected with PCV2. Moreover, such vaccines have not been described to confer immunity against PCV2 infection in sub-clinically infected groups of animals and/or to improve their growth performance.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic representation of the different forms of PCV2 infections and their relatedness;
FIG. 2 is a graph of the mortality rate and average daily weight gain in fattening on the study farm before and after study initiation;
FIG. 3 is a graph illustrating the development of the relative body weight difference (IVP-CP) and of the mean virus load (log 10) over the course of the study;
FIG. 4 is a graph illustrating a comparison of the percentage of animals with a virus load of >10 6 genomic equivalents/ml of serum in both treatment groups; and
FIG. 5 is a graph illustrating a comparison of the percentage of animals with a virus load of 10 4 -10E 6 genomic equivalents/ml of serum in both treatment groups.
DISCLOSURE OF THE INVENTION
Clinically apparent PCV2 infections are associated with different disease syndromes. Depending on the PCV2-related disease expression form, clinical signs of an acute PCV2 infection may be one or more of the following findings: a) a significantly increased mortality rate (4-20% higher), b) a significant increase in the frequency of runts (5-50% more) and c) other clinically apparent signs such as respiratory symptoms, diarrhea, paleness of the skin, icterus, and unthriftiness (morbidity rate 4-60%). In addition, high viral titers of more than 10 6 or 10 7 per ml serum or tissue are a characteristic finding in most of the animals with acute signs of PCVD. Beside this acute PCV2 infection, sub-clinical PCV2 infections characterized by no or a low morbidity rate become more and more visible. In some cases, a situation of an acute PCV2 infection might shift into a sub-clinical PCV2 infection. However, sub-clinical infections may also occur without any previous sign of an acute PCV2 infection.
It has been surprisingly found that a sub-clinical PCV2 infection has a significant impact on performance parameters of apparently healthy pigs, and in particular the growth performance of pigs. Even if sub-clinically infected animals do not develop typical clinical symptoms which allow the identification of PCVD or do show only a low morbidity, those animals are significantly affected by the sub-clinical PCV2 infection. Sub-clinical infections of pigs with PCV2 result in a significant growth impairment including loss in weight gain (e.g. see example 3). As already mentioned, no evidence is given in the prior art so far that sub-clinical PCV2 infections have any impact on the health, and in particular on the growth performance of pigs.
Moreover, it has also been surpisingly found that growth impairment including reduction in weight gain caused by a sub-clinical PCV2 infection can be reduced by the treatment/vaccination of animals that become sub-clinically infected with PCV2 antigen (e.g. see example 3). Thus, it was not only found that the sub-clinical PCV2 infections affect the growth performance of pigs, evidence is also given that such a negative impact can be significantly reduced by treatment/vaccination of animals with PCV2 antigen. In other words, even if the phenomenon of sub-clinical infections have been described in the prior art, evidence is given now for the first time that
the sub-clinical PCV2 infection, occasionally observed in the field, has a significant impact on the growth performance of pigs; vaccination of sub-clinically affected pigs or herds with PCV2 antigen can significantly reduce the negative impact of this sub-clinical PCV2 infection.
Therefore, according to one aspect, the present invention provides a method for the prophylaxis and treatment of a sub-clinical PCV2 infection in an animal or a group of animals, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to an animal in need of such administration.
A “sub-clinical PCV2 infection” as used herein is characterized by i) a viral load in an individual animal that remains during the entire life below 10 6 genomic copies of PCV2 per ml serum, ii) a low proportion of PCV2 positive animals within a group or herd with viral titers of more than 10 6 genomic copies per ml serum, iii) a virus persistence in a group or herd of at least 6 weeks, preferably of at least 8 weeks, more preferably of at least 10 weeks, and most preferably of at least 12 weeks, iv) the absence of typical clinical symptoms in a PCV2 positive animal, v) no or only a low morbidity rate within a group of animals or herd of PCV2 positive animals and/or vi) a low mortality rate within a group of PCV2 positive animals or herd.
The term “low proportion of PCV2 positive animals” as used in criteria ii) above means that less than 20%, preferably less than 15%, even more preferably less than 10%, even more preferably less than 8%, even more preferably less than 6%, even more preferably less than 4%, and most preferably less than 3% of the PCV-2 positive animals within a group of animals or a herd have viral titers of more than 10 6 genomic copies per ml serum. In other words, the term a “low proportion of PCV2 positive animals within a group or herd with viral titers of more than 10 6 genomic copies per ml serum” also means, that more than 80%, preferably more than 85%, even more preferably more than 90%, even more preferably more than 92%, even more preferably more than 94%, even more preferably more than 96%, and most preferably more than 97% of the PCV2 positive animals of a group of animals or herd have viral titers of less than 10 6 genomic copies of PCV2 per ml serum.
The term “PCV2 positive” as used herein means, but is not limited to, an animal that comprises a detectable amount of PCV2 genome equivalents (=viral copies) in a sample (1 ml serum or 1 mg tissue). A detectable amount of PCV2 genome equivalents means that PCV2 genome equivalents can be detected by a polymerase chain reaction (PCR) assay. A sample is considered PCR positive if two independent samples due to a positive PCR result in such assay.
Methods for quantification of PCV2 via a PCR assay are well known in the art. Actually, the quantification of PCV2 genome equivalents was/is done by the method described in Brunborg et al., 2004; J. Virol Methods 122: 171-178. For amplification of PCV2, primers PCV2-84-1265U21 and PCV2-84-1319L21 were/are used. Such methods shall function as reference assay in any case of doubt.
The term “virus persistence” as used herein means that the infected animal has a viral load of at least 10 4 viral copies of PCV2 per ml serum for such period of time, i.e. for at least 6 weeks or longer as defined above.
The term “the absence of typical clinical symptoms in PCV2 positive animal”, as used herein means the absence of any apparent clinical symptions normally associated with a clinically apparent PCV2 infection, that allow a precise and undoubtful identification of a PCV2 infection only by its typical clinical appearance. Such clinical symptoms are those known as PCVD, in particular paleness of the skin, unthriftiness, respiratory distress, diarrhea, icterus, or jaundice.
The term “low morbidity rate” as used herein is an indicator for the absence of clinical signs which allows the identification of an acute PCV2 infection by its clinical appearance. It is therefore an indicator for the existence of a sub-clinical PCV2 infection. The term “low morbidity rate” as used herein refers to the percentage of animals with altered general health. “Altered general health” as used herein is defined as the presence of one or more PCVD related clinical signs such as the occurrence of runts (defined herein as animals with a body weight 25% less than the mean weight of its animal group of the same age), paleness of the skin, unthriftiness, respiratory distress, diarrhea, icterus, or jaundice. Thus, a “low morbitidy” as used herein, means that less than 25%, preferably less than 20%, more preferably less than 15%, even more preferably less than 12%, even more preferably less than 10%, even more preferably less than 8%, even more preferably less than 6% and most preferably less than 4% of the animals of a group of animals or herd do show one or more clinical symptoms of PCVD, and more preferably do show the occurrence of runts as defined above, paleness of the skin, unthriftiness, respiratory distress, diarrhea, icterus, or jaundice.
The term “no morbidity rate” as used herein means, that less than 1% of the PCV2 positive animals of a group of animals or herd do show one or more clinical symptoms of PCVD, and more preferably do show the occurrence of runts as defined above, paleness of the skin, unthriftiness, respiratory distress, diarrhea, icterus, or jaundice.
The term “low mortality rate” as used herein means, but is not limited to, a mortality rate of less than 20%, preferably of less than 15%, more preferably of less than 12%, even more preferably of less than 10%, even more preferably of less than 8%, even more preferably of less than 6%, and most preferably of less than 4% of the PCV2 positive animals within a group of animals or a herd.
The term “in need of such administration” or “in need of such administration treatment”, as used herein means that the administration/treatment is associated with prevention of health or any other positive medicinal effect on health of the animals which receive the PCV2 antigen.
According to a preferred embodiment, a sub-clinical case of a PCV2 infection is given, when at least criteria i) “a viral load in an individual animal that remains during the entire life below 10 6 genomic copies of PCV2 per ml serum”, criteria ii) “a low proportion of PCV-2 positive animals within a group or herd with viral titers of more than 10 6 genomic copies per ml serum” or criteria iii) “a virus persistence in a group or herd of at least 6 weeks, preferably of at least 8 weeks, more preferably of at least 10 weeks, and most preferably of at least 12 weeks” mentioned above are applicable. Most preferably a sub-clinical case of PCV2 infection is given, when criteria i) and ii) as mentioned above, are applicable.
In cases, where criteria i) and/or criteria ii) is combined with criteria iii) “a virus persistence in a group or herd of at least 6 weeks, preferably of at least 8 weeks, more preferably of at least 10 weeks, and most preferably of at least 12 weeks”, or in any other cases comprising criteria iii) as defined above, the sub-clinical infection is considered to be a “chronic sub-clinical PCV2” infection.
According to a further aspect, the present invention provides a method for the prophylaxis and treatment of a sub-clinical PCV2 infection, wherein the sub-clinical PCV2 infection is characterized by a viral load in an individual animal of below 10 6 genomic copies of PCV2 per ml serum, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to that animal in need of such administration. Preferably, that sub-clinical PCV2 infection is further characterized by the presence of less than 20% of the animals with more than 10 6 preferably more than 10 7 viral copies of PCV2 per ml serum within a group of animals or a herd and/or a virus persistence in such group or herd of at least 6 weeks, preferably of at least 8 weeks, more preferably of at least 10 weeks, and most preferably of at least 12 weeks. More preferably, that sub-clinical infection is further characterized by the absence of any clinical signs in an individual PCV2 positive animal as defined above, no or a low morbidity rate as defined above, and/or a low mortality rate as defined above.
According to a further aspect, the present invention provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, wherein the sub-clinical PCV2 infection is characterized by a viral load in an individual animal that would remain during the entire life below 10 6 genomic copies of PCV2 per ml serum in the absence of any PCV2 antigen administration, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to that animal in need of such administration. Preferably, that sub-clinical PCV2 infection is further characterized by the presence of less than 20% of the animals with more than 10 6 preferably more than 10 7 viral copies of PCV2 per ml serum within a group of animals or a herd and/or a virus persistence in such group or herd of at least 6 weeks, preferably of at least 8 weeks, more preferably of at least 10 weeks, and most preferably of at least 12 weeks. More preferably, that sub-clinical infection is further characterized by the absence of any clinical signs in an individual PCV2 positive animal as defined above, no or a low morbidity rate as defined above, and/or a low mortality rate as defined above.
According to a further aspect, the present invention provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, wherein the sub-clinical PCV2 infection is characterized by the presence of less than 20% of the animals with more than 10 6 preferably more than 10 7 viral copies of PCV2 per ml serum within a group of animals or a herd, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to that animal in need of such administration. Preferably, that sub-clinical PCV2 infection is further characterized by a virus persistence in such group or herd of at least 6 weeks, preferably of at least 8 weeks, more preferably of at least 10 weeks, and most preferably of at least 12 weeks. More preferably, that sub-clinical infection is further characterized by the absence of any clinical signs in an individual PCV2 positive animal as defined above, no or a low morbidity rate as defined above, and/or a low mortality rate as defined above.
According to a further aspect, the present invention provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, wherein the sub-clinical PCV2 infection is characterized by a virus persistence in a group of PCV2 positive animals or herd of at least 6 weeks, preferably of at least 8 weeks, more preferably of at least 10 weeks, and most preferably of at least 12 weeks. Preferably, that sub-clinical PCV2 infection is further characterized by the absence of any clinical signs in an individual PCV2 positive animal as defined above, no or a low morbidity rate as defined above, and/or a low mortality rate as defined above.
According to a further aspect, the present invention also provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, wherein the sub-clinical PCV2 infection is characterized by the absence of any clinical signs in an individual PCV2 positive animal as defined above, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to an animal in need of such administration. Preferably, that sub-clinical PCV2 infection is further characterized by no or a low morbidity rate as defined above, and/or a low mortality rate as defined above. More preferably, such sub-clinical PCV2 infection is further characterized by a viral load in an individual animal that remains during the entire life below 10 6 genomic copies of PCV2 per ml serum and/or a low proportion of PCV-2 positive animals within a group or herd with viral titers of more than 10 6 genomic copies per ml serum.
According to a further aspect, the present invention also provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, wherein the sub-clinical PCV2 infection is characterized by no or low morbidity in a group of animals or a herd, preferably of less than 25% or lower as defined above, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to an animal in need of such administration. Preferably, such sub-clinical PCV2 infection is further characterized by a viral load in an individual animal that remains during the entire life below 10 6 genomic copies of PCV2 per ml serum and/or a low proportion of PCV2 positive animals within a group or herd with viral titers of more than 10 6 genomic copies per ml serum.
According to a further aspect, the present invention also provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, wherein the sub-clinical PCV2 infection is characterized by low mortality rate as defined herein, preferably of less than 20% or lower, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to an animal in need of such administration. Preferably, such sub-clinical PCV2 infection is further characterized by a viral load in an individual animal that remains during the entire life below 10 6 genomic copies of PCV2 per ml serum and/or a low proportion of PCV2 positive animals within a group or herd with viral titers of more than 10 6 genomic copies per ml serum.
The administration of an effective amount of PCV2 antigen to animals or a group of animals that are sub-clinically infected with PCV2 results in an enhanced weight gain of those animals in fattening, in reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, in reduction of virus nasal shedding, and/or in reduction of duration of viremia.
Thus according to a further aspect, the present invention also provides a method for reduction of loss of weight gain in animals sub-clinically infected with PCV2, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to an animal in need of such administration. Preferably, average weight gain is increased in weeks 10 to 22 of age for more than 1.5 kg as compared to non vaccinated animals. The term “during fattening” as used herein means, but is not limited to, weeks 1 to 36 of age, preferably to weeks 10 to 28 of age of those animals.
The term “in animals sub-clinically infected with PCV2” as used herein means the individual animal that becomes sub-clinically infected with PCV2, but also refers to a group of animals wherein most of the animals of that group become sub-clinically infected with PCV2. Thus, the term “in animals sub-clinically infected with PCV2” has to be read as i) “in animals sub-clinically infected with PCV2” and ii) as “in animals of a herd, wherein said herd is sub-clinically infected with PCV2”.
According to a further aspect, the present invention also provides a method for reduction of the number of animals with viral load comprising between 10 4 to 10 6 genomic copies per ml serum in a group of animals (herd) sub-clinically infected with PCV2, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to an animal in need of such administration. Preferably, the number of animals with 10 4 to 10 6 genomic copies per ml serum could be reduced due to vaccination with PCV2 antigen to less than 30%, preferably less than 20%, even more preferably to less than 10%, and most preferably to less than 5%, whereas in the non-vaccinated control group of the sub-clinically infected animals (with viral load comprised between 10 4 to 10 6 genomic copies per ml serum) more than 40% developed PCV2 titers with 10 4 to 10 6 genomic copies per ml serum.
According to a further aspect, the present invention also provides a method for the reduction of the number of animals with a clinically relevant viral load (above 10 6 genomic copies per ml serum) in a group of animals (herd) sub-clinically infected with PCV2, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising an PCV2 antigen to an animal in need of such administration. Preferably, the number of animals with a viral load above 10 6 genomic copies per ml serum could be reduced due to vaccination with PCV2 antigen to less than 10%, preferably less than 5%, even more preferably to less than 4%, even more preferably to less than 3%, even more preferably to less than 2%, and most preferably to less than 0.5%.
According to a further aspect, the present invention also provides a method for the reduction of nasal virus shedding, or reduction of the duration of viremia in animals sub-clinically infected with PCV2, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising an PCV2 antigen to an animal in need of such administration. As described above, vaccination/treatment of animals sub-clinically infected with PCV2 resulted in shortening of viremic phase as compared to non-vaccinated control animals. The average shortening time of the duration of the viremia was 17 days as compared to non-vaccinated control animals of the same species. Thus, according to a further aspect, the present invention also provides a method for reduction of duration of viremia in animals sub-clinically infected with PCV2, comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to an animal in need of such administration, wherein the treatment or prophylaxis results in shortening of the viremia phase of 5 or more days, preferably 6 or more days, even more preferably of 7 or more days, even more preferably of 8 or more days, even more preferably of 9, even more preferably of 10, even more preferably of 12, even more preferably of 14, and most preferably of more than 16 days as compared to animals of a non-treated control group of the same species.
The term “antigen” as used herein refers to an amino acid sequence which elicits an immune response in a host. An antigen, as used herein, includes the full-length sequence of any PCV2 proteins, analogs thereof, or immunogenic fragments thereof. The term “immunogenic fragment” refers to a fragment of a protein which includes one or more epitopes and thus elicits the immune response in a host. Such fragments can be identified using any number of epitope mapping techniques well known in the art. See, e.g., Epitope Mapping Protocols in Methods in Molecular Biology, Vol. 66 (Glenn E. Morris, Ed., 1996) Humana Press, Totowa, N.J. For example, linear epitopes may be determined by e.g., concurrently synthesizing large numbers of peptides on solid supports, the peptides corresponding to portions of the protein molecule, and reacting the peptides with antibodies while the peptides are still attached to the supports. Such techniques are known in the art and described in, e.g., U.S. Pat. No. 4,708,871; Geysen et al. (1984) Proc. Natl. Acad. Sci. USA 81:3998-4002; Geysen et al. (1986) Molec. Immunol. 23:709-715. Similarly, conformational epitopes are readily identified by determining spatial conformation of amino acids such as by, e.g., x-ray crystallography and 2-dimensional nuclear magnetic resonance. See, e.g., Epitope Mapping Protocols, supra.
Synthetic antigens are also included within the definition, for example, polyepitopes, flanking epitopes, and other recombinant or synthetically derived antigens. See, e.g., Bergmann et al. (1993) Eur. J. Immunol. 23:2777-2781; Bergmann et al. (1996), J. Immunol. 157:3242-3249; Suhrbier, A. (1997), Immunol. and Cell Biol. 75:402-408; Gardner et al., (1998) 12th World AIDS Conference, Geneva, Switzerland, Jun. 28-Jul. 3, 1998.
An “immune response” means, but is not limited to, the development in a host of a cellular and/or antibody-mediated immune response to an antigen, an immunogenic composition, or a vaccine of interest. Usually, an “immune response” includes but is not limited to one or more of the following effects: the production or activation of antibodies, B cells, helper T cells, suppressor T cells, and/or cytotoxic T cells, directed specifically to an antigen or antigens included in the composition or vaccine of interest. Preferably, the host will display either a therapeutic or a protective immunological (memory) response such that resistance to new infection will be enhanced and/or the clinical severity of the disease reduced. Such protection will be demonstrated by either a reduction in number or severity of, or lack of one or more of the symptoms associated with PCV2 infections, in delay of onset of viremia, in a reduced viral persistence, in a reduction of the overall viral load, and/or a reduction of viral excretion.
The terms “immunogenic composition” or “vaccine” (both terms are used synonymously) as used herein refers to any pharmaceutical composition containing a PCV2 antigen, which composition can be used to prevent or treat a PCV2 infection-associated disease or condition in a subject. A preferred immunogenic composition can induce, stimulate or enhance the immune response against PCV2. The term thus encompasses both subunit immunogenic compositions, as described below, as well as compositions containing whole killed, or attenuated, and/or inactivated PCV2.
Thus according to another aspect, the present invention provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, a method for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, a method for the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, a method for the reduction of the number of animals with viral load above 10 6 genome per ml serum within a sub-clinically infected herd, a method for the reduction of nasal virus shedding, a method for the reduction of duration of viremia in animals sub-clinically infected with PCV2, a method for the reduction of the morbidity rate within a sub-clinically infected herd, and a method for the reduction of the mortality rate within a sub-clinically infected herd, all comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising an PCV2 antigen to an animal in need of such treatment, wherein the immunogenic composition is a subunit immunogenic composition, and/or a composition containing whole killed, or attenuated, and/or inactivated PCV2.
The term “subunit immunogenic composition” as used herein refers to a composition containing at least one immunogenic polypeptide or antigen, but not all antigens, derived from or homologous to an antigen from PCV2. Such a composition is substantially free of intact PCV2. Thus, a “subunit immunogenic composition” is prepared from at least partially purified or fractionated (preferably substantially purified) immunogenic polypeptides from PCV2, or recombinant analogs thereof. A subunit immunogenic composition can comprise the subunit antigen or antigens of interest substantially free of other antigens or polypeptides from PCV2, or in fractionated form. A preferred immunogenic subunit composition comprises the PCV2 ORF-2 protein as described below. Most preferred are immunogenic subunit compositions, which comprise any of the PCV2 antigens provided in WO06/072065, which are all incorporated herein by reference in their entirety.
According to a further aspect, the immunogenic composition as used herein most preferably comprises the polypeptide, or a fragment thereof, expressed by ORF-2 of PCV2. PCV2 ORF-2 DNA and protein, used herein for the preparation of the compositions and within the processes provided herein, is a highly conserved domain within PCV2 isolates and thereby, any PCV2 ORF-2 would be effective as the source of the PCV2 ORF-2 DNA and/or polypeptide as used herein. A preferred PCV2 ORF-2 protein is that of SEQ ID NO: 11 of WO06/072065. A further preferred PCV ORF-2 polypeptide is provided as SEQ ID NO: 5 of WO06/072065. However, it is understood by those of skill in the art that this sequence could vary by as much as 6-10% in sequence homology and still retain the antigenic characteristics that render it useful in immunogenic compositions. The antigenic characteristics of an immunological composition can be, for example, estimated by the challenge experiment as provided by Example 4 of WO06/072065. Moreover, the antigenic characteristic of a modified antigen is still retained, when the modified antigen confers at least 70%, preferably 80%, more preferably 90% of the protective immunity as compared to the PCV2 ORF-2 protein, encoded by the polynucleotide sequence of SEQ ID NO:3 or SEQ ID NO:4 as provided in WO06/072065.
Thus according to another aspect, the present invention provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, a method for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, a method for the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, a method for the reduction of the number of animals with viral load above 10 6 genome per ml serum within a sub-clinically infected herd, a method for the reduction of nasal virus shedding, a method for the reduction of duration of viremia in animals sub-clinically infected with PCV2, a method for the reduction of the morbidity rate within a sub-clinically infected herd, and a method for the reduction of the mortality rate within a sub-clinically infected herd, all comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to an animal in need of such administration, wherein the PCV2 antigen is an antigen such as PCV2 ORF-2 protein that has at least 70%, preferably 80%, even more preferably 90% of the protective immunity as compared to the PCV2 ORF-2 protein, encoded by the polynucleotide sequence of SEQ ID NO:3 or SEQ ID NO:4 as provided in WO06/072065. Preferably said PCV2 ORF-2 has the sequence of SEQ ID NO: 11 or SEQ ID NO: 5 of WO06/072065.
In some forms, immunogenic portions of PCV2 ORF-2 protein are used as the antigenic component in the immunogenic composition, comprising PCV2 antigen. The term “immunogenic portion” as used herein refers to truncated and/or substituted forms, or fragments of PCV2 ORF-2 protein and/or polynucleotide, respectively. Preferably, such truncated and/or substituted forms or fragments will comprise at least 6 contiguous amino acids from the full-length ORF-2 polypeptide. More preferably, the truncated or substituted forms or fragments will have at least 5, preferably at least 8, more preferably at least 10, more preferably at least 15, and still more preferably at least 19 contiguous amino acids from the full-length PCV ORF-2 polypeptide. Two preferred sequences in this respect are provided as SEQ ID NO: 9 and SEQ ID NO: 10 of WO06/072065. It is further understood that such sequences may be a part of larger fragments or truncated forms.
As mentioned above, a further preferred PCV2 ORF-2 polypeptide is any one encoded by the nucleotide sequences of SEQ ID NO: 3 or SEQ ID NO: 4. However, it is understood by those of skill in the art that this sequence could vary by as much as 6-20% in sequence homology and still retain the antigenic characteristics that render it useful in immunogenic compositions. In some forms, a truncated or substituted form or fragment of this PVC2 ORF -2 polypeptide is used as the antigenic component in the composition. Preferably, such truncated or substituted forms or fragments will comprise at least 18 contiguous nucleotides from the full-length PCV2 ORF-2 nucleotide sequence, e.g. of SEQ ID NO: 3 or SEQ ID NO: 4. More preferably, the truncated or substituted forms or fragments, will have at least 30, more preferably at least 45, and still more preferably at least 57 contiguous nucleotides of the full-length PCV2 ORF-2 nucleotide sequence, e.g. SEQ ID NO: 3 or SEQ ID NO: 4.
“Sequence Identity” as it is known in the art refers to a relationship between two or more polypeptide sequences or two or more polynucleotide sequences, namely a reference sequence and a given sequence to be compared with the reference sequence. Sequence identity is determined by comparing the given sequence to the reference sequence after the sequences have been optimally aligned to produce the highest degree of sequence similarity, as determined by the match between strings of such sequences. Upon such alignment, sequence identity is ascertained on a position-by-position basis, e.g., the sequences are “identical” at a particular position if at that position, the nucleotides or amino acid residues are identical. The total number of such position identities is then divided by the total number of nucleotides or residues in the reference sequence to give % sequence identity. Sequence identity can be readily calculated by known methods, including but not limited to, those described in Computational Molecular Biology, Lesk, A. N., ed., Oxford University Press, New York (1988), Biocomputing: Informatics and Genome Projects, Smith, D. W., ed., Academic Press, New York (1993); Computer Analysis of Sequence Data, Part 1, Griffin, A.M., and Griffin, H. G., eds., Humana Press, New Jersey (1994); Sequence Analysis in Molecular Biology, von Heinge, G., Academic Press (1987); Sequence Analysis Primer, Gribskov, M. and Devereux, J., eds., M. Stockton Press, New York (1991); and Carillo, H., and Lipman, D., SIAM J. Applied Math., 48: 1073 (1988), the teachings of which are incorporated herein by reference. Preferred methods to determine the sequence identity are designed to give the largest match between the sequences tested. Methods to determine sequence identity are codified in publicly available computer programs which determine sequence identity between given sequences. Examples of such programs include, but are not limited to, the GCG program package (Devereux, J., et al., Nucleic Acids Research, 12(1):387 (1984)), BLASTP, BLASTN and FASTA (Altschul, S. F. et al., J. Molec. Biol., 215:403-410 (1990). The BLASTX program is publicly available from NCBI and other sources (BLAST Manual, Altschul, S. et al., NCVI NLM NIH Bethesda, Md. 20894, Altschul, S. F. et al., J. Molec. Biol., 215:403-410 (1990)), the teachings of which are incorporated herein by reference. These programs optimally align sequences using default gap weights in order to produce the highest level of sequence identity between the given and reference sequences. As an illustration, by a polynucleotide having a nucleotide sequence having at least, for example, 85%, preferably 90%, even more preferably 95% “sequence identity” to a reference nucleotide sequence, it is intended that the nucleotide sequence of the given polynucleotide is identical to the reference sequence except that the given polynucleotide sequence may include up to 15, preferably up to 10, even more preferably up to 5 point mutations per each 100 nucleotides of the reference nucleotide sequence. In other words, in a polynucleotide having a nucleotide sequence having at least 85%, preferably 90%, even more preferably 95% identity relative to the reference nucleotide sequence, up to 15%, preferably 10%, even more preferably 5% of the nucleotides in the reference sequence may be deleted or substituted with another nucleotide, or a number of nucleotides up to 15%, preferably 10%, even more preferably 5% of the total nucleotides in the reference sequence may be inserted into the reference sequence. These mutations of the reference sequence may occur at the 5′ or 3′ terminal positions of the reference nucleotide sequence or anywhere between those terminal positions, interspersed either individually among nucleotides in the reference sequence or in one or more contiguous groups within the reference sequence. Analogously, by a polypeptide having a given amino acid sequence having at least, for example, 85%, preferably 90%, even more preferably 95% sequence identity to a reference amino acid sequence, it is intended that the given amino acid sequence of the polypeptide is identical to the reference sequence except that the given polypeptide sequence may include up to 15, preferably up to 10, even more preferably up to 5 amino acid alterations per each 100 amino acids of the reference amino acid sequence. In other words, to obtain a given polypeptide sequence having at least 85%, preferably 90%, even more preferably 95% sequence identity with a reference amino acid sequence, up to 15%, preferably up to 10%, even more preferably up to 5% of the amino acid residues in the reference sequence may be deleted or substituted with another amino acid, or a number of amino acids up to 15%, preferably up to 10%, even more preferably up to 5% of the total number of amino acid residues in the reference sequence may be inserted into the reference sequence. These alterations of the reference sequence may occur at the amino or the carboxy terminal positions of the reference amino acid sequence or anywhere between those terminal positions, interspersed either individually among residues in the reference sequence or in the one or more contiguous groups within the reference sequence. Preferably, residue positions which are not identical differ by conservative amino acid substitutions. However, conservative substitutions are not included as a match when determining sequence identity.
“Sequence homology”, as used herein, refers to a method of determining the relatedness of two sequences. To determine sequence homology, two or more sequences are optimally aligned, and gaps are introduced if necessary. However, in contrast to “sequence identity”, conservative amino acid substitutions are counted as a match when determining sequence homology. In other words, to obtain a polypeptide or polynucleotide having 95% sequence homology with a reference sequence, 85%, preferably 90%, even more preferably 95% of the amino acid residues or nucleotides in the reference sequence must match or comprise a conservative substitution with another amino acid or nucleotide, or a number of amino acids or nucleotides up to 15%, preferably up to 10%, even more preferably up to 5% of the total amino acid residues or nucleotides, not including conservative substitutions, in the reference sequence may be inserted into the reference sequence. Preferably the homolog sequence comprises at least a stretch of 50, even more preferably at least 100, even more preferably at least 250, and even more preferably at least 500 nucleotides.
A “conservative substitution” refers to the substitution of an amino acid residue or nucleotide with another amino acid residue or nucleotide having similar characteristics or properties including size, hydrophobicity, etc., such that the overall functionality does not change significantly.
“Isolated” means altered “by the hand of man” from its natural state, i.e., if it occurs in nature, it has been changed or removed from its original environment, or both. For example, a polynucleotide or polypeptide naturally present in a living organism is not “isolated,” but the same polynucleotide or polypeptide separated from the coexisting materials of its natural state is “isolated”, as the term is employed herein.
Thus according to another aspect, the present invention provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, a method for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, a method for the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, a method for the reduction of the number of animals with viral load above 10 6 genome per ml serum within a sub-clinically infected herd, a method for the reduction of nasal virus shedding, a method for the reduction of duration of viremia in animals sub-clinically infected with PCV2, a method for the reduction of the morbidity rate within a sub-clinically infected herd, and a method for the reduction of the mortality rate within a sub-clinically infected herd, all comprising the step of administering a therapeutically effective amount of PCV2 ORF-2 protein to an animal in need of such administration, wherein said PCV2 ORF-2 protein is any one of those described above. Preferably, said PCV2 ORF-2 protein is
i) a polypeptide comprising the sequence of SEQ ID NO: 5, SEQ ID NO: 6, SEQ ID NO: 9, SEQ ID NO: 10 or SEQ ID NO: 11 of WO06/07065; ii) any polypeptide that is at least 80% homologous to the polypeptide of i), iii) any immunogenic portion of the polypeptides of i) and/or ii) iv) the immunogenic portion of iii), comprising at least 5, preferably at least 8, even more preferably at least 10 contiguous amino acids included in the sequences of SEQ ID NO: 5, SEQ ID NO: 6, SEQ ID NO: 9, SEQ ID NO: 10 or SEQ ID NO: 11 of WO06/072065, v) a polypeptide that is encoded by a DNA comprising the sequence of SEQ ID NO: 3 or SEQ ID NO: 4 of WO06/072065. vi) any polypeptide that is encoded by a polynucleotide that is at least 80% homologous to the polynucleotide of v), vii) any immunogenic portion of the polypeptides encoded by the polynucleotide of v) and/or vi) viii) the immunogenic portion of vii), wherein the polynucleotide coding for said immunogenic portion comprises at least 30 contiguous nucleotides included in the sequences of SEQ ID NO: 3, or SEQ ID NO: 4 of WO06/072065.
Preferably any of those immunogenic portions have the immunogenic characteristics of PCV2 ORF-2 protein that is encoded by the sequence of SEQ ID NO: 3 or SEQ ID NO: 4 of WO06/07065.
According to a further aspect, PCV2 ORF-2 protein is provided in the immunogenic composition at an antigen inclusion level effective for the treatment of animals sub-clinically infected with PCV2. Preferably, the PCV2 ORF-2 protein inclusion level is at least 0.2 μg antigen/ml of the final immunogenic composition (μg/ml), more preferably from about 0.2 to about 400 μg/ml, still more preferably from about 0.3 to about 200 μg/ml, even more preferably from about 0.35 to about 100 μg/ml, still more preferably from about 0.4 to about 50 μg/ml, still more preferably from about 0.45 to about 30 μg/ml, still more preferably from about 0.6 to about 15 μg/ml, even more preferably from about 0.75 to about 8 μg/ml, even more preferably from about 1.0 to about 6 μg/ml, still more preferably from about 1.3 to about 3.0 μg/ml, even more preferably from about 1.4 to about 2.5 μg/ml, even more preferably from about 1.5 to about 2.0 μg/ml, and most preferably about 1.6 μg/ml.
According to a further aspect, the PCV ORF-2 antigen inclusion level is at least 0.2 μg/PCV2 ORF-2 protein as described above per dose of the final antigenic composition (μg/dose), more preferably from about 0.2 to about 400 μg/dose, still more preferably from about 0.3 to about 200 μg/dose, even more preferably from about 0.35 to about 100 μg/dose, still more preferably from about 0.4 to about 50 μg/dose, still more preferably from about 0.45 to about 30 μg/dose, still more preferably from about 0.6 to about 15 μg/dose, even more preferably from about 0.75 to about 8 μg/dose, even more preferably from about 1.0 to about 6 μg/dose, still more preferably from about 1.3 to about 3.0 μg/dose, even more preferably from about 1.4 to about 2.5 μg/dose, even more preferably from about 1.5 to about 2.0 μg/dose, and most preferably about 1.6 μg/dose.
The PCV2 ORF-2 polypeptide used in the immunogenic composition in accordance with the present invention can be derived in any fashion including isolation and purification of PCV2 ORF2, standard protein synthesis, and recombinant methodology. Preferred methods for obtaining PCV2 ORF-2 polypeptide are provided in WO06/072065, the teachings and content of which are hereby incorporated by reference in its entirety. Briefly, susceptible cells are infected with a recombinant viral vector containing PCV2 ORF-2 DNA coding sequences, PCV2 ORF-2 polypeptide is expressed by the recombinant virus, and the expressed PCV2 ORF-2 polypeptide is recovered from the supernatant by filtration and inactivated by any conventional method, preferably using binary ethylenimine, which is then neutralized to stop the inactivation process.
The immunogenic composition as used herein also refers to a composition that comprises i) any of the PCV2 ORF-2 proteins described above, preferably in concentrations described above, and ii) at least a portion of the viral vector expressing said PCV2 ORF-2 protein, preferably of a recombinant baculovirus. Moreover, the immunogenic composition can comprise i) any of the PCV2 ORF-2 proteins described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF-2 protein, preferably of a recombinant baculovirus, and iii) a portion of the cell culture supernatant.
Thus according to another aspect, the present invention provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, a method for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, a method for the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, a method for the reduction of the number of animals with viral load above 10 6 genome per ml serum within a sub-clinically infected herd, a method for the reduction of nasal virus shedding, a method for the reduction of duration of viremia in animals sub-clinically infected with PCV2, a method for the reduction of the morbidity rate within a sub-clinically infected herd, and a method for the reduction of the mortality rate within a sub-clinically infected herd, all comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising an PCV2 antigen to an animal in need of such treatment, wherein the PCV2 antigen is recombinant PCV2 ORF-2, preferably a baculovirus expressed PCV2 ORF-2, most preferably those recombinant or baculovirus expressed PCV2 ORF-2 having the sequence as described above.
The immunogenic composition as used herein also refers to a composition that comprises i) any of the PCV2 ORF-2 proteins described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF-2 protein, preferably of a recombinant baculovirus, and iii) a portion of the cell culture; wherein about 90% of the components have a size smaller than 1 μm.
The immunogenic composition as used herein also refers to a composition that comprises i) any of the PCV2 ORF-2 proteins described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF-2 protein, iii) a portion of the cell culture, iv) and an inactivating agent to inactivate the recombinant viral vector, preferably BEI, wherein about 90% of the components i) to iii) have a size smaller than 1 μm. Preferably, BEI is present in concentrations effective to inactivate the baculovirus, preferably in an amount of 2 to about 8 mM BEI, and more preferably of about 5 mM BEI.
The immunogenic composition as used herein also refers to a composition that comprises i) any of the PCV2 ORF-2 proteins described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF-2 protein, iii) a portion of the cell culture, iv) an inactivating agent to inactivate the recombinant viral vector, preferably BEI, and v) a neutralization agent to stop the inactivation mediated by the inactivating agent, wherein about 90% of the components i) to iii) have a size smaller than 1 μm. Preferably, if the inactivating agent is BEI, said composition comprises sodium thiosulfate in equivalent amounts to BEI.
The polypeptide is incorporated into a composition that can be administered to an animal susceptible to PCV2 infection. In preferred forms, the composition may also include additional components known to those of skill in the art (see also Remington's Pharmaceutical Sciences. (1990). 18th ed. Mack Publ., Easton). Additionally, the composition may include one or more veterinary-acceptable carriers. As used herein, “a veterinary-acceptable carrier” includes any and all solvents, dispersion media, coatings, adjuvants, stabilizing agents, diluents, preservatives, antibacterial and antifungal agents, isotonic agents, adsorption delaying agents, and the like. In a preferred embodiment, the immunogenic composition comprises PCV2 ORF-2 protein as provided herewith, preferably in concentrations described above, which is mixed with an adjuvant, preferably Carbopol, and physiological saline.
Those of skill in the art will understand that the composition used herein may incorporate known injectable, physiologically acceptable sterile solutions. For preparing a ready-to-use solution for parenteral injection or infusion, aqueous isotonic solutions, such as e.g. saline or corresponding plasma protein solutions, are readily available. In addition, the immunogenic and vaccine compositions of the present invention can include diluents, isotonic agents, stabilizers, or adjuvants. Diluents can include water, saline, dextrose, ethanol, glycerol, and the like. Isotonic agents can include sodium chloride, dextrose, mannitol, sorbitol, and lactose, among others. Stabilizers include albumin and alkali salts of ethylendiamintetracetic acid, among others.
“Adjuvants” as used herein, can include aluminium hydroxide and aluminium phosphate, saponins e.g., Quil A, QS-21 (Cambridge Biotech Inc., Cambridge Mass.), GPI-0100 (Galenica Pharmaceuticals, Inc., Birmingham, Ala.), water-in-oil emulsion, oil-in-water emulsion, water-in-oil-in-water emulsion. The emulsion can be based in particular on light liquid paraffin oil (European Pharmacopea type); isoprenoid oil such as squalane or squalene oil resulting from the oligomerization of alkenes, in particular of isobutene or decene; esters of acids or of alcohols containing a linear alkyl group, more particularly plant oils, ethyl oleate, propylene glycol di-(caprylate/caprate), glyceryl tri-(caprylate/caprate) or propylene glycol dioleate; esters of branched fatty acids or alcohols, in particular isostearic acid esters. The oil is used in combination with emulsifiers to form the emulsion. The emulsifiers are preferably nonionic surfactants, in particular esters of sorbitan, of mannide (e.g. anhydromannitol oleate), of glycol, of polyglycerol, of propylene glycol and of oleic, isostearic, ricinoleic or hydroxystearic acid, which are optionally ethoxylated, and polyoxypropylene-polyoxyethylene copolymer blocks, in particular the Pluronic products, especially L121. See Hunter et al., The Theory and Practical Application of Adjuvants (Ed. Stewart-Tull, D. E. S.). JohnWiley and Sons, NY, pp 51-94 (1995) and Todd et al., Vaccine 15:564-570 (1997).
For example, it is possible to use the SPT emulsion described on page 147 of “Vaccine Design, The Subunit and Adjuvant Approach” edited by M. Powell and M. Newman, Plenum Press, 1995, and the emulsion MF59 described on page 183 of this same book.
A further instance of an adjuvant is a compound chosen from the polymers of acrylic or methacrylic acid and the copolymers of maleic anhydride and alkenyl derivative. Advantageous adjuvant compounds are the polymers of acrylic or methacrylic acid which are cross-linked, especially with polyalkenyl ethers of sugars or polyalcohols. These compounds are known by the term carbomer (Phameuropa Vol. 8, No. 2, June 1996). Persons skilled in the art can also refer to U.S. Pat. No. 2,909,462 which describes such acrylic polymers cross-linked with a polyhydroxylated compound having at least 3 hydroxyl groups, preferably not more than 8, the hydrogen atoms of at least three hydroxyls being replaced by unsaturated aliphatic radicals having at least 2 carbon atoms. The preferred radicals are those containing from 2 to 4 carbon atoms. e.g. vinyls, allyls and other ethylenically unsaturated groups. The unsaturated radicals may themselves contain other substituents, such as methyl. The products sold under the name Carbopol (BF Goodrich, Ohio, USA) are particularly appropriate. They are cross-linked with an allyl sucrose or with allyl pentaerythritol. Among them, there may be mentioned Carbopol 974P, 934P and 971P. Most preferred is the use of Carbopol, in particular the use of Carbopol 971P, preferably in amounts of about 500 μg to about 5 mg per dose, even more preferred in an amount of about 750 μg to about 2.5 mg per dose and most preferred in an amount of about 1 mg per dose.
Further suitable adjuvants include, but are not limited to, the RIBI adjuvant system (Ribi Inc.), Block co-polymer (CytPx, Atlanta Ga.), SAF-M (Chiron, Emeryville Calif.), monophosphoryl lipid A, Avridine lipid-amine adjuvant, heat-labile enterotoxin from E. coli (recombinant or otherwise), cholera toxin, IMS 1314, or muramyl dipeptide among many others.
Preferably, the adjuvant is added in an amount of about 100 μg to about 10 mg per dose. Even more preferably, the adjuvant is added in an amount of about 100 μg to about 10 mg per dose. Even more preferably, the adjuvant is added in an amount of about 500 μg to about 5 mg per dose. Even more preferably, the adjuvant is added in an amount of about 750 μg to about 2.5 mg per dose. Most preferably, the adjuvant is added in an amount of about 1 mg per dose.
Additionally, the composition can include one or more pharmaceutical-acceptable carriers. As used herein, “a pharmaceutical-acceptable carrier” includes any and all solvents, dispersion media, coatings, stabilizing agents, diluents, preservatives, antibacterial and antifungal agents, isotonic agents, adsorption delaying agents, and the like. Most preferably, the composition provided herewith contains PCV2 ORF-2 protein recovered from the supernatant of in vitro cultured cells, wherein said cells were infected with a recombinant viral vector containing PCV2 ORF-2 DNA and expressing PCV2 ORF-2 protein, and wherein said cell culture was treated with about 2 to about 8 mM BEI, and more preferably with about 5 mM BEI to inactivate the viral vector, and an equivalent concentration of a neutralization agent, preferably sodium thiosulfate solution, to a final concentration of about 2 to about 8 mM, and more preferably of about 5 mM.
The present invention also relates to the use of an immunogenic composition for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, the reduction of the number of animals with viral load above 10 6 genome per ml serum within a sub-clinically infected herd, the reduction of nasal virus shedding, reduction of duration of viremia in animals sub-clinically infected with PCV2, a reduction of the morbidity rate within a sub-clinically infected herd, a method for the reduction of the mortality rate within a sub-clinically infected herd, wherein said immunogenic composition comprises i) any of the PCV2 ORF-2 proteins described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF-2 protein, iii) a portion of the cell culture, iv) an inactivating agent to inactivate the recombinant viral vector, preferably BEI, and v) a neutralization agent to stop the inactivation mediated by the inactivating agent, preferably sodium thiosulfate in equivalent amounts to BEI; and vi) a suitable adjuvant, preferably Carbopol 971 in amounts described above; wherein about 90% of the components i) to iii) have a size smaller than 1 μm.
According to a further aspect, this immunogenic composition further comprises a pharmaceutical acceptable salt, preferably a phosphate salt in physiologically acceptable concentrations. Preferably, the pH of said immunogenic composition is adjusted to a physiological pH, meaning between about 6.5 and 7.5.
The immunogenic composition as used herein also refers to a composition that comprises per one ml i) at least 1.6 μg of PCV2 ORF-2 protein described above, ii) at least a portion of baculovirus expressing said PCV2 ORF-2 protein iii) a portion of the cell culture, iv) about 2 to 8 mM BEI, v) sodium thiosulfate in equivalent amounts to BEI, vi) about 1 mg Carbopol 971, and vii) phosphate salt in a physiologically acceptable concentration; wherein about 90% of the components i) to iii) have a size smaller than 1 μm and the pH of said immunogenic composition is adjusted to about 6.5 to 7.5.
The immunogenic compositions can further include one or more other immuno-modulatory agents such as, e.g., interleukins, interferons, or other cytokines. The immunogenic compositions can also include Gentamicin and Merthiolate. While the amounts and concentrations of adjuvants and additives useful in the context of the present invention can readily be determined by the skilled artisan, the present invention contemplates compositions comprising from about 50 μg to about 2000 μg of adjuvant and preferably about 250 μg/ml dose of the vaccine composition. Thus, the immunogenic composition as used herein also refers to a composition that comprises from about 1 ug/ml to about 60 μg/ml of antibiotics, and more preferably less than about 30 μg/ml of antibiotics.
The immunogenic composition as used herein also refers to a composition that comprises i) any of the PCV2 ORF-2 proteins described above, preferably in concentrations described above, ii) at least a portion of the viral vector expressing said PCV2 ORF-2 protein, iii) a portion of the cell culture, iv) an inactivating agent to inactivate the recombinant viral vector, preferably BEI, v) a neutralization agent to stop the inactivation mediated by the inactivating agent, preferably sodium thiosulfate in equivalent amounts to BEI, vi) a suitable adjuvant, preferably Carbopol 971 in amounts described above, vii) a pharmaceutical acceptable concentration of a saline buffer, preferably of a phosphate salt, and viii) an anti-microbiological active agent; wherein about 90% of the components i) to iii) have a size smaller than 1 μm.
The immunogenic composition as used herein also refers to Ingelvac® CircoFLEX™, (Boehringer Ingelheim Vetmedica Inc, St Joseph, Mo., USA), CircoVac® (Merial SAS, Lyon, France), CircoVent (Intervet Inc., Millsboro, Del., USA), or Suvaxyn PCV-2 One Dose® (Fort Dodge Animal Health, Kansas City, Kans., USA). Thus according to another aspect, the present invention provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, a method for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, a method for the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, a method for the reduction of the number of animals with viral load above 10 6 genomic copies per ml serum within a sub-clinically infected herd, a method for the reduction of nasal virus shedding, a method for the reduction of the duration of viremia in animals sub-clinically infected with PCV2, a method for the reduction of the morbidity rate within a sub-clinically infected herd, and a method for the reduction of the mortality rate within a sub-clinically infected herd, comprising the step of administering an effective amount of PCV2 antigen to an animal in need of such administration, wherein said immunogenic composition comprising a PCV2 antigen is Ingelvac® CircoFLEX™, CircoVac®, CircoVent and/or Suvaxyn PCV-2 One Dose®, and preferably it is Ingelvac® CircoFLEX™.
The term “an effective amount of PCV2 antigen” as used herein means, but is not limited to, an amount of PCV2 antigen that elicits or is able to elicit an immune response in an animal, to which said effective amount of PCV2 antigen is administered.
The amount that is effective depends on the ingredients of the vaccine and the schedule of administration. Typically, when an inactivated virus or a modified live virus preparation is used in the vaccine, an amount of the vaccine containing about 10 2.0 to about 10 9.0 TCID 50 per dose, preferably about 10 3.0 to about 10 8.0 TCID 50 per dose, and more preferably about 10 4.0 to about 10 8.0 TCID 50 per dose is used. In particular, when modified live PCV2 is used in the vaccines, the recommended dose to be administered to the susceptible animal is preferably about 10 3.0 TCID 50 (tissue culture infective dose 50% end point)/dose to about 10 6.0 TCID 50 /dose and more preferably about 10 4.0 TCID 50 /dose to about 10 5.0 TCID 50 /dose. In general, the quantity of antigen will be between 0.2 and 5000 micrograms, and between 10 2.0 and 10 9.0 TCID 50 , preferably between 10 3.0 and 10 6.0 TCID 50 , and more preferably between 10 4.0 and 10 5.0 TCID 50 , when purified antigen is used.
Sub-unit vaccines are normally administered with an antigen inclusion level of at least 0.2 μg antigen per dose, preferably with about 0.2 to about 400 μg/dose, still more preferably with about 0.3 to about 200 μg/dose, even more preferably with about 0.35 to about 100 μg/dose, still more preferably with about 0.4 to about 50 μg/dose, still more preferably with about 0.45 to about 30 μg/dose, still more preferably with about 0.6 to about 16 μg/dose, even more preferably with about 0.75 to about 8 μg/dose, even more preferably with about 1.0 to about 6 μg/dose, and still more preferably with about 1.3 to about 3.0 μg/dose.
Maternally derived immunity has been shown to confer a certain degree of protection against PCV2 infection and clinical diseases associated with PCV2 infections. This protection has been shown to be titer dependent: higher titers are generally protective whereas lower titers are not (McKeown et al., 2005; Clin. Diagn. Lab. Immunol.; 12: 1347-1351). The mean antibody half-life in weanlings has been estimated to be 19.0 days and the window for PCV2-passive antibody decay within a population is relatively wide (Opriessnig et al. 2004, J. Swine Health Prod. 12:186-191). The presence of maternally derived antibody not only may confer a certain degree of protection against viral infections, which however is not predictable, but is also known to impair the efficacy of immunization. It has been surprisingly found that the presence of anti-PCV2 antibodies, in particular of anti-PCV2 antibody titers of up to 1:1000, does not affect the efficacy of the PCV2 treatment.
Thus according to another aspect, the present invention provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, a method for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, a method for the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, a method for reduction of the number of animals with viral load above 10 6 genomic copies per ml serum within a sub-clinically infected herd, a method for the reduction of nasal virus shedding, a method for the reduction of the duration of viremia in animals sub-clinically infected with PCV2, a method for the reduction of the morbidity rate within a sub-clinically infected herd, and a method for the reduction of the mortality rate within a sub-clinically infected herd all comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to an animal in need of such administration, wherein the animals at the time of vaccination have anti-PCV2 antibodies, preferably wherein said animals have at the time of vaccination a detectable anti-PCV2 antibody titer of up to 1:100, preferably of more than 1:100, even more preferably of more than 1:250, even more preferably of more than 1:500, even more preferably of 1:640; even more preferably of more than 1:750, and most preferably of more than 1:1000. Preferably, the anti-PCV2 antibody titer is detectable and quantifiable in a specific anti-PCV2 immune assay, preferably in the assay as described in Example 2.
Methods for the detection and quantification of anti-PCV2 antibodies are well known in the art. For example, the detection and quantification of PCV2 antibodies can be performed by indirect immunofluorescence as described in Magar et al., 2000, Can. J. Vet Res.; 64: 184-186 or Magar et al., 2000, J. Comp. Pathol.; 123: 258-269. Further assays for quantification of anti-PCV2 antibodies are described in Opriessnig et al., 2006, 37 th Annual Meeting of the American Association of Swine Veterinarians. Moreover, Example 2 also describes an indirect immunofluorescence assay, which can be used by a person skilled in the art. In cases of controversial results and in any question of doubt, anti-PCV2 titers as mentioned herein refer to those which are/can be estimated by the assay as described in Example 2.
Thus according to another aspect, the present invention provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection, a method for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, a method for the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, a method for the reduction of the number of animals with viral load above 10 6 genomic copies per ml serum within a sub-clinically infected herd, a method for the reduction of nasal virus shedding, a method for the reduction of duration of viremia in animals sub-clinically infected with PCV2, a method for the reduction of the morbidity rate within a sub-clinically infected herd, and a method for the reduction of the mortality rate within a sub-clinically infected herd, all comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to a young animal in need of such administration.
The term “young animal” as used herein refers to an animal of 1 to 22 days of age. Preferably, by the term young animal, an animal of 1 to 20 days of age is meant. More preferably, the term young animal refers to an animal of 1 to 15 days of age, even more preferably of 1 day of age to 14 days of age, even more preferably of 1 to 12 days of age, even more preferably of 1 to 10 days of age, even more preferably of 1 to 8 days of age, even more preferably of 1 to 7 days of age, even more preferably of 1 to 6 days of age, even more preferably of 1 to 5 days of age, even more preferably of 1 to 4 days of age, even more preferably of 1 to 3 days of age, even more preferably of 1 or 2 day(s) of age, and most preferably to an animal of 1 day of age.
Due to the ubiquity of PCV2 in the field, most of the young piglets are seropositive in respect to PCV2. Thus according to a further aspect, said young animals, at the day of vaccination/treatment, have a detectable anti-PCV2 antibody titer of up to 1:100, preferably of more than 1:100, even more preferably of more than 1:250, even more preferably of more than 1:500, even more preferably of 1:640, even more preferably of more than 1:750, most preferably of more than 1:1000 at the day of vaccination/treatment.
The composition according to the invention may be applied intradermally, intratracheally, or intravaginally. The composition preferably may be applied intramuscularly or intranasally, most preferably intramuscularly. In an animal body, it can prove advantageous to apply the pharmaceutical compositions as described above via an intravenous or by direct injection into target tissues. For systemic application, the intravenous, intravascular, intramuscular, intranasal, intraarterial, intraperitoneal, oral, or intrathecal routes are preferred. A more local application can be effected subcutaneously, intradermally, intracutaneously, intracardially, intralobally, intramedullarly, intrapulmonarily or directly in or near the tissue to be treated (connective-, bone-, muscle-, nerve-, epithelial tissue). Depending on the desired duration and effectiveness of the treatment, the compositions according to the invention may be administered once or several times, also intermittently, for instance on a daily basis for several days, weeks or months and in different dosages.
Preferably, at least one dose of the immunogenic composition as described above is intramuscularly administered to the subject in need thereof. According to a further aspect, the PCV2 antigen or the immunogenic composition comprising any such PCV2 antigen as described herein is bottled in and administered at one (1) ml to five (5) ml per dose, preferably to 1 ml per dose. Thus, according to a further aspect, the present invention also provides a 1 ml to 5 ml, preferably a 1 ml immunogenic composition, comprising PCV-2 antigen as described herein, for the prophylaxis and treatment of sub-clinical PCV2 infection in an animal or group of animals (herds), for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, the reduction of the number of animals with viral load above 10 6 genomic copies per ml serum within a sub-clinically infected herd, the reduction of nasal virus shedding and reduction of duration of viremia in animals sub-clinically infected with PCV2, a method for the reduction of morbidity rate within a sub-clinically infected herd, and a method for the reduction of the mortality rate within a sub-clinically infected herd all comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to an animal in need of such administration. The present invention also relates to a method for the prophylaxis and treatment of sub-clinical PCV2 infection in an animal or group of animals (herds), a method for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, a method for the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, a method for the reduction of the number of animals with viral load above 10 6 genomic copies per ml serum within a sub-clinically infected herd, a method for the reduction of nasal virus shedding, a method for the reduction of the duration of viremia in animals sub-clinically infected with PCV2, a method for the reduction of the mobidity rate within a sub-clinically infected herd, and a method for the reduction of the mortality rate within a sub-clinically infected herd, all comprising the step of administering 1 to 5 ml, preferably 1 ml of a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising an PCV2 antigen to an animal in need of such administration.
According to a further aspect, at least one further administration of at least one dose of the immunogenic composition as described above is given to a subject in need thereof, wherein the second or any further administration is given at least 14 days beyond the initial or any former administrations. Preferably, the immunogenic composition is administered with an immune stimulant. Preferably, said immune stimulant is given at least twice. Preferably, at least 3 days, more preferably at least 5 days, even more preferably at least 7 days are in between the first and the second or any further administration of the immune stimulant. Preferably, the immune stimulant is given at least 10 days, preferably 15 days, even more preferably 20 days, and even more preferably at least 22 days beyond the initial administration of the immunogenic composition provided herein. A preferred immune stimulant is, for example, keyhole limpet hemocyanin (KLH), preferably emulsified with incomplete Freund's adjuvant (KLH/ICFA). However, it is herewith understood, that any other immune stimulant known to a person skilled in the art can also be used. The term “immune stimulant” as used herein, means any agent or composition that can trigger the immune response, preferably without initiating or increasing a specific immune response, for example the immune response against a specific pathogen. It is further instructed to administer the immune stimulant in a suitable dose.
The present invention also relates to the use of a PCV2 antigen or an immunogenic composition comprising PCV2 antigen for the preparation of a medicine for the prophylaxis and treatment of chronic PCV2 infection in an animal or group of animals (herds), for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, the reduction of the number of animals with viral load above 10 6 genomic copies per ml serum within a sub-clinically infected herd, the reduction of nasal virus shedding and the reduction of the duration of viremia in animals sub-clinically infected with PCV2, method for the reduction of the morbidity rate within a sub-clinically infected herd, and a method for the reduction of the mortality rate within a sub-clinically infected herd. Preferably, the PCV2 antigen is a recombinant antigen, preferably PCV2 ORF-2, even more preferably Ingelvac® CircoFLEX™.
The “animal” as used herein means swine, pig or piglet. Thus according to another aspect, the present invention provides a method for the prophylaxis and treatment of sub-clinical PCV2 infection in pigs, a method for increasing average weight gain in an animal or a group of animals (herd) sub-clinically infected with PCV2, a method for the reduction of the number of animals with viral load comprised between 10 4 to 10 6 genomic copies per ml serum, a method for the reduction of the number of animals with viral load above 10 6 genomic copies per ml serum within a sub-clinically infected herd, a method for the reduction of nasal virus shedding, a method for the reduction of the duration of viremia in animals sub-clinically infected with PCV2, a method for the reduction of the morbidity rate within a sub-clinically infected herd, and a method for the reduction of the mortality rate within a sub-clinically infected herd, all comprising the step of administering a therapeutically effective amount of PCV2 antigen or an immunogenic composition comprising a PCV2 antigen to pigs in need of such administration. Preferably, the PCV2 antigen or immunogenic composition comprising PCV2 antigen is anyone of those described supra, most preferably the PCV2 antigen is Ingelvac® CircoFLEX™.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The following examples set forth preferred materials and procedures in accordance with the present invention. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, the preferred methods, devices, and materials are now described. It is to be understood, however, that these examples are provided by way of illustration only, and nothing therein should be deemed a limitation upon the overall scope of the invention.
EXAMPLE 1
Preparation of PCV2 ORF-2 Antigen
Initial SF+ cell cultures from liquid nitrogen storage were grown in Excell 420 media (JRH Biosciences, Inc., Lenexa, Kans.) in suspension in sterile spinner flasks with constant agitation. The cultures were grown in 100 mL to 250 mL spinner flasks with 25 to 150 mL of Excell 420 serum-free media. When the cells had multiplied to a cell density of 1.0-8.0×10 6 cells/mL, they were split to new vessels with a planting density of 0.5-1.5×10 6 cells/mL. Subsequent expansion cultures were grown in spinner flasks up to 36 liters in size or in stainless steel bioreactors of up to 300 liters for a period of 2-7 days at 25-29° C.
After seeding, the flasks were incubated at 27° C. for four hours. Subsequently, each flask was seeded with a recombinant baculovirus containing the PCV2 ORF-2 gene (SEQ ID NO: 4). The recombinant baculovirus containing the PCV2 ORF-2 gene was generated as described in WO06/072065. After being seeded with the baculovirus, the flasks were then incubated at 27±2° C. for 7 days and were also agitated at 100 rpm during that time. The flasks used ventilated caps to allow for air flow.
After incubation, the resulting supernatant was harvested, filtered in order to remove cell debris, and inactivated. The supernatant was inactivated by bringing its temperature to 37±2° C. and binary ethlylenimine (BEI) was added to the supernatant to a final concentration of 5 mM. The samples were then stirred continuously for 72 to 96 hrs. A 1.0 M sodium thiosulfate solution to give a final minimum concentration of 5 mM was added to neutralize any residual BEI. After inactivation, PCV2 ORF-2 buffered with phosphate buffer and Carbopol was added to about 0.5 to 2.5 mg/dose. The final dose comprises about 16 μg PCV2 ORF-2 antigen.
EXAMPLE 2
Anti PCV-2 Immuno Assay
PK15 (e.g. ATCC CCL-33) or VIDO R1 cells described in WO 02/07721, are seeded onto a 96 well plate (about 20.000 to 60.000 cells per wells). Cells are infected with a PCV2 isolate, when monolayers are approximately 65 to 85% confluent. Infected cells are incubated for 48 hours. Medium is removed and wells are washed 2 times with PBS. The wash buffer is discarded and cells are treated with cold 50/50 methanol/acetone fixative (˜100 μl/well) for about 15 min at about −20° C. The fixative is discarded and the plates are air tried. Serial dilutions of porcine serum samples are prepared in PBS, added to the plates and incubated to allow antibodies to bind if present in the serum samples for about 1 hr at 36.5±1° C. In addition, serial dilutions of an anti-PCV2 positive and negative control sample (Positive Control and Negative Control Samples) are run in parallel. The plates are then washed three times with PBS. The PBS is discarded. Plates are then stained with a commercial Goat anti-Swine FITC conjugate diluted 1:100 in PBS and incubated for about 1 hr at 36.5±1° C., which allows detection of antibodies bound to infected cells. After incubation is complete, the microplates are removed from the incubator, the conjugate is discarded and the plates are washed 2 times with PBS. The plates were read using UV microscopy and individual wells reported as positive or negative. The Positive Control and Negative Control samples are used to monitor the test system. If the controls are within expected ranges the test results are acceptable in regard to test method parameters. The serum antibody titers were calculated using the highest dilution showing specific IFA reactivity and the number of wells positive per dilution, or a 50% endpoint is calculated using the appropriate Reed-Muench formula.
EXAMPLE 3
Efficacy of PCV2 ORF-2 (Ingelvac® CircoFLEX™) in Treatment of Chronic PCV2 Infection
Study Objective and Design
Conventional piglets from five consecutive week groups, each comprising approximately 300 animals were included into this study. Animals were equally distributed among two treatment groups with respect to initial body weight and litter assignment. At the day of weaning, one group (n=775) was vaccinated with Ingelvac® CircoFLEX, containing the minimum release antigen content and the other group of piglets (n=773) received control product (physiological saline). The vaccine and the control product (CP) were given as a single 1 ml dose intramuscularly in the right neck region when piglets were approx. 21 days old. Individual live body weights of all study animals were collected. Clinical observations with respect to PCV2 associated symptoms were performed and deviations from normal general health were recorded on an individual animal basis.
Serum samples and nasal secretions were analyzed quantitatively by Polymerase Chain Reaction (PCR) for the presence of PCV2. In addition, the PCV2 antibody titers from all study animals at the time of vaccination and from the same 5% of the pre-selected study animals were analyzed by an Indirect Fluorescent Antibody Titration (IFAT) test as described in Example 2.
Confirmation of the Chronic (Sub-Clinical) Status of the Study Site:
The first diagnosis of PCVD on the farm was done 4 months before the performance of the study. A mortality rate of 14.1% and the presence of runts in the fattening unit were identified. The growth performance was rather low (644 g/d). The presence of a PCV2 infection was confirmed by histological examination. The lung sample showed interstitial pneumonia and PCV-2 was identified by IHC among the lesions.
When looking at FIG. 1 , it can be seen that the mortality rate in fattening decreased considerably from 14.1% to 8.1% suggesting a shift of an acute PCVD infection to sub-clinical infection.
Confirmation of the Subclinical Infection of the Study Animals
The shift to sub-clinical infection on the farm was confirmed by the results obtained during the study. The study animals were characterized by a predominant sub-clinical viral load, a low mortality rate (below 10%) and a low morbidity rate (below 10%).
RESULTS
Viremia
The highest proportion of viremic animals was observed at study week 14 with 55.5% viremic animals in the CP-treated group and approximately 10% viremic animals in the vaccinated group. As shown in FIGS. 4 and 5 , the majority of animals in both treatment groups had only sub-clinical viral loads (defined as 10 4 -10 6 genomic equivalents per ml). The highest proportion of animals with clinically relevant PCV2 loads (>10 6 genomic equivalents per ml) was 2.52% for CP-treated animals and 0.87% for vaccinated animals.
Mortality
The mortality rate before and after onset of viremia was rather low. Prior to the onset of viremia, the mortality rate was 1.55% in the vaccinated animals and 2.19% in the CP -treated animals. After the onset of viremia an increase in the mortality rate was observed in CP-treated animals (from 1.55% to 3.02%) whereas the mortality rate in vaccinated animals was slightly decreased compared to the time before onset of viremia (from 2.19% to 1.98%). The differences in the mortality rate among both treatment groups before and after onset of viremia did not reach statistical significance.
Clinical Signs
Before onset of viremia only few clinical signs were detected in both treatment groups with incidences below 1% for each of the analyzed parameters. The onset of viremia was accompanied by a co-infection with PRRSV and Mycoplasma hyopneumoniae . However, neither PCV2 nor any other co-infectious pathogen caused severe clinical signs. Accordingly, the proportion of animals with respiratory symptoms such as cough and/or dyspnea was only 3.9% and 0.7% in the CP-treated group and 3.0% and 0.4% in the vaccinated group. The frequency of other clinical findings was always below 1% and not different between treatment groups.
Frequency of Runts
No significant differences in the frequency of ‘runts’ could be observed between the vaccinated and the placebo-treated group on any of the respective weighing time points. After the overall onset of PCV2 viremia, the frequency of ‘runts’ was generally low in both treatment groups (3.3-4.7%).
TABLE 1 Comparison of the frequency of ‘runts’ (pooled data of all three week groups) Before Onset of viremia After Onset of viremia Study week 0 7 12 17 22 CP 11.51% 11.94% 5.68% 4.72% 4.53% IVP 10.84% 10.46% 4.78% 3.36% 3.27% P 0.6874 0.3728 0.4884 0.1898 0.2259 P: p-value of t-test for comparison between groups; p > 0.05 no significant
Impact of Subclinical Infection on Growth Performances
Body weight gain until study week 17 was 2.36 kg higher and until study week 19 it was 2.39 kg higher in the vaccinated group than in the CP-treated group. As shown in FIG. 3 , the body weight difference began to rise slightly at the time of the onset of viremia (study week 12). On study week 17, the difference reached was already 2.36 kg. Due to the higher weight gain, the mean time from weaning to slaughter was 1.9 days shorter for the vaccinated animals than for the CP-treated animals.
TABLE 2 Comparison of Weight gain and ADWG (pooled data of all five week groups) CP-treated Vaccinated Difference Study Group Group (IPV minus week (LSMean) (LSMean) CP) p-value 1) Weight gain 0-7 20.63 kg 20.71 kg 0.08 kg 0.7166 ns 0-17 76.73 kg 79.09 kg 2.36 kg >0.0001 *** 0-19 86.75 kg 89.14 kg 2.39 kg <0.0001 *** 12-17 29.05 kg 30.73 kg 1.68 kg <0.0001 *** 7-19 66.07 kg 68.38 kg 2.31 kg <0.0001 *** 1) p-value of t-test for comparison between groups, ns: not significant; * significant, p ≦ 0.05; *** significant, p ≦ 0.001
Duration of Viremia in the Blood
When comparing the overall mean and median duration of viremia in the two treatment groups, a significantly longer (p=0.0003) duration of viremia was detected in the CP-treated animals. The IVP group had a mean duration of viremia of 5.8 days while the CP group showed a mean duration of 21.8 days. This corresponds to a reduced duration of viremia by 73% in the IVP group.
TABLE 3
Mean and median duration of viremia
Treatment
Number of
Mean
Median
group
pigs
(days)
(days)
p-value
Total
CP
76
21.8
14.0
0.0003
IVP
18
5.8
0.0
***
IVP minus CP
−16.0
−14.0
P: p-value of t-test for comparison between groups
ns: not significant,
p > 0.05;
* significant, p ≦ 0.05
CONCLUSION
The study has been conducted on a farm that shifted from an acute to a chronic status with sub-clinical infection shortly before the implementation of the study. The viral load of the study animals during the study confirmed that assumption. Very few study animals (<2.19%) had viral load in serum above the “clinical cut-off” of 10 6 /ml genomic copies.
The vaccination succeeded in lowering tremendously the percentage of infected animals in the vaccinated group. Therefore, the vaccination enabled the comparison of non-infected animals (vaccinated group) with sub-clinically infected animals (placebo group). Vaccinated animals demonstrated better growth performances than sub-clinically infected animals. On study week 17, the difference reached already 2.36 kg. Vaccinated animals had a more than 16 day shorter duration of viremia as compared to the non-vaccinated group.
It can be concluded that although infected animals remained apparently healthy, PCV2 subclinical infection can have a relevant negative impact on the growth performances. | The present invention relates to the use of an immunogenic composition comprising a porcine circovirus type 2 (PCV2) antigen for the prevention and treatment of sub-clinical PCV2 infection in animals, preferably in pigs. | 2 |
BACKGROUND OF THE INVENTION
In a scroll compressor the trapped volumes are in the shape of lunettes and are defined between the wraps or elements of the fixed and orbiting scrolls and their end plates. The lunettes extend for approximately 360° with the ends of the lunettes defining points of tangency or contact between the wraps of the fixed and orbiting scrolls. These points of tangency or contact are transient in that they are continuously moving towards the center of the wraps as the trapped volumes continue to reduce in size until they are exposed to the outlet port. As the trapped volumes are reduced in volume the ever increasing pressure acts on the wrap and end plate of the orbiting scroll tending to axially and radially move the orbiting scroll with respect to the fixed scroll.
Radial movement of the orbiting scroll away from the fixed scroll is controlled through radial compliance. Eccentric bushings, swing link connections and slider blocks have all been disclosed for achieving radial compliance. Each approach ultimately relies upon the centrifugal force produced through the rotation of the crankshaft to keep the wraps in sealing contact.
Axial movement of the orbiting scroll away from the fixed scroll produces a thrust force. The weight of the orbiting scroll, crankshaft and rotor may act with, oppose or have no significant impact upon the thrust force depending upon whether the compressor is vertical or horizontal and, if vertical, whether the motor is above or below the orbiting scroll. Also, the highest pressures correspond to the smallest volumes so that the greatest thrust loadings are produced in the central portion of the orbiting scroll but over a limited area. The thrust forces push the orbiting scroll against the crankcase with a large potential frictional loading and resultant wear. A number of approaches have been used to counter the thrust forces such as thrust bearings and a fluid pressure back bias on the orbiting scroll. Discharge pressure and intermediate pressure from the trapped volumes as well as an external pressure source have been used to provide the back bias. Specifically, U.S. Pat. Nos. 3,600,114, 3,924,977 and 3,994,633 utilize a single fluid pressure chamber to provide a scroll biasing force. This approach provides a biasing force on the orbiting scroll at the expense of very large net thrust forces at some operating conditions. As noted, above, the high pressure is concentrated at the center of the orbiting scroll but over a relatively small area. If the area of back bias is similarly located, there is a potential for tipping since some thrust force will be located radially outward of the back bias. Also, with the large area available on the back of the orbiting scroll, it is possible to provide a back bias well in excess of the thrust forces.
SUMMARY OF THE INVENTION
An axial ring is provided which coacts with the back of the orbiting scroll to form two annular fluid pressure chambers for providing a back bias to the orbiting scroll. Preferably the inner annular chamber is at discharge pressure and the outer annular chamber is at an intermediate pressure. This arrangement locates the discharge chamber and the greatest back bias opposite the greatest thrust force. A wider operating envelope is possible because the dual pocket configuration allows for a smaller range of thrust forces than a single pocket configuration and thereby provides a more stable arrangement. The annular axial ring is carried by the orbiting scroll so that there is no relative radial movement between the members defining the annular chambers. As a result, radial seals can be employed which essentially eliminate wear on the seals. Thus, the present invention provides a smaller range of net thrust forces throughout the operating envelope and is therefore at least as efficient as known designs while avoiding seizure at the scroll tips and excessive wear due to excessive thrust forces.
It is an object of this invention to provide a wider and more stable operating envelope.
It is another object of this invention to improve axial compliance over the entire operating envelope.
It is a further object of this invention to minimize thrust losses on the back face of the orbiting scroll.
It is an additional object of this invention to provide a radial seal to thereby decrease seal friction and tolerance sensitivity in the axial direction. These objects, and others as will become apparent hereafter, are accomplished by the present invention.
Basically, two pressure pockets are created to push the orbiting scroll against the fixed scroll to minimize leakage. One pocket is at intermediate pressure and the other is at discharge pressure. The pockets are defined between an axial ring which moves with the orbiting scroll and the orbiting scroll so that radial seals can be used with no relative movement between the parts defining the pockets during operation.
BRIEF DESCRIPTION OF THE DRAWINGS
For a fuller understanding of the present inventions, reference should now be made to the following detailed description thereof taken in conjunction with the accompanying drawings wherein:
FIG. 1 is a sectional view of the fixed and orbiting scroll of a scroll compressor taken along line 1--1 of FIG. 2;
FIG. 2 is a sectional view taken along line 2--2 of FIG. 1;
FIG. 3 is a sectional view taken along line 3--3 of FIG. 2; and
FIG. 4 is an enlarged sectional view of the sealing structure.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In FIG. 1, the numeral 10 generally designates the orbiting scroll of a scroll compressor. Orbiting scroll 10 has wrap 10-1 and an inner axial bore 10-2 and an outer axial bore 10-3. Referring now to FIG. 2, it will be noted that bore 10-2 is in fluid communication with annular pocket or chamber 12 via radial bore 10-4 and axial bore 10-5. Similarly, bore 10-3 is in fluid communication with annular pocket or chamber 13 via radial bore 10-6 and axial bore 10-7. Axial ring 16 coacts with the plate portion 10-11 of orbiting scroll 10 to define radially spaced annular pockets or chambers 12 and 13. Specifically, orbiting scroll 10 has an inner annular recess 10-8 partially defining chamber 12, an outer annular recess 10-10 partially defining chamber 13 with an axial annular projection 10-9 separating recesses 10-8 and 10-10. Axial ring 16 is received in recesses 10-8 and, 10-10 to partially define chambers 12 and 13 and is movable with orbiting scroll 10. Axial ring 16 has an outer annular shoulder 16-1, an inner annular shoulder 16-3 and intermediate annular recess 16-2. Annular radial seal 21 is located on annular shoulder 16-1 and sealingly engages the outer wall of recess 10-10. Annular radial seal 22 is located in annular recess 16-2 as is annular projection 10-9 which coacts therewith to provide a fluid seal. Annular radial seal 23 is located on annular shoulder 16-3 and sealingly engages the inner wall of recess 10-8. The relationship of chambers 12 and 13 as well as that of seals 21-23 is best illustrated in FIG. 3 which clearly shows that chamber 13 is defined in part by seal 21, axial ring 16 and annular projection 10-9 while chamber 12 is defined in part by seal 22, axial ring 16 and seal 23. The rear or bottom face 16-4 of axial ring 16 engages surface 30-1 of crankcase 30 in a thrust relationship with axial ring 16 orbiting with respect to surface 30-1.
Referring now specifically to FIG. 4, it will be noted that annular projection 10-9 is of a lesser axial extent than the depth of annular recess 16-2. Sealing between chambers 12 and 13 is achieved by annular radial seal 22 which is forced against the inner wall and bottom of annular recess 16-2 and the inner wall of annular projection 10-9 by the pressure in chamber 12 as well as the resiliency of radial seal 22. Similarly, the pressure in chamber 13 as well as the resiliency of radial seal 21 causes seal 21 to seal against the bottom and side of shoulder 16-1 as well as the outer wall of recess 10-10. The pressure in chamber 12 as well as the resiliency of radial seal 23 causes seal 23 to seal against the bottom and side of shoulder 16-3 as well as the inner wall of recess 10-8.
In operation, as orbiting scroll 10 is driven by the crankshaft (not illustrated), it carries axial ring 16 through its orbital movement so that there is, in general, no relative movement between orbiting scroll 10 and axial ring 16. As wrap 10-1 of orbiting scroll 10 coacts with wrap 11-1 of the fixed scroll 11 to establish and compress trapped volumes of gas, A-E, gas in the trapped volume D which is exposed to bore 10-3 is communicated to chamber 13 while gas in the trapped volume A which is exposed to bore 10-2 and the outlet (not illustrated) in fixed scroll 11 is communicated to chamber 12. Since bore 10-3 is located at an intermediate point in the compression process while bore 10-2 is located in the vicinity of the outlet, chamber 12 is nominally at discharge pressure while chamber 13 is at an intermediate pressure. The pressures in chambers 12 and 13 act against orbiting scroll 10 to keep it in engagement with the fixed scroll 11 to thereby minimize leakage at the tips of the wraps 10-1 and 11-1. The pressures in chambers 12 and 13 also act against axial ring 16 to force it against surface 30-1 of crankcase 30. This combination of axial forces may cause axial ring 16 and seals 21-23 to be moved axially at start up and shutdown but the movement will be relatively small. Because axial ring 16 moves with orbiting scroll 10 and is forced against surface 30-1, any wear will tend to take place between these two members but such wear will be minimized through proper lubrication.
Although chamber 13 has been described as being at intermediate pressure and chamber 12 at discharge pressure, bore 10-4 could be relocated so as to communicate bores 10-2 and 10-7 and bore 10-6 can similarly be relocated to communicate bores 10-3 and 10-5. This would result in discharge pressure being supplied to chamber 13 and intermediate pressure being supplied to chamber 12. While intermediate pressure is generally less than discharge pressure it is not necessarily true during all operating conditions and therefore just describes an intermediate point during the compression process. Specifically, the pressures achieved during the compression process depend upon a number of factors such as the mass being compressed and leakage. Thus, under some conditions, over compression can take place such that the intermediate pressure is greater than the discharge pressure since the discharge pressure is influenced by the system downstream of the discharge rather than, solely, the pressure delivered to the discharge from the compression process.
From the foregoing description, it should be clear that there is an improved axial compliance over the entire operating envelope because of the relatively large total radial extent and areas of pockets 12 and 13 and because they are responsive to two pressures in the compression process. The seal design is such that there is little if any movement relative to the seals which decreases seal wear and axial sensitivity.
Although a preferred embodiment of the present invention has been illustrated and described, other changes will occur to those skilled in the art. It is therefore intended that the scope of the present invention is to be limited only by the scope of the appended claims. | Two annular pressure pockets are used to push the orbiting scroll against the fixed scroll to minimize leakage. One pocket is at intermediate pressure and the other is at discharge pressure. The pockets are defined by the orbiting scroll and an axial ring carried by the orbiting scroll which permits the use of radial seals thereby essentially eliminating wear on the seals. | 5 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a framework for 3D non-photorealistic rendering and a method of configuring the framework, and more particularly, to a framework that renders a 3D model in a general and intuitive manner like the way an artist selects a style and paints a model with the selected style and has a flexible style expandability for efficient non-photorealistic rendering by using a unified concept of expressing various rendering styles using just two rendering methods (face painting and line drawing), and a method of configuring the framework.
[0003] 2. Description of the Related Art
[0004] With the increasing interest in non-photorealistic rendering and animation, a number of researches have been conducted to generate images in an artistic style that look like a painting or drawing. Early researches are focused on developing non-photorealistic rendering and animation systems that are individually dedicated to expressing a particular rendering style. Such systems use a non-photorealistic rendering pipeline that is obtained by slightly modifying a traditional rendering pipeline.
[0005] Recently, unified frameworks have been researched to establish such an individual non-photorealistic rendering pipeline and provide a non-photorealistic rendering that is different from the existing photorealistic rendering. In a framework for non-photorealistic rendering based on a particle (1996), a particle is used to determine the position of a stroke (denoting a brush touch). The particle-based framework is the earliest framework that is still in use. Further, examples of recently proposed frameworks include a framework that expresses a 3D model using an adaptively sampled distance field (ADF) (an article titled “A New Framework for Non-photorealistic rendering”, 2001) and a framework based on a graphic processing unit (GPU). However, in the above-described frameworks, main concerns of non-photorealistic rendering systems (i.e., processing techniques for expressing styles) are not mentioned.
[0006] A framework somewhat different from the above-described frameworks is disclosed in “OpenNPAR (2003, an article titled ‘OpenNPAR: A system for developing, programming, and designing non-photorealistic animation and rendering’).” This OpenNPAR system is an OpenInventor-based framework, in which each rendering style for expressing a non-photorealistic effect is matched with a combination of components and a desired style is generated by recombining the components. Although the OpenNPAR system modularizes detail non-photorealistic rendering styles (detail functions) and expresses a number of styles by recombining the modularized styles, the OpenNPAR system has a complicated basic concept in intuitive and non-photorealistic expressing. Further, the OpenNPAR system has a complicated basic pipeline that supports a developer (develops modules), a programmer (produces modifiers using the modules), a designer (generates styles using the modifiers), and a user.
SUMMARY OF THE INVENTION
[0007] Accordingly, the present invention is directed to a unified framework based on extensible styles for 3D non-photorealistic rendering and a method of configuring the framework, which substantially obviates one or more problems due to limitations and disadvantages of the related art.
[0008] It is an object of the present invention to provide a unified framework based on extensible styles for 3D non-photorealistic rendering and a method of configuring the framework. The framework has an intuitive structure such that rendering styles can be conveniently expanded for both face-painting and line-drawing methods.
[0009] It is another object of the present invention to provide a rendering system employing a unified framework based on extensible styles for 3D non-photorealistic rendering, the unified framework unifying all rendering methods using face-painting and line-drawing methods such that system developers can easily provide styles satisfying designers' demand.
[0010] Therefore, the rendering styles generated by the unified framework of the present invention can be intuitively used for rendering a 3D model without distinguishing the interior, outside, and lines of the 3D model.
[0011] Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
[0012] To achieve these objects and other advantages and in accordance with the purpose of the invention, as embodied and broadly described herein, there is provided a unified framework based on extensible styles for 3D non-photorealistic rendering, the unified framework including: 3D model data processing means for generating a scene graph by converting a 3D model input into 3D data and organizing the scene graph using vertexes, faces, and edges; face painting means for selecting a brusher to paint faces (interiors) of the 3D model using the scene graph; line drawing means for extracting line information from the 3D model using the scene graph and managing the extracted line information; style expressing means for generating a rendering style for the 3D model and storing the rendering style as a stroke, the rendering style being equally applied to a face-painting method and a line-drawing method; and rendering means for combining the stroke and the selected brusher to render the 3D model using both the face-painting method and the line-drawing method.
[0013] In another aspect of the present invention, there is provided a method of configuring a unified framework based on extensible styles for 3D non-photorealistic rendering. The method configures the framework to render a 3D model in a general and intuitive manner like an artist selects a style and paints a model with the selected style, and to apply various rendering styles to face-painting and line-drawing such that all 3D models can be rendered only by face-painting and line-drawing regardless of rendering styles for the 3D models.
[0014] In a further another aspect of the present invention, there is provided a method of configuring a unified framework based on extensible styles for 3D non-photorealistic rendering, the method including the step of configuring the unified framework to generate a rendering style for a 3D model and simultaneously apply the style by combining the style with a face-painting brusher and a line-drawing brusher, wherein the step of configuring the unified framework includes: parsing 3D model data of the 3D model according to a predetermined format to generate a scene graph; organizing the 3D model data based on vertexes, faces, and edges using the scene graph; selecting a brusher for painting an interior of the 3D model using the scene graph; extracting line characteristic information including silhouette, crease, and boundary line information by using the scene graph; generating interior lines (hatch lines) using the scene graph for the interior of the 3D model; and generating a rendering style for being used to render the 3D model finally.
[0015] It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory and are intended to provide further explanation of the invention as claimed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The accompanying drawings, which are included to provide a further understanding of the invention, are incorporated in and constitute a part of this application, illustrate embodiments of the invention and together with the description serve to explain the principle of the invention. In the drawings:
[0017] FIG. 1 is a schematic view illustrating a framework for non-photorealistic rendering according to the present invention;
[0018] FIG. 2 is a block diagram illustrating a framework for non-photorealistic rendering according to an embodiment of the present invention;
[0019] FIG. 3 is a schematic view illustrating a set of a style and a brusher used in a non-photorealistic rendering framework as a basic component for style expression according to the present invention;
[0020] FIG. 4 is a view for explaining intermediate outputs of operation steps of a non-photorealistic rendering framework according to the present invention; and
[0021] FIG. 5 shows examples of rendering styles developed based on a non-photorealistic rendering framework according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0022] A unified framework based on extensible styles for 3D non-photorealistic rendering will now be described in detail with reference to the accompanying drawings according to preferred embodiments of the present invention.
[0023] FIG. 1 is a schematic view illustrating a framework for generating a non-photorealistically rendered image according to the present invention. Referring to FIG. 1 , the framework of the present invention is configured based on the way a person draws a picture.
[0024] In the framework of the present invention, non-photorealistic images are rendered by imitating the way an artist paints a picture and based on the concept that all non-photorealistic images can be rendered through interior area (face) painting and line drawing.
[0025] The framework can be easily expanded and modified for non-photorealistically rendering a 3D model using various styles. For this, the framework is configured such that rendering is performed using two methods (face painting and line drawing) for a 3D model selected for “what to paint?” and a style selected for “how to paint” is defined as a pair of a stroke and a brusher (rendering tool).
[0026] FIG. 2 is a block diagram illustrating a framework for non-photorealistic rendering according to an embodiment of the present invention. Each part of the non-photorealistic rendering framework will now be described with reference to FIG. 2 according to the embodiment of the present invention.
[0027] The non-photorealistic rendering framework includes a 3D model data manager 100 , a style manager 200 , a face painting manager 300 , a line drawing manager 400 , a characteristic line extracting manager 500 , an interior line extracting manager 600 , a motion line extracting manager 700 , a face painting brusher group 800 , a line drawing brusher group 900 , and a state manager 1000 .
[0028] In detail, the 3D model data manager 100 is a processor that processes and manages all 3D data used in the non-photorealistic rendering framework. The 3D model data manager 100 includes a 3D model data parsing module 110 that reads 3D model data and generates a scene graph in a predetermined format, and a 3D model data organizing module 120 that expresses the generated scene graph using vertexes, faces, and edges.
[0029] The style manager 200 is a processor that produces and manages non-photorealistic rendering styles used in the non-photorealistic rendering framework. The style manager 200 includes a style generating module 210 providing common functions for generating various styles, and a detail style generating module 220 for expressing detail features of each style generated by the style generating module 210 .
[0030] The face painting manager 300 is a processor for painting faces (interior areas) of a 3D model used in the non-photorealistic framework according to a rendering style generated by the style manager 200 . The face painting manager 300 includes a face painting control module 310 for receiving controls from a user.
[0031] The line drawing manager 400 is a processor for drawing lines of a 3D model used in the non-photorealistic framework according to a rendering style generated by the style manager 200 . The line drawing manager 400 includes a line drawing control module 410 for receiving controls from a user.
[0032] The characteristic line extracting manager 500 is a process that extracts characteristic lines from a 3D model used in the non-photorealistic rendering framework and manages the extracted characteristic lines. The characteristic line extracting manager 500 includes a characteristic line extracting group 510 that provides upper functions commonly used for extracting characteristic lines, a characteristic line extracting module 520 that provides a common interface based on each extracted characteristic line, and a detail characteristic line extracting module 530 that extracts characteristic lines according to detail categories.
[0033] The interior line extracting manager 600 is a process that generates interior lines (hatch lines) of a 3D model used in the non-photorealistic rendering framework. The interior line extracting manager 600 includes an interior line extracting group 610 that provides upper functions commonly used for generating interior lines, an interior line extracting module 620 providing a common interface based on each generated interior line, a detail interior line extracting module 630 extracting interior lines according to detail categories, and a particle placer module 640 determining start positions when interior lines are generated.
[0034] The motion line extracting manager 700 is a process that generates motion lines of a 3D model used in the non-photorealistic rendering framework. The motion line extracting manager 700 includes a motion line extracting group 710 that provides upper functions commonly used for generating motion lines, a motion line extracting module 720 providing a common interface based on each generated motion line, and a detail motion line extracting module 730 extracting motion lines according to detail categories.
[0035] The characteristic line extracting manger 500 , the interior line extracting manager 600 , and the motion line extracting manager 700 , which are provided for generating three kinds of lines, have the same configuration. Thus, the framework can be easily extended or modified according to the size of a developed system.
[0036] The face painting brusher group 800 is a processor for painting the inside of a 3D model used in the non-photorealistic rendering framework. The face painting brusher group 800 includes a brusher group 810 providing a face painting brusher as a painting tool and a brusher module 820 providing a detail face painting function.
[0037] The line drawing brusher group 900 is a processor for drawing lines of a 3D model used in the non-photorealistic rendering framework. The line drawing brusher group 900 includes a line drawing brusher module 910 providing a line drawing brusher as a line drawing tool and a detail line drawing brusher module 920 providing a detail line drawing function. The state manager 1000 stores and manages states of all processors of the non-photorealistic framework and states of a system developed based on the non-photorealistic framework.
[0038] A face painting render 20 and a line drawing render 30 perform rendering functions (face painting and line drawing) using data output from the above-described processors 100 to 900 based on states stored in the state manager 1000 . Processing operations of the processors 100 to 900 are performed for each frame of a rendering model by a non-photorealistic render 10 .
[0039] The structures and functions of the processors 100 to 900 of the non-photorealistic rendering framework shown in FIG. 2 will now be more fully described with reference to FIG. 4 that shows intermediate outputs of the processors 100 to 900 .
[0040] The 3D model data manager 100 performs various functions for processing 3D data using a scene graph generated by the 3D model data parsing module 110 . The 3D model data organizing module 120 performs the most importance function in the non-photorealistic rendering process using the scene graph. That is, the 3D model data organizing module 120 calculates boundary information for vertexes and faces. Therefore, in the non-photorealistic rendering framework of the present invention, all physical data are stored based on vertexes, and in other structures, pointer information of the vertexes are used. Thus, costs for storing and processing data can be minimized.
[0041] That is, in the framework of the present invention, an Xparser is provided as a basic module for parsing directX data, and optimization is performed by searching and removing overlapped vertex information to improve the efficiency of vertex-based calculation since the directX data are stored in the form of a connected structure of overlapped vertexes. Here, a current vertex is compared with a vertex located after the current vertex in the data structure (one-on-one comparison) to determine whether it is overlapped. Therefore, the time for this optimization depends on the number of vertexes of an object.
[0042] The style manager 200 manages color and test information and allows the face painting manager 300 and the line drawing manager 400 to access a stroke array 230 in which various styles are stored for expressing a 3D model using various styles. The style generating module 210 performs common functions for generating styles using information expressed using 3D model data such as vertexes, faces, and edges by the 3D model data manager 100 , and the detail style generating module 220 determines detail features of the generated styles. That is, the style generating module 210 provides a common interface for the detail style generating module 220 , so that a user (or a developer) can easily expand the style.
[0043] The face painting manager 300 and the line drawing manager 400 perform uppermost managing functions for painting faces and drawing lines, respectively. That is, the face painting manager 300 and the line drawing manager 400 manage rendering works of the render processors 10 , 20 , and 30 .
[0044] The characteristic line extracting manager 500 is a processor including modules that extracts characteristic lines and performs management functions. That is, the characteristic line extracting manager 500 extracts characteristic lines collectively called contour. When the characteristic line extracting group 510 extracts characteristic lines, the characteristic line extracting module 520 provides a common interface according to each characteristic line. The detail characteristic line extracting module 530 extracts detail characteristic lines for the extracted characteristic lines through the common interface according to detail categories, thereby extracting characteristic lines called contour.
[0045] That is, the framework of the present invention provides basic characteristic lines: silhouette, crease, boundary, and suggestive contour lines. Typical tools available in the market provide functions for extracting silhouette, crease, and boundary lines. The suggestive contour line extracting scheme has been recently developed. The framework of the present invention is configured such that a user (or a developer) can easily apply an additional structure to the framework for extracting characteristic lines of new types.
[0046] When the characteristic line extracting manager 500 extracts a 3D contour from an object, the interior line extracting manager 600 generates interior lines for expressing the faces (defined between contour lines) of the object. The interior lines are defined using start points and directions. The start points of the interior lines are defined by the particle placer module 640 . Additionally, the start points of the interior lines can be manually defined by an end user through the line drawing control module 410 in a device configured based on the framework of the present invention. The interior lines are defined from the start points along directional fields generated by the 3D model data manager 100 . The interior lines may be straight or curved depending on the direction fields. Like the characteristic line extracting manager 500 , the interior line extracting manager 600 is configured such that a user (or a developer) can easily apply an additional structure for generating interior lines having a different type.
[0047] The motion line extracting manager 700 generates motion lines for each frame of a rendering image according to motions obtained by animating the rendering image regardless of geometrical information of a 3D model. Like in the interior line extracting manager 600 , initial positions of the motion lines can be determined by receiving inputs from a used through the line drawing control module 410 .
[0048] The interior painting brusher group 800 and the line drawing brusher group 900 are tools actually performing face painting and line drawing. Each brusher is coupled with a stroke expressing a style for drawing an image according to a predetermined style. That is, a stroke expressing a style generated by the style manager 200 is coupled to each brusher selected from the face painting brusher group 800 and the line drawing brusher group 900 , such that the number of styles can be N*M when the used numbers of strokes and brushers are N and M.
[0049] Although the brushers of the framework of the present invention are classified into the face painting brusher group 800 and the line drawing brusher group 900 , common brushers can be used for face painting and line drawing. The brushers include a 3D polygon brusher, a 2D projection brusher, a 2D brusher, a color brusher, and a texture brusher in order to express a given style.
[0050] Since the framework of the present invention is configured based on face painting and line drawing, the state manager 1000 manages the overall operation of the framework and the face painting and line drawing operations of the framework. The framework of the present invention has a very intuitive and easily understandable structure, such that the state of the framework can be simply performed.
[0051] The non-photorealistic render 10 calls the face painting render 20 and the line drawing render 30 and performs line drawing and face painting by using data generated or extracted by the processors of the framework.
[0052] FIG. 3 is a schematic view illustrating a set of a style and a brusher used in a non-photorealistic rendering framework as a basic component for style expression according to the present invention. That is, the brusher is coupled with a predetermined stroke expressing a particular style, and then it is used as a tool for painting or drawing faces and lines in an intuitive manner.
[0053] FIG. 5 shows exemplarily images rendered using various styles generated by a non-photorealistic rendering system developed based on the framework of the present invention.
[0054] As described above, according to the unified framework base on extensible styles for 3D non-photorealistic rendering, functions for generating various non-photorealistic rendering styles are included in the same structure (the style manager 200 ) to use the functions in the same way, and an intuitive painting tool (refer to FIG. 3 ) for expressing a particular style is made by replacing a stroke coupled to a brusher with another stroke expressing the particular style, such that each required function can be effectively provided for non-photorealistic rendering. Further, every non-photorealistic rendering style is expressed by the unified concept of face painting and line drawing, so that easily understandable framework can be provided. As a result, tools and styles can be easily developed for non-photorealistic rendering and animation.
[0055] It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention. Thus, it is intended that the present invention covers the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. | There are provided a unified framework based on extensible styles for 3D non-photorealistic rendering and a method of configuring the framework. The unified framework includes: 3D model data processing means for generating a scene graph by converting a 3D model input into 3D data and organizing the scene graph using vertexes, faces, and edges; face painting means for selecting a brusher to paint faces (interiors) of the 3D model using the scene graph; line drawing means for extracting line information from the 3D model using the scene graph and managing the extracted line information; style expressing means for generating a rendering style for the 3D model and storing the rendering style as a stroke, the rendering style being equally applied to a face-painting method and a line-drawing method; and rendering means for combining the stroke and the selected brusher to render the 3D model using both the face-painting method and the line-drawing method. The framework can be used to develop tools and new rendering styles for non-photorealistic rendering and animation. | 6 |
CROSS REFERENCE TO RELATED APPLICATION
[0001] This patent specification is based on U.S. provisional application 60/766,576, filed on Jan. 29, 2006 in the U.S. Patent and Trademark Office, the entire contents of which are incorporated by reference herein.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] This disclosure relates to a system, method, and computer program for providing brokerage services, and particularly for aggregated access to a plurality of brokerage services related to financial markets.
[0004] 2. Discussion of the Background
[0005] Today investors are discovering that computers and, in particular, electronic trading of financial instruments over computer networks such as the Internet, have greatly empowered investors to self-manage and track their financial investment portfolios. Whether an individual investor is seeking to occasionally buy or sell stocks, bonds, or other financial instruments; a day trader conducting numerous such transactions each day; or a professional investor such as a licensed broker who manages the financial portfolios of numerous clients, access via a computer network to financial markets has become increasingly an important channel to conduct these transactions.
[0006] The ease of access to electronic trading has opened up great opportunities for novice investors to actively trade and maintain portfolios of their own without requiring participation in mutual funds or assistance from financial advisors or professional portfolio managers. This has resulted in the individual investor gaining hands-on experience with trading in financial instruments such as equities, and allowing them to transition to instruments such as bonds, foreign exchanges, and other instruments over global markets.
[0007] In order to have access to concurrent access to multiple markets it is necessary to access multiple brokerage services simultaneously. First, simultaneous brokerage access allows a user to monitor and take actions on multiple markets without delay. Second, this would create a natural competitive market among the participating brokers to offer competitive brokerage commissions. For example, an options specialized broker may offer the best brokerage rates for options contracts while another broker could offer the best margins over equity trades. Similarly a specialized foreign exchange (forex) commodities broker can be in a position to offer the better deal than a generic one.
[0008] Traditionally, concurrent trading in multiple markets and multiple instruments has been the domain of big institutional investors due to the resource heavy requirement of having dedicated fund managers for each channel of execution or type of financial instrument or market. However, complex trading strategies are difficult for an individual because usually each brokerage service requires a different access terminal client or user interface that each demands dedicated extra resources when managing a personal portfolio.
SUMMARY OF THE INVENTION
[0009] According to an aspect of the present invention, a brokerage aggregation system for receiving an electronic message having at least one activity request directed to one or more brokerage service firms and outputting the activity request includes an input interface configured to receive the electronic message in a first predetermined format, a plurality of output interfaces, each configured to connect to a corresponding brokerage service firm, and to transmit the at least one activity request in one of a plurality of second predetermined formats, wherein each of the plurality of second predetermined formats corresponds with a particular brokerage service firm, and a controller configured to receive and extract the at least one activity request from the electronic message, determine to which of the plurality of output interfaces the at least one activity request is to be transferred for subsequent transmission to a destination brokerage service firm, reformat the at least one activity request from the first predetermined format to the second predetermined format corresponding to the output interface previously determined, and transfer the at least one activity request after reformatting to the determined output interface for subsequent transmission to the destination brokerage service firm.
[0010] According to another aspect of the present invention, a brokerage aggregation method for receiving an electronic message having at least one activity request directed to one or more brokerage service firms and outputting the activity request includes receiving from an input interface the electronic message in a first predetermined format; extracting the at least one activity request from the electronic message; determining to which of a plurality of output interfaces the at least one activity request is to be transferred for subsequent transmission to a destination brokerage service firm; reformatting the at least one activity request from the first predetermined format to a second predetermined format corresponding to the output interface previously determined, the second predetermined format corresponding with a particular brokerage service firm; transferring the at least one activity request after reformatting, to the determined output interface; and transmitting the reformatted at least one activity request to the destination brokerage service firm.
[0011] Still according to another aspect of the present invention, a computer readable program including instructions for receiving an electronic message having at least one activity request directed to one or more brokerage service firms and outputting the activity request, the computer program being embedded in a computer readable medium, includes receiving from an input interface the electronic message in a first predetermined format; extracting the at least one activity request from the electronic message; determining to which of a plurality of output interfaces the at least one activity request is to be transferred for subsequent transmission to a destination brokerage service firm; reformatting the at least one activity request from the first predetermined format to a second predetermined format corresponding to the output interface previously determined, the second predetermined format corresponding with a particular brokerage service firm; transferring the at least one activity request after reformatting, to the determined output interface; and transmitting the reformatted at least one activity request to the destination brokerage service firm.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] A more complete appreciation of the invention and many of the attendant advantages thereof will be readily obtained as the same becomes better understood by reference to the following detailed description when considered in connection with the accompanying drawings, wherein:
[0013] FIG. 1 shows a conventional system for accessing multiple brokerage service firms;
[0014] FIG. 2 shows a brokerage aggregator according to one embodiment of the present invention;
[0015] FIG. 3 shows a method of operation of the brokerage aggregator;
[0016] FIG. 4 shows a routing table used by the brokerage aggregator according to an embodiment of the invention;
[0017] FIG. 5 shows a method of operation of a reformatting unit used by the brokerage aggregator according to an embodiment of the present invention; and
[0018] FIG. 6 shows one implementation of a computer processing unit used in the present invention.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0019] In the following description, various aspects of the present invention will be described. For purposes of explanation, specific configurations and details are set forth in order to provide a thorough understanding of the present invention. However, it will also be apparent to one skilled in the art that the present invention may be practiced without the specific details. Furthermore, well known features may be omitted from or simplified in the specification in order not to obscure the present invention.
[0020] FIG. 1 shows a conventional system 100 used to access multiple brokerage services. In the example of FIG. 1 , a user 102 intends to make financial activity requests, such as buying or selling equities, on clearing exchanges 116 , 118 , and 120 . The clearing exchanges can represent one or more financial markets or financial exchange institutions, such as NASDAQ, The New York Stock Exchange, or any foreign exchange. Such clearing exchanges are widely known to the public and those skilled in the art.
[0021] The user has accounts with brokerage firms 110 , 112 , and 114 , each firm being able to execute transactions on a different clearing exchange. Such Brokerage firms include for example Ameritrade, E-trade, or Fidelity and other firms that are widely known to the public. The user wishes to maintain access to brokerage firms 110 , 112 , and 114 concurrently in order to efficiently complete transactions over multiple clearing exchanges. In order to accomplish this, the user must access three separate access clients 104 , 106 , and 108 simultaneously. FIG. 1 shows that each access client is running on a separate machine, with three separate connections to each brokerage firm, but the access client can also represent different interfaces that must be kept open simultaneously on the same machine. In either case, the user must switch between various user interfaces to complete each transaction, which consumes time and computer resources.
[0022] FIG. 2 shows one possible implementation of an embodiment of the claimed invention. A Brokerage Aggregation System 200 is shown having a controller 220 , an input interface 208 , and output interfaces 222 , 224 , and 226 .
[0023] In FIG. 2 , an access terminal client 204 connects to the input interface 208 . Access terminal client 204 is preferably a computer processing unit (CPU) operated by a user 202 . However it is not limited to a CPU. Access terminal client 204 may be replaced with other types of devices including, but not limited to, client terminals in communications with one or more servers, or with personal digital/data assistants (PDA), laptop computers, mobile computers, Internet appliances, two-way pagers, mobile phones, or other similar desktop, mobile or hand-held electronic devices. Other or equivalent devices can also be used to practice the invention.
[0024] The input interface 208 is preferably an Ethernet interface, however it may be any type of networking interface that is commonly known to those skilled in the art, including but not limited to a wireless interface or a serial interface. The link 206 between the access terminal client 204 and the input interface 208 is optionally achieved by an Ethernet cable connection. However, the link, and any other link or connection described in this specification, may be any type of connection achieved between two electronic devices on a network. Examples of such links are a serial communications link, a wireless connection, or any other type of connection commonly known to achieve network connectivity. Further, the communication link 206 is preferably over any IP access network, including but not limited to various derivatives of IP, TCP, UDP protocol carriers such as Internet, an intranet, a wireless access such as GPRS, a Virtual Private Network (VPN), and other types of communications networks.
[0025] The input interface 208 connects to the controller 220 . The controller 220 is shown as a sub-system within the Brokerage Aggregation System 200 . Controller 220 includes a determination unit 210 , communication bridging unit 218 , and reformatting units 212 , 214 , and 216 . Throughout this specification, the term “determination unit” may be interchanged with the term “routing unit” or “router” without changing its meaning. Also, the term “reformatting unit” may be interchanged with the term “gateway” or “gateway server” without changing its meaning.
[0026] The input interface 208 is connected to the determination unit 210 . The determination unit 210 is in one embodiment a CPU, but it may also be any computing device or router with the ability to receive, process, and transmit data according to a routing table. Such devices are commonly known to those skilled in the art.
[0027] The determination unit 210 is shown in FIG. 2 with three outputted connections 250 , 252 , and 254 , however there may be any number of outputs depending on the scale of the system. The determination unit also has a storage unit 211 for storing a routing table. The determination unit 210 further has an interface 260 that is connected to an information server 264 via a link 262 .
[0028] The outputs from determination unit 210 connect to reformatting units 212 , 214 , and 216 . FIG. 2 also shows a communication bridge 218 between the determination unit 210 and the reformatting units, however the determination unit can connect directly to the reformatting units or through any network such as a private network or the internet. There are three reformatting units 212 , 214 , and 216 shown in FIG. 2 , however there may be more depending on the scale of the system. Each reformatting unit may be implemented as a CPU, however it may be any equivalent device that can receive, process, and transmit data.
[0029] In an exemplary configuration, each determination unit is connected to a brokerage service firm, such as brokerage firms 234 , 236 , and 238 via the output interfaces 222 , 224 , and 226 . FIG. 2 shows separate physical interfaces used for the output interfaces 222 , 224 and 226 , however each output interface may instead be a virtual interface. An example of a virtual interface is where there is a single physical interface that supports one or more network addresses allowing external devices to view each network address as a separate virtual interface.
[0030] The links 228 , 230 , and 232 , that are located between each determination unit and each brokerage firm, can be any type of network connection as was discussed above.
[0031] FIG. 2 additionally shows clearing exchanges 240 , 242 , and 244 connected to the brokerage firms 234 , 236 , and 238 respectively. Each brokerage firm and clearing exchange shown in FIG. 2 may be similar to the brokerage firms and clearing exchanges discussed in reference to the conventional system in FIG. 1 .
[0032] Next, an operation of the aggregator system 200 will be described.
[0033] In the example embodiment of FIG. 2 , the client 204 has network connectivity with each brokerage firm 234 , 236 , and 238 . Preferably, this network connectivity can be achieved with normal methods of establishing IP connectivity through an IP network as is well known in the art. In this example, the user has already been authenticated to communicate with each of the brokerage firms upon establishing connectivity with the brokerage firms. Such authentication procedures are well known to those skilled in the art and will not be discussed in detail.
[0034] The user 202 interacts with the access terminal client 204 . The access terminal client 204 is shown having a graphical user interface (GUI) 205 . GUI 205 displays a variety of user options to the user. Through GUI 205 , the user can access multiple brokerage services associated with the brokerage firms 234 , 236 , and 238 to initiate activity requests. Activity requests can be any action requested by the user that pertains to a capability of the system. Examples of activity requests include, but are not limited to, an order request to buy or sell an electronically traded financial instrument, a modification request to modify an order to buy/sell a financial instrument, a request to view the portfolio for a given investor account, and a request to view recent trade history for a given investor account.
[0035] After the user makes a selection on a type of activity request, the access terminal client 204 generates an activity request to be sent to the controller 220 . The activity request itself contains information data pertaining to the type of specific transaction that the user inputted to the GUI 205 . The activity request is contained in an electronic message that is formatted for transmission to the controller 220 . It is noted that multiple activity requests may be contained in the message for situations where the user wishes to perform multiple activity requests simultaneously.
[0036] The access terminal client 204 formats the message containing the activity request into a common intermediate format (CIF) standard such as Financial Information eXchange (FIX). The FIX standard is exemplary, but any other open standard for formatting financial transactions may be used.
[0037] A method illustrating how the message from the user 202 is transmitted to the brokerage firms is shown in FIG. 3 . In step 302 , the input interface 208 receives the message over link 206 and delivers it to the determination unit 210 . The determination unit 210 stores an order routing table in the storage unit 211 . In step 304 , the determination unit 210 extracts the activity request from the message formatted in the common intermediate format (first predetermined format).
[0038] In FIG. 3 , step 306 , the determination unit 210 determines to which output interface to transfer the activity request(s). The activity request or order is matched against the entry in the order routing table for a valid pathway to the brokerage service firm. In this example, the order routing table optionally checks a user ID, a destination brokerage firm ID, and then checks to see the proper destination reformatting unit 212 , 214 , or 216 . If a valid entry exists, the same order still in the common intermediate format is forwarded further to the proper reformatting unit.
[0039] An exemplary order routing table 400 is illustrated in FIG. 4 . The activity request is checked to see which user and which broker have been specified. The “Gateway” column 408 indicates which gateway, or reformatting unit the request will be routed to. As an optional column, the type of market as listed in column 406 may be specified in the activity request as an indicator on where to route the message.
[0040] Additionally, a list of symbols to route to a specific brokerage firm may be in an optional column 410 (example “IBM.L” traded on FTSE is linked to “BROKER- 2 ” for execution action in FTSE not NYSE that “BROKER- 1 ” provides which is also associated with “USER- 1 ”). The information illustrated in FIG. 4 is exemplary only. Other types of electronic information in other formats can also be used and the invention is not limited to the electronic information displayed in FIG. 4 .
[0041] In FIG. 3 , step 308 , the reformatting unit receives the activity request from the determination unit and reformats it from the CIF format to the brokerage firm format (second predetermined format) for the corresponding destination brokerage service firm. Each reformatting unit maintains a communication link with a specific brokerage service firm. The brokerage service firm may be a private institution that is designed to receive activity requests in a predetermined format or protocol. The protocol employed by each brokerage firm will be different from the CIF used by the terminal access client 204 , and in many cases the protocol used by the brokerage service firm will be proprietary to the brokerage service firm.
[0042] In FIG. 3 , step 310 , the reformatting unit transfers the reformatted activity request to a corresponding output interface, which is either 222 , 224 , or 226 in FIG. 2 . Then, in step 312 , the output interface transmits the reformatted activity request to the destination brokerage firm.
[0043] FIG. 5 shows an example activity request and the resulting translating action the gateway server performs. Here an activity request such as 508 for a buy order of 100 stocks of symbol IBM at market price is requested from access terminal client, and the request in common intermediate format (such as FIX). The activity request is transformed into the broker specific format using the database 502 based on table 504 . A sample structure of table 504 is shown in FIG. 5 and may contain an activity type (such as 514 ), a broker side proprietary format string (such as 512 ) and a system side common intermediate format (such as 510 ).
[0044] Although not shown in FIG. 5 , it should be understood that the similar reverse transformation from proprietary brokerage format to common intermediate format is also performed for resulting response in connection to the original user activity request. In FIG. 5 when the brokerage service 550 informs the relaying gateway 500 of the order's execution or resulting status in response to user's activity request, the response is translated back into the common intermediate format and is relayed back to the access terminal client for display to the user.
[0045] Thus, the above disclosed configuration allows the user to use a single graphical user interface to communicate with multiple brokerage service firms that use various different protocols.
[0046] FIG. 2 shows an additional interface 260 connected to the determination unit 210 . The interface 260 allows the determination unit to be connected to an information server 264 over communications link 262 . The information server 264 provides information data to the determination unit such as financial news, brokerage firm information, and financial market values. The information provided by information server 264 is preferably in quantifiable numerical form, such as stock quotes, or price information about brokerage firm rates. An example of such an information server is any web-based stock tracker such as Google Finance or Yahoo Finance.
[0047] The determination unit 210 can utilize the information received from the information server in multiple ways. The determination unit can update the routing table 400 with an indication of a stock that is available on a particular market. Additionally, the determination unit 210 can have a triggering mechanism in which the change in price of a stock can trigger a buy or sell order if the stock reaches a certain price. The stock price that triggers such an action can be pre-programmed into the determination unit 210 by the user. When the determination unit 210 triggers such a buy or sell order it then generates an activity request as if the user had sent it. The activity request is then forwarded to the proper reformatting unit based on the route indicated in the routing table, which then forwards the activity request to the designated brokerage firm.
[0048] FIG. 6 illustrates a computer system 601 upon which the access client terminal 204 , the determination unit 210 , and the reformatting units 212 , 214 , and 216 of FIG. 2 may be implemented. The computer system 601 includes a bus 602 or other communication mechanism for communicating information, and a processor 603 coupled with the bus 602 for processing the information. The computer system 601 also includes a main memory 604 , such as a random access memory (RAM) or other dynamic storage device (e.g., dynamic RAM (DRAM), static RAM (SRAM), and synchronous DRAM (SDRAM)), coupled to the bus 602 for storing information and instructions to be executed by processor 603 . In addition, the main memory 604 may be used for storing temporary variables or other intermediate information during the execution of instructions by the processor 603 . The computer system 601 further includes a read only memory (ROM) 605 or other static storage device (e.g., programmable ROM (PROM), erasable PROM (EPROM), and electrically erasable PROM (EEPROM)) coupled to the bus 602 for storing static information and instructions for the processor 603 .
[0049] The computer system 601 also includes a disk controller 606 coupled to the bus 602 to control one or more storage devices for storing information and instructions, such as a magnetic hard disk 607 , and a removable media drive 608 (e.g., floppy disk drive, read-only compact disc drive, read/write compact disc drive, compact disc jukebox, tape drive, and removable magneto-optical drive). The storage devices may be added to the computer system 601 using an appropriate device interface (e.g., small computer system interface (SCSI), integrated device electronics (IDE), enhanced-IDE (E-IDE), direct memory access (DMA), or ultra-DMA).
[0050] The computer system 601 may also include special purpose logic devices (e.g., application specific integrated circuits (ASICs)) or configurable logic devices (e.g., simple programmable logic devices (SPLDs), complex programmable logic devices (CPLDs), and field programmable gate arrays (FPGAs)).
[0051] The computer system 601 may also include a display controller 609 coupled to the bus 602 to control a display 610 , such as a cathode ray tube (CRT), for displaying information to a computer user. The computer system includes input devices, such as a keyboard 611 and a pointing device 612 , for interacting with a computer user and providing information to the processor 603 . The pointing device 612 , for example, may be a mouse, a trackball, or a pointing stick for communicating direction information and command selections to the processor 603 and for controlling cursor movement on the display 610 . In addition, a printer may provide printed listings of data stored and/or generated by the computer system 601 .
[0052] The computer system 601 performs a portion or all of the processing steps of the invention in response to the processor 603 executing one or more sequences of one or more instructions contained in a memory, such as the main memory 604 . Such instructions may be read into the main memory 604 from another computer readable medium, such as a hard disk 607 or a removable media drive 608 . One or more processors in a multi-processing arrangement may also be employed to execute the sequences of instructions contained in main memory 604 . In alternative embodiments, hard-wired circuitry may be used in place of or in combination with software instructions. Thus, embodiments are not limited to any specific combination of hardware circuitry and software.
[0053] As stated above, the computer system 601 includes at least one computer readable medium or memory for holding instructions programmed according to the teachings of the invention and for containing data structures, tables, records, or other data described herein. Examples of computer readable media are compact discs, hard disks, floppy disks, tape, magneto-optical disks, PROMs (EPROM, EEPROM, flash EPROM), DRAM, SRAM, SDRAM, or any other magnetic medium, compact discs (e.g., CD-ROM), or any other optical medium, punch cards, paper tape, or other physical medium with patterns of holes, a carrier wave (described below), or any other medium from which a computer can read.
[0054] Stored on any one or on a combination of computer readable media, the present invention includes software for controlling the computer system 601 , for driving a device or devices for implementing the invention, and for enabling the computer system 601 to interact with a human user (e.g., print production personnel). Such software may include, but is not limited to, device drivers, operating systems, development tools, and applications software. Such computer readable media further includes the computer program product of the present invention for performing all or a portion (if processing is distributed) of the processing performed in implementing the invention.
[0055] The computer code devices of the present invention may be any interpretable or executable code mechanism, including but not limited to scripts, interpretable programs, dynamic link libraries (DLLs), Java classes, and complete executable programs. Moreover, parts of the processing of the present invention may be distributed for better performance, reliability, and/or cost.
[0056] The term “computer readable medium” as used herein refers to any medium that participates in providing instructions to the processor 603 for execution. A computer readable medium may take many forms, including but not limited to, non-volatile media, volatile media, and transmission media. Non-volatile media includes, for example, optical, magnetic disks, and magneto-optical disks, such as the hard disk 607 or the removable media drive 608 . Volatile media includes dynamic memory, such as the main memory 604 . Transmission media includes coaxial cables, copper wire and fiber optics, including the wires that make up the bus 602 . Transmission media also may also take the form of acoustic or light waves, such as those generated during radio wave and infrared data communications.
[0057] Various forms of computer readable media may be involved in carrying out one or more sequences of one or more instructions to processor 603 for execution. For example, the instructions may initially be carried on a magnetic disk of a remote computer. The remote computer can load the instructions for implementing all or a portion of the present invention remotely into a dynamic memory and send the instructions over a telephone line using a modem. A modem local to the computer system 601 may receive the data on the telephone line and use an infrared transmitter to convert the data to an infrared signal. An infrared detector coupled to the bus 602 can receive the data carried in the infrared signal and place the data on the bus 602 . The bus 602 carries the data to the main memory 604 , from which the processor 603 retrieves and executes the instructions. The instructions received by the main memory 604 may optionally be stored on storage device 607 or 608 either before or after execution by processor 603 .
[0058] The computer system 601 also includes a communication interface 613 coupled to the bus 602 . The communication interface 613 provides a two-way data communication coupling to a network link 614 that is connected to, for example, a local area network (LAN) 615 , or to another communications network 616 such as the Internet. For example, the communication interface 613 may be a network interface card to attach to any packet switched LAN. As another example, the communication interface 613 may be an asymmetrical digital subscriber line (ADSL) card, an integrated services digital network (ISDN) card or a modem to provide a data communication connection to a corresponding type of communications line. Wireless links may also be implemented. In any such implementation, the communication interface 613 sends and receives electrical, electromagnetic or optical signals that carry digital data streams representing various types of information.
[0059] The network link 614 typically provides data communication through one or more networks to other data devices. For example, the network link 614 may provide a connection to another computer through a local network 615 (e.g., a LAN) or through equipment operated by a service provider, which provides communication services through a communications network 616 . The local network 614 and the communications network 616 use, for example, electrical, electromagnetic, or optical signals that carry digital data streams, and the associated physical layer (e.g., CAT 5 cable, coaxial cable, optical fiber, etc). The signals through the various networks and the signals on the network link 614 and through the communication interface 613 , which carry the digital data to and from the computer system 601 maybe implemented in baseband signals, or carrier wave based signals. The baseband signals convey the digital data as unmodulated electrical pulses that are descriptive of a stream of digital data bits, where the term “bits” is to be construed broadly to mean symbol, where each symbol conveys at least one or more information bits. The digital data may also be used to modulate a carrier wave, such as with amplitude, phase and/or frequency shift keyed signals that are propagated over a conductive media, or transmitted as electromagnetic waves through a propagation medium. Thus, the digital data may be sent as unmodulated baseband data through a “wired” communication channel and/or sent within a predetermined frequency band, different than baseband, by modulating a carrier wave. The computer system 601 can transmit and receive data, including program code, through the network(s) 615 and 616 , the network link 614 and the communication interface 613 . Moreover, the network link 614 may provide a connection through a LAN 615 to a mobile device 617 such as a personal digital assistant (PDA) laptop computer, or cellular telephone.
[0060] In view of the wide variety of embodiments to which the principles of the present invention can be applied, it should be understood that the illustrated embodiments are exemplary only, and should not be taken as limiting the scope of the present invention. For example, the steps of the flow diagrams may be taken in sequences other than those described, and more or fewer elements may be used in the block diagrams.
[0061] While various elements of the preferred embodiments have been described as being implemented in software, in other embodiments hardware or firmware implementations may alternatively be used, and vice-versa. | A brokerage aggregation system, method and computer program for receiving an electronic message having at least one activity request directed to one or more brokerage service firms and outputting the activity request. The system includes an input interface configured to receive the electronic message in a first predetermined format, a plurality of output interfaces, each configured to connect to a corresponding brokerage service firm, and to transmit the at least one activity request in one of a plurality of second predetermined formats, wherein each of the plurality of second predetermined formats corresponds with a particular brokerage service firm, and a controller configured to receive and extract the at least one activity request from the electronic message, determine to which of the plurality of output interfaces the at least one activity request is to be transferred for subsequent transmission to a destination brokerage service firm, reformat the at least one activity request from the first predetermined format to the second predetermined format corresponding to the output interface previously determined, and transfer the at least one activity request after reformatting to the determined output interface for subsequent transmission to the destination brokerage service firm. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to method and apparatus for inspecting printed circuit boards, and more particularly to method and apparatus for detecting defective patters on printed circuit boards.
2. Description of the Prior Art
Generally, in production of a printed circuit board, the creation of defective patterns such as cut-offs, short-circuits, irregular thinnesses of projections in the circuit printing step may result in the formation of a defectivce circuit board which causes serious damage to its circuit property if the circuit board is etched without removing those defective patterns therefrom. Nowadays, most circuit boards are inspected via the naked eyes of inspectors before or after the etching step. However, it is inevitable that "naked eye" inspections are occasionaly faulty or uneven because there are human factors such as individual differences between the inspectors, and or fatigue.
There is already in existance an apparatus for automatically inspecting printed circuit boards, whose inspection method can roughly be classified into a mutual comparison method and feature extraction method.
The two methods are generally employed in processing image data scanned by a video camera or CCD line sensor. In the mutual comparison method, defects in the circuit pattern are detected by the logical subtraction of the scanned bit image of the circuit board under inspection from the normal bit image stored in a memory device. On the other hand, in the feature extraction method, the defect is detected by extracting the local image data from the whole scanned image data and analyzing the feature such as the width, the area, or the angle of the pattern under inspection or analyzing whether the pattern have certain characteristics.
The mutual comparison method has the following drawbacks. The method requires such a large capacity memory device that it increases production costs of the inspection system. Although defects in the pattern can be detected without concern of its type or shape, the circuit board to be inspected must be aligned in a predetermined location for accurate inspection. Defective patterns of a smaller size than the order of the board alignment error cannot be detected, and the alignment error sometimes generates a pseudo defect.
On the contrary, the feature extraction method does not have such severe board alignment requirements and has a greater capability of detecting small defects than the mutual comparison method. It is, however, impossible for this method to detect defects which have a similar shape to the normal pattern and which are located at a position where the shape must not exist. However, in the detection of defects having large size according to this method, the image processing becomes complicated, thus requiring a sophisticated image processing system, so that it is very difficult to reduce the price of the apparatus.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide method and apparatus for inspecting printed circuit boards capable of reducing the production cost.
It is a another object of the present invention to provide method and apparatus for inspecting printed circuits boards which will allow the reliable detection of defects in the printed circuit pattern.
In the present invention, both the feature extraction method and the mutual comparison method are employed. The image data of the printed circuit board under inspection is scanned, digitized and entered independently into the feature extraction process and the mutual comparison process. In the feature extraction process, local image data extracted from the digitized image data are examined to detect the pattern defects, while, in the mutual comparison process, the image data of the circuit board are compared with the image data scanned, digitized and stored prior to the inspection. The results from the two methods are combined to control certain output devices for displaying or marking the detected printed pattern defect.
According to one feature of the present invention, it is possible to improve the reliability of defect detection. The two complementary analysis methods compensate each other's drawbacks. Further, it is possible to detect defects including defective patterns having similar shape to the normal pattern and of smaller size than the order of board alignment error, or patterns located at a position where the pattern should not exist. Further, it is possible to reduce the pseudo defect detection due to the deviation of the board alignment.
According to another feature of the present invention, the resolution of the image data of the normal circuit pattern and the pattern to be inspected are reduced prior to the comparison in the mutual comparison process.
According to other features of the present invention, the memory capacity required for the storage of the image data of the normal circuit pattern or the pattern to be inspected is reduced, so that it is possible to reduce the production costs of the inspection apparatus.
BRIEF DESCRIPTION OF THE DRAWINGS
The objects and features of the present invention will become more apparent from a consideration of the following detailed description taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a block diagram showing the configuration of an apparatus for inspecting printed circuit board according to the present invention;
FIG. 2 is an explanatory drawing illustrating defective patterns which may appear on a printed circuit board;
FIGS. 3a to 3k are explanatory drawings illustrating the feature extraction method used in the present invention;
FIGS. 4a to 4c are explanatory drawings illustrating the mutual comparison method used in the present invention; and
FIG. 5 is a flow chart illustrating the operation and processing procedure in the apparatus as shown in FIG. 1.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
FIG. 1 is a block diagram showing a preferred embodiment of an inspection apparatus in accordance with this invention. In FIG. 1, reference numeral 2 denotes a CCD video camera for scanning a printed pattern on an printed circuit board 1, which is disposed on a table 1a for inspection prior to ( or after ) the etching process. The printed pattern is scanned as the camera 2 or the circuit board 1 moves. The camera 2 may be constructed as a two-dimensional photosensor for scanning two-dimensional image data.
The scanned image data from the camera 2 are converted into a black-and-white binary digital data by a binary digitizer 3 and then fed to two image data processors, which are a feature extraction processor 4 and a mutual comparison processor 7. In this embodiment, defects in the printed pattern are thus detected using the two processors by the feature extraction method as well as the mutual comparison method.
FIG. 2 shows typical defects 11 to 19 on the printed pattern, which are respectively an irregular thinness, a cutoff, a projection, a swelling of the pattern, an irregular vicinity of the patterns caused by the projection or the swelling, a short-circuit, a dot point isolated from the virtual pattern, a missing point or a pinhole in the pattern etc. The defects 11 to 19, whose sizes or dimensions are smaller than the positioning error of the circuit board 1, are detected by the feature extraction processor 4, while the defects of greater size or dimension than the positioning error are detected by the mutual comparison processor 7.
The detection output signals generated by the image data processors 4 and 7 are entered to a data processor 32. The data processor 32 is comprised of a processing circuit such as a microprocessor, and controls a CRT display 33 to display thereon the detected defective patterns or their coordinates, as well as a marking device 34 to mark the defect pattern on the circuit board 1. The processor 32 controls the display 33 and/or the marking device 34 by combining the output detection signals from the two image processors 4, 7 with predetermined logical criteria such as OR or AND condition.
The feature extraction processor 4 is structured as described below. The binary image data generated by the digitizer 3 are entered into a local image cutter 5 composed of shift registers. The image cutter 5 divides the scanned image comprised of a plurality of digitized image elements into a plurality of localized two-dimensional image segments each having a row-and-column matrix configuration in the form of a 7×7 picture or image element configuration as shown in FIG. 3a. Then the central 1 bit of image element and the peripheral circular or equi-angularly disposed 8 bits of image elements are extracted or selected as shown in FIG. 3b, and the extracted 9 bit image 20 is fed to a detecting processor 6.
The whole width of the 7×7 configuration of the picture elements is a little narrower than that of a lead (straight portion of the printed pattern) 21. The sum of the possible combination of the extracted or selected 9 bit black and white images is 512 (=2 9 ). All of the combinations can be divided into two categories or groups. One is composed of the bit patterns that may appear in the scanning of the normal circuit pattern and that indicate an absence of a pattern defect, and the other is composed of the bit patterns that must not appear in the normal circuit pattern and that indicate a presence of a pattern defect.
Accordingly, in this embodiment, a ROM is employed for the detecting processor 6 and the extracted 9 bit signal 20 is fed as an address input of the ROM, whose memory cell has `1` (normal) or `0` (defective) data or memory content corresponding to the its address input.
Even though the criteria that determines whether a pattern is normal or defective is different corresponding to the characteristics of the scanned pattern, the patterns are regarded as normal or defective as described below.
If the lead 21 is scanned as shown in FIG. 3c, the extracted 9 bit image data 20 are all black. The black and white patterns of the image data 20 shown in FIGS. 3d and 3e are allowed to appear when the camera 2 scans a border area of the lead 21 or a land 22.
On the other hand, FIGS. 3f, 3g and 3h show black and white patterns of extracted image data 20, which must not appear in the scanning of the normal printed pattern. FIGS. 3f to 3h show a black and white pattern extracted respectively from a irregular thinness (or vicinity) of the circuit pattern, from an irregular projection (or losing) of the circuit pattern and from an isolated pattern (or a pinhole). The above description in the parentheses denotes the defects which appear when the black and white bit pattern is reversed.
Thus, the circuit board can be inspected by reading out the memory content of the detecting processor (ROM) 6 in synchronism with the scanning of the circuit patterns. The experimental inspection showed that 70% of the defects can be detected using only the 9 bit image extraction method shown above.
In this embodiment, the detection processor 6 can be structured in a simple configuration, employing a ROM having at least 512 bits capacity, so that the production cost can be reduced, and the defect detection can be made with very simple programming which in turn enables very fast processing speed.
Various alternative arrangements may be made for the feature extraction processor 4. For example, 8 bits of outer picture or image elements can be added around the 9 bits of inner image elements as the input image data as shown in FIGS. 3i, 3j, in order to increase the detection area. FIGS. 3i and 3j respectively show the detection of the large projection and isolated pattern. The detection area can be increased to as broad as a 25 bit area as shown in FIG. 3k.
Most of the relatively small defective patterns on the circuit board can be detected using the feature extraction method without any pseudo defect detection.
The mutual comparison processor 7 is constructed as described below.
Generally in the mutual comparison method, all of the scanned image data are memorized and the scanned image is compared with the stored image data of the normal or master pattern.
However, if a picture element taken by the CCD of the camera 2 corresponds to a 30×30 micron area, the memory capacity required for the storage of the 500×500 mm board image becomes as great as 32 megabytes (=500×10 3 /30) 2 .
In this embodiment, the resolution of the stored normal image data and scanned image data is reduced by a filter 8, in order to make the memory capacity requirement smaller. The filter 8 reduces the resolution of both sample and master pattern image data, for example, to 1/2 of the resolution of the CCD of the camera 2 with respect to the length of the CCD (to 1/4 with respect to the area of the CCD).
With this resolution reduction, the memory capacity for normal image data can be reduced to 1/4. In the above referred instance, the 32 megabyte memory capacity requirement can be reduced to 8 megabytes.
The scanned binary image data from the digitizer 3, with their resolution low-resolution reduced by the filter 8 are compared (subtracted) by the comparator 31 with the normal image data prepared in the memory 9. The normal image data fed into the comparator 31 are enlarged or compacted by the scale changing circuit 10.
The purpose of the scale change is to reduce the pseudo defect detection, which often occurs under the condition that the circuit board 1 is disposed with some alignment error.
Assume that the printed pattern 40 under inspection has a projected portion 14, or a lost portion 18 as shown in FIG. 4a. The lost or indent portion 18 can be detected if the normal image data are compacted or similarly reduced as shown in FIG. 4b, while the projected portion 14 can be detected if the normal image data is enlarged as shown in FIG. 4c. If the scanned image data are compared both with the enlarged and the compacted pattern, both of the projected and lost portions can be detected.
With the change of the scale, up to 100 microns of alignment error of the circuit board 1 can be allowed, where 1 bit data of the memory 9 correspond to the 60×60 micron picture element.
The results of the feature extraction and the mutual comparison are combined as described below.
FIG. 5 is a flow chart showing procedures of the operator and the image data processing of the apparatus.
First of all, in step S1 of FIG. 5, a printed circuit board having normal printed pattern is mounted on the inspection table 1a. The normal circuit board is inspected via naked eyes of the inspector prior to this step. In step S2, the board is brought into alignment with the determined position using a positioning device such as a guide plate or grooves.
In step S3, the scanning conditions including the scanning area of the camera 2, the illumination light value or the threshold value of the binary digitizer 3 are determined. The light value and the threshold value are determined by a conventional method using a reference white surface.
The image data of the normal pattern are scanned in step S4, digitized by the digitizer 3, reduced in resolution and then stored in the memory 9 in step S5.
In step S6, the circuit board with the normal pattern on the table 1a is substituted with a sample board to be inspected.
In step S7, it is determined how the inspection result should be utilized. The result output using the CRT display 33 or marking device 34 can be selected via an input device such as a keyboard (not shown in the drawings). In the illustrated embodiment, the coordinates of the defect can be displayed on the CRT display 33, or the defect can be marked by the marking device 34.
In step S8, the circuit board (in the pre- or post-etching process) is brought into alignment with the determined position, and scanned by the camera 2 with the same scanning condition utilized in the scanning of the normal board.
In steps S10 and S11, the scanned and digitized image data are entered into image processors 4 and 7, where both the feature extraction process and the mutual comparison process are simultaneously carried out.
The results of the feature extraction and the mutual comparison are entered into the data processor 32, and combined with a certain logical condition such as OR or AND in step S12. The processor 32 converts the combined result into the acceptable data by the CRT display 33 or the marking device 34.
In step S13, the processor 32 judges whether a defect exists or not. In case of no defect, the result is displayed on the CRT display in step S14. If some defect is detected, the result is fed to the display 33 or the marking device 34 according to the selection made in step S7.
Thus, in the illustrated embodiment, both the feature extraction and the mutual comparison method are employed, so that it is possible to detect the defects, including defects having a certain shape or size smaller than the order of the board alignment error, which could not be detected in conventional apparatus using only one of the detection methods. The filter and the scale changing circuit solve, respectively the two major drawbacks of the mutual comparison method namely, the large capacity memory requirement and the detection of pseudo defects caused by alignment error. The combination of the two methods allows the detection of defects having an indetectable shape.
While the invention 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 invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention should not be limited to the particular embodiment disclosed as the best mode contemplated for carrying out the invention, but that the invention will include all embodiments falling within the scope of the appended claims. | Method and apparatus for inspecting a printed circuit board wherein scanned image data are digitized and analyzed according to a feature extraction method and a mutual comparison method. The result of both of the analysis methods is combined with predetermined conditions to control output devices including a CRT display or a marking device. The two complementary methods compensate each others drawbacks so that the reliability of inspection can be improved. | 6 |
BACKGROUND AND SUMMARY OF THE INVENTION
The present invention relates to topical compositions comprising ozonizing compounds derived from ozonolysis of fixed oils and unsaturated esters, alcohols, ethers and fatty acids. More particularly, the invention relates to compositions containing ozonized oil-soluble materials and the use of such compositions for the effective, nonirritating treatment of acne.
Acne is a condition of the human skin that affects many adolescents beginning about twelve years of age and continuing through the age of 25 years. During adolescence, the sebaceous glands enlarge, due to a hormonal stimulus, and increased sebum is produced and secreted on the skin. When the ducts through which the sebum flows are obstructed due to hyperkeratinization, a thickening and solidification of the sebum occurs, forming a solid plug known as a comedone. These lesions may eventuate to papules which in turn may evolve into pustules or deeper nodules which enlarge into cysts. The microorganism within the follicle of the skin is propionibacterium acnes, hereinafter referred to as P. acne. This microorganism produces an enzyme, lipase, which hydrolyzes triglycerides in the sebum to form free fatty acids which are responsible for the comedone formation. Acne is characterized by the presence of comedones, inflammatory papules, pustules or cysts, and the effects range from slight skin irritation to pitting and disfiguring scars.
Many compounds and compositions have been tested and prescribed for treatment of acne. A number of them have been fairly effective, but no complete cure for acne is presently available. The concept of the use of nascent or active oxygen to kill the anaerobic P. acne microorganism was introduced with the use of benzoyl peroxide. Such methods are described, for example, in the following U.S. patents: U.S. Pat. No. 3,535,422 to Cox et al; U.S. Pat. No. 4,056,611 to Young; U.S. Pat. No. 4,163,800 to Wickett et al; and U.S. Pat. No. 4,189,501 to Fulton.
However, the use of benzoyl peroxide is known to cause dryness and exfoliation, both of which are undesirable, particularly for teenagers and young adults.
By the present invention, there are provided therapeutic compositions for the treatment of acne, including the use of stable, ozonized oil-soluble compounds having the ability to penetrate the comedone and deliver nascent oxygen directly to the anaerobic P. acne microorganisms without the characteristic dryness and skin irritation which have been associated with the use of peroxide compounds.
The ozonolysis of oil-soluble compounds is well known in the art, being disclosed, for example, in the following U.S. patents: U.S. Pat. No. 925,590 to Neel; U.S. Pat. No. 984,722 to Twombly; U.S. Pat. No. 1,081,617 to Know; U.S. Pat. No. 2,083,572 to McKee; U.S. Pat. No. 2,897,231 to Niegowiski; U.S. Pat. No. 3,083,209 to Habib et al; and U.S. Pat. No. 3,145,217 to Horeczy et al.
The use of ozonized materials in formulations for medicinal purposes is disclosed in U.S. Pat. No. 1,210,949 to Knox and U.S. Pat. No. 2,356,062 to Johnson. Ozonized materials herein referred to as ozonides or ozonide compounds have been employed in the past for such uses as antiseptics, deodorizing agents and for treatment of dermatitis, inflammation of the nose and throat and for vaginal conditions. No method has been previously known, however, for the treatment of a skin disease, such as acne, by the use of ozonide compounds. Thus, the only method currently known for the treatment of acne utilizing the concept of the release of nascent oxygen for killing the anaerobic P. acne organisms is by the use of the peroxide compounds. However, due to the fact that such peroxide compounds are water-insoluble and cause skin irritation as previously discussed, it would be highly advantageous to employ an alternate method in which the nascent oxygen is released, without causing primary skin irritation such as is frequently experienced in the use of peroxide compounds.
The present invention provides just such an improved method for the treatment of acne, utilizing oil-soluble ozonides which have been found to demonstrate excellent characteristics in the killing of anaerobic P. acne, the organism active in the acne condition, by the release of nascent or active oxygen. The present invention is particularly beneficial, since the ozonide compositions have the capability to deliver nascent oxygen deep within the lesion where the infection exists, without causing primary skin irritation. The compositions of the present invention are applied topically to the afflicted area to release nascent oxygen. The ozonides are miscible with many organic cosmetic based materials, thus facilitating the incorporation of the ozonides into an elegant compound which is invisible on the skin during use. In one aspect of the invention, the ozonides are produced by the use of oxygen having a high degree of purity, thus eliminating the possibility of contamination of the ozone with nitrogen and other extraneous elements.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The compositions of the present invention must contain sufficient ozonide to be therapeutically effective while providing a cosmetically acceptable nonirritating treatment for acne. This composition provides oil-soluble ozonides in a formulation to provide a sustained release of nascent oxygen which is bacteriocidal to P. acne. A major requirement of the compositions is that the ozonide-containing preparations may be of many types, but must be nonirritating and cosmetically acceptable. This invention satisfies the above criteria by providing a topical, nonirritating acne treatment comprising a cosmetically acceptable base combined with at least one oil-soluble ozonide.
Any base material employed for the final product must be cosmetically acceptable and also must be nonirritating. The cosmetically acceptable base may, for example, be composed of a material such as: an ester such as isopropyl myristate, isopropyl palmitate, butyl stearate or propylene glycol dipelargenate; paraffin oils and waxes; animal and vegetable oils including coconut oil and derivatives, palm oil, corn oil and the like; lanolin derivatives; fatty alcohols such as isostearyl alcohol and straight chain alcohols containing from 6 to 18 carbon atoms; certain petroleum distillates which are toxicologically safe such as isoparaffin hydrocarbon solvents containing from 8 to 18 carbon atoms; and silicone fluids and waxes including the volatile silicones.
As the solvent component for the ozonide formulation, there may be employed the following; polyols such as propylene glycol; glycerine and alcohols such as anhydrous ethanol and isopropyl alcohol; other solvents such as acetone, and chlorinated solvents such as methylene chloride can be used in this invention if desired. A surface active agent such as an ethyoxylated fatty alcohol, a polyglycerol fatty ester or a sorbitan ester may also be used. Other commonly used formulation ingredients to improve cosmetic acceptability may be used, including fragrances and essential oils, preservatives, opacifiers, titanium dioxide, zinc oxide and similar materials. The formulation materials mentioned in this list are merely examples and are not intended to limit the invention in any way. In general, any non-aqueous material or mixtures thereof which are toxicologically safe for human use and are non-comedogenic in the concentrations used may be used as the carrier for the ozonide.
The ozonides employed in the present invention may be prepared by the Harries Ozonide Reaction with the basic reaction being described, for example, in U.S. Pat. No. 984,722 to Twombly; U.S. Pat. No. 2,083,572 to McKee and U.S. Pat. No. 2,356,062 to Johnson, all of which are incorporated herein by reference. The preparation of ozonides by the Harries Ozonide Reaction is well documented in the literature, being described, for example, in the Merck Index, 8th Edition, p. 1174, Section of Named Reactions. As stated in these references, the reaction can be carried out by treating the olefinic substrate with gaseous ozone. This is accomplished, for example, by sparging the olefin with ozone-laden oxygen. Basically, this reaction involves the treatment of an olefin with ozone to form an ozonide according to the following sequence: ##STR1##
In general, any olefin can be so treated with gaseous ozone to form an ozonide. In order to be acceptable as an ingredient in the formulations described herein, the olefin should be nontoxic and cosmetically acceptable. The reaction products, upon hydrolysis of the ozonide on the skin, should likewise not produce toxic or skin-irritating substances. Examples of olefins that are acceptable for the production of ozonides to be employed in the present invention include fixed oils such as corn, olive, castor, sesame, jojoba and similar oils containing olefinic linkages. Other olefinic materials including fatty acids such as oleic acid, linoleic acid or elaidic acid and fatty alcohols such as oleyl alcohol can be ozonized to produce ozonides that are useful as active ingredients in the acne preparations herein described.
The ozonide used as the antibacterial preparation in this invention can be derived from fixed oils and unsaturated esters, alcohols, ethers and fatty acids olefins moeities of the general formula: ##STR2## where for example R 3 and/or R 4 may be hydrogen (H) or: ##STR3## where R 5 =(CH 2 ) n -CH 3 and
n=an integer from 0 to 12.
NOTE: R 1 and R 2 can be any value given for R 3 and R 4 except that R 1 and R 2 cannot both equal H; also R 3 and R 4 cannot both equal H.
The compositions employed in the present invention may contain about 5 to 100% by weight of the ozonide. The active oxygen content in the compositions should be in the range from about 0.1% to about 15%, preferably from about 0.2 to about 2%, by weight of the ozonide component.
The amount of active oxygen that can be attached to a compound depends on the number of free double bonds available. The amount may generally range from 0% by weight to about 18% by weight of the compound. Thus, for example, as a sample of olive oil is ozonized, the olive oil will gain weight as the reaction proceeds. This increase in weight is due to the ozone absorbed by the olive oil. Olive oil, for example, can react with about 17 grams of ozone per 100 grams of oil. Of the 17 grams, approximately 1/3 or 5.7 grams is nascent or active oxygen. The maximum capacity of other olefins for absorbing ozone will in general depend on the amount of unsaturation contained in the molecule. For example, 2-butene theoretically will react with 82 grams of ozone per 100 grams of 2-butene and the active oxygen content would be about 27 weight % of the initial 82 grams.
It should be noted that a composition of the present invention for treating acne containing 1% by weight of active oxygen in the ozonide component could, for example, be prepared from ozonized 2-butene or olive oil that had been ozonized to a level greater than 1% by weight active oxygen. The procedure would involve simple dilution of these or any of the other above mentioned ozonides to the desired level with unozonized olefinic materials.
The compositions containing these ozonide preparations can be varied to produce a wide variety of finished products. Pomades, sticks, anhydrous creams, solutions, powders and gels are easily formulated by those experienced in the art. One olefin substrate that has been ozonized for medicinal use in olive oil. This fixed oil contains unsaturation that is readily transformed into ozonides by reacting it with ozone. Olive oil will react with ozone, forming ozonide at room temperature in a mildly exothermic reaction. As the olefinic groups are ozonized, the viscosity increases.
The acne treatment compositions of the invention may be further illustrated by the following nonlimiting examples:
EXAMPLE 1
A quantity of virgin Spanish olive oil was added to a gas washing bottle equipped with a fritted glass sparger. Medical grade oxygen was passed through a Union Carbide Ozonizer at 15 psig and a flow rate of 0.5 cu. ft./min. After a predetermined time, the olive oil samples showed a weight gain due to the reaction of ozone and the olefinic groups present in the oil being treated. The oxygen content of various samples was determined by the increase in weight to be from 1.94% to 8.27% by weight after ozonizing. Various ozonide samples were tested by chemical analysis and found to have active oxygen contents ranging from 0.35% to 1.58% by weight.
The ozonide products were subjected to microbiological testing using the organism P. acne under anaerobic atmospheric conditions. A 1/4 inch antibiotic assay disc was placed on the inoculated Brain Heart Infusion (BHI) agar surface and 20 μl of product was delivered on the disc. After 48 hours incubation, the zone of bacteriocidal activity correlated well with the concentration of the test material. Nascent oxygen was released from the olive oil, diffused into the agar and was bacteriocidal to P. acne at all concentrations, greatest at the higher concentration of active ingredient. Further testing showed the olive oil ozonide to be noncomedogenic. This was an unexpected result due to the oily nature of the material. This ozonide without further modification was found to be non-irritating when applied to the skin. It is easily applied to acne lesions leaving an acceptable invisible film of ozonide. The active oxygen content of this formulation may be altered by either continuing the ozonizing to raise the active oxygen content or the oxygen content can be lowered by simple dilution with virgin Spanish olive oil or other suitable diluents.
Various other samples of olive, jojoba, sesame, castor and peanut oils were also ozonized as outlined above.
EXAMPLE 2
In this formulation, the solvency of acetone that is commonly used in acne preparations is incorporated into the ozonide-containing formula.
______________________________________Ingredient Parts By Weight______________________________________Olive Oil Ozonide 15.0Acetone 15.0Dow Corning #344 Silicone Fluid 68.8(Polydimethylcyclosiloxane)Menthol 0.2______________________________________
The resultant clear solution is cosmetically elegant and can be applied with the fingers or various types of applicators. Alternatively it could be conveniently packaged on towlette material in a foil package.
EXAMPLE 3
______________________________________Ingredient Parts By Weight______________________________________Olive Oil Ozonide 20.0Isopropyl Palmitate 15.0Isopropyl Alcohol 64.5Menthol 0.5______________________________________
This example demonstrates an alcohol-containing, elegant, invisible composition that can be applied as in Example 2.
The following formulations are liquids suitable for application with sponge-type or roll-on applicators.
EXAMPLE 4
______________________________________Weight % Ingredient______________________________________33% C.sub.12-15 Alcohols Benzoate (Finetex)13% Ozonized Olive Oil54% 344 Silicone Fluid (Dow Corning)______________________________________
EXAMPLE 5
______________________________________Weight % Ingredient______________________________________25% Robane (Squalane)25% Ozonized Sesame Oil50% Acetone______________________________________
EXAMPLE 6
______________________________________Weight % Ingredient______________________________________35% Neobee M-5 (vegetable triglycerides)20% Ozonized Peanut Oil45% 345 Silicone Fluid (Dow Corning)______________________________________
EXAMPLE 7
______________________________________Weight % Ingredient______________________________________10% Ozonized Peanut Oil60% Acetone30% Robane (Squalane)______________________________________
The following formulation is a gel suitable for packaging in a jar or in the above applicators.
EXAMPLE 8
______________________________________Weight % Ingredient______________________________________10% Synthetic Silica (Silicone Dioxide)50% Mineral Oil, Light15% 344 Silicone Fluid50% Ozonized Olive Oil20% C.sub.12-15 Alcohols Benzoate______________________________________
The composition is applied topically to the skin of the patient by rubbing the ozonized product onto the areas being treated, one or more times daily. It should be therapeutically effective and cosmetically acceptable without skin irritation.
From the foregoing description of the present composition and method for the treatment of acne, it can be seen that the present invention provides an important contribution to the art to which the invention relates.
The invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. | A composition and method for the effective, nonirritating treatment of acne is disclosed. The method includes treatment of the affected area by topical application of an ozonized material derived by ozonizing various fixed oils and unsaturated esters, alcohols, ethers and fatty acids. The ozonized materials of the present invention have the ability to penetrate the comedone and deliver nascent oxygen directly to the acne microorganisms without the characteristic dryness and skin irritation associated with previous methods of acne treatment. | 8 |
CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims the priority right from the German patent application DE 102008063385.2 that was filed on Dec. 30, 2008, the content of which is herewith incorporated in its entirety by reference.
BACKGROUND OF THE INVENTION
[0002] The invention relates to clutch support for supporting a clutch hub of a clutch such that the clutch hub is rotatable, comprising a flange that is fixable at a clutch housing or the like, the clutch support comprising a substantially cylindrical element for receiving the clutch hub in a rotatable manner and comprising a sleeve with at least one groove formed therein for providing at least one channel that allows oil to be supplied to the clutch through this channel.
[0003] From the WO 2007/051627 A1 a clutch support is known supporting a rotatably mounted clutch hub of a clutch that comprises two friction clutches that can be actuated independently from each other. The friction clutches are so-called wet clutches requiring that both friction clutches are supplied with oil. The two friction clutches are actuated hydraulically. Therefore, in addition to supplying oil for cooling, the friction clutches have to be provided with pressurized hydraulic oil for actuating the friction clutches.
[0004] The clutch support of WO 2007/051627 A1 does not only support the clutch hub, but also supplies oil via the clutch hub to the friction clutches. For this purpose, the clutch support comprises a cylindrical element that is provided with a plurality of ring-shaped grooves. The ring-shaped grooves are in contact with different channels that are provided by grooves formed in a sleeve of the clutch support. The structure of this sleeve is relatively complex since separate channels that are separated from each other have to be formed within the sleeve for allowing to pressurize the two friction clutches independently from each other and independently from the cooling oil flow with pressurized hydraulic oil.
[0005] Due to the complex structure, the clutch support can only be manufactured at high cost. For example, for manufacturing of the sleeve, a forged blank has to be processed further by chip removing machining such as turning, milling, precision turning and grinding. This plurality of manufacturing steps in manufacturing the clutch support is very cost intensive.
SUMMARY OF THE INVENTION
[0006] It is therefore an object of the invention to provide a clutch support that can be manufactured in a simple manner and at comparatively low cost.
[0007] This object is achieved according to the invention by a clutch support for supporting a clutch hub of a clutch such that the clutch hub is rotatable, comprising a flange that is fixable at a clutch housing or the like; a substantially cylindrical element for receiving the clutch hub such that the clutch hub is rotatable; and a sleeve with at least one groove formed therein for providing at least one channel that allows oil to be supplied to the clutch through this channel; wherein the sleeve is manufactured substantially without any chip removing chip removing machining action.
DETAILED DESCRIPTION OF THE INVENTION
[0008] The clutch support according to the invention is characterized in that the sleeve is manufactured substantially without any chip removing machining action. The sleeve presses according to a preferred embodiment against the inner wall of the cylindrical element by a press fit and can be manufactured from at least one strip material that is rolled cylindrically or curled. In addition to the press fit also other options for connecting the sleeve with the cylindrical element are possible (for instance gluing).
[0009] The strip material may comprise such a length that it comprises in its cylindrically rolled state a diameter that matches the desired diameter of the sleeve, wherein the two ends of the curled strip material form a seam with each other that is either gap free or comprises a small gap and extends in axial direction of the sleeve. In this case, only one axial seam results from the curling process. However, it is also possible that the sleeve is formed by two half-shells manufactured by curling. In this case, the sleeve comprises two axial seams that are offset in a circumferential direction by 180 degrees if both half-shells are of the same size.
[0010] A connection between the two opposing ends of the curled strip material along the seam is not absolutely necessary if the sleeve attaches to the inner wall of the cylindrical element of the clutch support by a press fit. In this case, the seam is a simple butt joint where due to the rigid press fit of the sleeve within the cylindrical element the ends of the curled strip material cannot separate from each other.
[0011] According to a preferred embodiment, the two ends of the curled strip material are connected to each other along the seam. One preferred option is that one end of the curled strip material comprises at least one undercut portion while the other end comprises a recess portion matching the undercut portion, and the interlocking between the undercut portion and the recess receiving the undercut portion provides a positive interlocking in a circumferential direction. The undercut portion can for example be dovetail shaped, so that a dovetail connection between the ends of the curled strip material is created. Along the seam a plurality of undercut portions can be provided so that over the entire length of the sleeve a rigid connection between the opposing ends of the curled strip material is created.
[0012] Another option is that the opposing ends of the curled strip material are glued to each other or welded together. In the latter case, a finishing treatment of the weld seam maybe necessary if the sleeve has to rest against the inner wall of the cylindrical element in a flush or sealing manner. Such finishing treatment may comprise chip removing machining (such as for instance grinding). A clutch support having such a weld seam that was subjected to a finishing treatment should nevertheless be covered by the scope of protection claimed in claim 1 since the major shape of the sleeve comprising the formed-in grooves was manufactured without any chip removing machining steps and not by the finishing treatment.
[0013] The seam might extend along the bottom of the groove so that a weld seam connecting the ends of the curled material is positioned within the groove. If the groove extends over the entire axial length of the sleeve, no finishing treatment of the weld seam is necessary for securing that the sleeve with its outer circumferential face rests against the inner wall of the cylindrical element in a flush and sealing manner since the weld seam is offset towards the inside within the groove.
[0014] The sleeve may comprise an outer sleeve and an inner sleeve, wherein the outer sleeve and/or the inner sleeve is provided with punch outs for forming at least one groove. If for instance the outer sleeve comprises an elongated punch out, while the inner sleeve comprises a continuous circumferential face, in the assembled position of the sleeve a channel is formed between the inner wall of the cylindrical element and the inner sleeve of the sleeve.
[0015] The outer sleeve and inner sleeve can be interconnected by means of a press fit. Another preferred embodiment is that the inner sleeve and the outer sleeve are glued together. Also other connections are possible (for example welding).
[0016] For simple manufacturing of the outer sleeve, at first portions are punched out from the plane strip material. Thereafter, the outer sleeve is curled such as to receive its cylindrical shape.
[0017] The sleeve may also be integrally formed. For this purpose, parts of the strip material can be deep-drawn such that recesses or grooves are formed into the sleeve. After the deep drawing process the deep-drawn strip material is curled into a sleeve. One preferred alternative is hydroforming allowing to manufacture the outline of the sleeve from the strip material (sheet material) and curling it thereafter.
[0018] Hydroforming may also be applied to a sheet material having a thin wall so that a seamless sleeve may be manufactured directly.
[0019] In the alternative, the sleeve may also be manufactured as an injection molded part or a molded part. Preferred embodiments are made from plastic or aluminum (aluminum diecasting).
[0020] The flange and the cylindrical element of the clutch support may be manufactured separately and interconnected with each other along a seam. The connection at the seam location may for instance be achieved by gluing or creating a weld seam. It is further possible to interconnect the flange and the cylindrical element via a press fit with each other.
[0021] The flange and/or the cylindrical element can also be manufactured without chip removing machining. For example, the cylindrical element may be a tube having a thin wall that has been curled from a strip material.
[0022] The sleeve, the flange and/or the cylindrical element may also be subjected to a finishing treatment in the form of chip removing machining. This finishing treatment allows to remove sharp edges, but the overall manufacturing of these parts is still deemed to be in a non-machining fashion since it does not change the shape of the individual component parts in any substantial manner.
[0023] The invention is described in the following in more detail by referring to the embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
[0024] In the drawings show:
[0025] FIG. 1 a longitudinal section of an embodiment of the clutch support according to the present invention;
[0026] FIG. 2 a perspective view of a sleeve of the clutch support according to a first embodiment; and
[0027] FIG. 3 a sleeve of a clutch support according to a second embodiment of the present invention.
DETAILED DESCRIPTION OF THE DRAWINGS
[0028] FIG. 1 shows a clutch support that is denoted by reference numeral 1 in its entirety. The clutch support 1 provides a bearing so as to rotatably support a clutch hub of a clutch. The clutch hub as well as the clutch are not shown in FIG. 1 . Further, the clutch support 1 provides oil lubrication for the clutch.
[0029] The clutch is designed as a dual clutch comprising two friction clutches. The friction clutches can be actuated hydraulically and independently from each other. Further, the friction clutches are wet clutches that are cooled with oil.
[0030] The clutch support 1 comprises a flange 20 , a cylindrical element 40 and a sleeve 60 that is flush with an inner cylindrical wall 41 of the cylindrical element 40 . The flange 20 and the cylindrical element 40 are integrally formed. The non-shown clutch hub is supported on the cylindrical element 40 via a radial needle bearing 42 , and the clutch hub can be rotated around a rotational axis 2 . On its outer side 43 the cylindrical element 40 comprises ring-shaped grooves as 44 a to 44 d that are connected via holes 45 with the various grooves or recesses 61 in the sleeve 60 . The grooves 61 are in connection with oil feeding lines, one of which has been shown in FIG. 1 and denoted with reference numeral 21 . The flange 20 does in addition to having the function of securing oil feeding also have the function of fixing the clutch support 1 and a clutch housing or the like.
[0031] The various ring-shaped grooves 44 a to 44 d are in the assembled state of the clutches connected to channels in the non-shown clutch hub. Seals 46 provided between the ring-shaped grooves 44 a to 44 c are sealing the ring-shaped grooves with respect to each other. While via two of the four ring-shaped grooves clutch actuating cylinders of the clutch are subjected to pressurized oil, the other two ring-shaped grooves are provided for cooling the friction clutches of the clutch with oil.
[0032] As already discussed, the sleeve 60 is in contact with the inner cylindrical wall 41 of the cylindrical element 40 in a flush manner. The various grooves 61 in the sleeve 60 do therefore form in connection with the inner wall 21 a plurality of channels between the sleeve 60 and the cylindrical element 40 , allowing oil to be fed through the oil feeding lines 21 into the ring-shaped grooves 44 a to 44 d.
[0033] FIG. 1 shows at the cylindrical inner wall 22 of the flange 20 a further radial needle bearing 23 supporting a here non-shown shaft connecting the clutch with a transmission.
[0034] The FIGS. 2 and 3 show a perspective view of different embodiments of the sleeve 60 resting against the inner wall 41 of the cylindrical element 40 .
[0035] The sleeve shown in FIG. 2 , also denoted with reference numeral 60 , comprises an outer sleeve 62 and an inner sleeve 63 . The outer sleeve 62 as well as the inner sleeve 63 are manufactured from a plane strip material that was bent by a curling for forming the cylindrical shape of the sleeves 62 , 63 . The outer sleeve 62 comprises a plurality of punch outs 64 a , 64 and 64 c that have been punched out from the plane strip material prior to the curling process. When the sleeves are stuck together as shown in FIG. 2 , for instance the punch out 64 a forms in connection with the inner sleeve 63 grooves 61 a, wherein the groove bottom 65 is formed by the outer cylindrical face 66 of the sleeve 63 . The lateral groove walls 66 , 67 are formed by punched out edges that have been created due to punching out the punch out 64 a in the outer sleeve 62 .
[0036] The punch outs 64 a , 64 b , 64 c are provided at the circumference of the outer sleeve 62 and spaced apart from each other and comprise different axial lengths. Therefore, it is possible to create the desired channels between a particular one of the oil supply lines 21 and a particular one of the holes 45 at the outer face of the cylindrical element 40 .
[0037] FIG. 3 shows a sleeve 60 that is integrally formed. The sleeve 60 according to FIG. 3 is also made from a strip material that has been curled for creating the basic cylindrical shape. Prior to the curling process the strip material has been subjected to a deep drawing process for creating deep-drawn recesses 68 a , 68 b and 68 c in the material of the sleeve 60 . These deep-drawn recesses 68 provide the grooves 61 that form in connection with the inner face 41 of the cylindrical element 40 the channels for the oil supply.
LIST OF REFERENCE NUMERALS
[0000]
1 clutch support
2 rotational axis
20 flange
21 oil supply lines
22 inner face
23 radial needle bearing
40 cylindrical element
41 inner wall
42 radial needle bearing
43 outer face
44 ring-shaped groove
45 hole
46 seal
60 sleeve
61 groove
62 outer sleeve
63 inner sleeve
64 punch out
65 groove bottom
66 edge
67 edge
68 deep-drawn recess | A clutch support for supporting a clutch hub of a clutch such that the clutch hub is rotatable is described. The clutch hub comprises a flange that is fixable at clutch housing or the like; a substantially cylindrical element for receiving the clutch hub such that the clutch hub is rotatable; and a sleeve with at least one groove formed therein for providing at least one channel that allows oil to be supplied to the clutch through this channel. The sleeve is manufactured substantially without any chip removing machining action. This achieves the goal to provide a clutch support that can be manufactured in a simple manner and at comparatively low cost. | 5 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is related to the commonly assigned application filed contemporaneously herewith and entitled: AIR BAG CHUTE SEAL, U.S. Ser. No. 12/404,410.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the field of air bag deployment systems for an automotive vehicle and more particularly to the area of an air bag chute structure.
2. Description of the Related Art
In this technology field, there have been several methods of providing attachment of a passenger air bag chute to a vehicle interior panel. In cases where there is a foam-in-place process used to provide the foam layer between the air bag deployment door of a chute that is mounted on the instrument panel substrate and the outer skin layer, a seal element is typically employed to prevent leakage of the foam material during the process. In addition, the air bag chute is typically clamped in place to the instrument panel substrate by the use of screws or bolts.
U.S. Pat. No. 6,644,685 describes an air bag chute with a base reinforcement portion that surrounds a deployment door. When foam is injected as a liquid between the instrument panel substrate and the outer skin, a gasket or adhesive tape is described as being used to prevent leakage of the liquid foam from gaps formed between the reinforcement portion and the substrate. In the disclosed configuration, the adhesive tape layer is placed over the door panel and has its hinge edge clamped against the chute support structure with fasteners such as bolts. The entire air bag chute structure is attached to the instrument panel substrate by the use of fasteners which extend through an outer compression frame, the adhesive layer, the instrument panel substrate and the upper flange of the air bag support frame.
U.S. Pat. No. 6,709,007 describes an embodiment of an air bag deployment chute attached to the substrate of an instrument panel with bolts. A layer of masking tape or a die cut polymer with an adhesive on each surface is applied between the reinforcing ring and the instrument panel substrate to prevent the foam from penetrating between those elements.
U.S. Pat. No. 6,716,519 shows the use of a urethane sealing layer to prevent foam migration through mating lower surface of an air bag chute flange against the upper surface of an instrument panel substrate. The air bag chute is an integrated molding that attaches to the instrument panel substrate in a generally flush manner.
U.S. Pat. No. 7,237,797 shows the use of a masking tape sealing layer to prevent foam migration through mating surfaces on the instrument panel. The tape is folded over the edge of the door panel and the air bag chute frame to keep the door in the closed position. Studs and nuts are used to attach the air bag chute to the instrument panel substrate.
SUMMARY OF THE INVENTION
The inventive concept is directed to an improved method and apparatus, for use in an air bag deployment system that includes an air bag deployment chute formed to have an encircling flange member that seals itself against the upper surface of an instrument panel substrate to prevent foam migration during the foam-in-place injection process. The air bag chute structure is configured with a plurality of elements that interlock with the edge of the substrate aperture during installation of the chute into the aperture. The interlocking elements serve to retain the chute in place. One interlocking element is an elongated single tab (or series of tabs) that defines a slot beneath the flange on a first side wall of the chute skirt to capture the edge of an air bag aperture formed in the instrument panel substrate when the chute structure is inserted into the aperture. A series of indentations on the opposite side wall of the air bag chute skirt reside below the flange and are disposed to catch corresponding tab elements protruding from the instrument panel aperture as the air bag chute becomes fully inserted into the aperture. Flexible gussets that function to support the flange on the other two side walls of the air bag chute skirt contain notches that engage the instrument panel substrate when it is fully engaged into the aperture.
The inventive concept includes an integrated air bag deployment chute structure with a support base for attachment to an opening in a vehicle interior substrate. The support base is configured with a flange that surrounds a door support panel and overlays the opening in the vehicle interior substrate when inserted therein. The flange has outer edges that are flexible and tapered to lie flat against the substrate surface to both seal the interface and minimize interference to the flow of foam during the foam-in-place injection process employed after the chute structure is inserted into the aperture of an instrument panel substrate and locked in place.
A rectangular air bag chute skirt extends downward from the support base. The chute side walls are made up of two opposing major walls that run parallel with each other and two opposing minor walls that join the two major walls. The major walls are also parallel to the hinge and leading edge of a door support panel defined in the upper portion adjacent to the flange. The four walls form a skirt for surrounding a separate air bag container and define the path for deployment of the air bag from the air bag container. In the described embodiment, the door support panel is generally co-planar with the support base flange and has defined door edges formed on three sides by pre-weakened molding or scoring. The door support edges remain attached to the support base prior to deployment of the air bag. A door support hinge element is formed to extend along one side of the defined door. In the described embodiment, the entire upper surface of the air bag deployment chute that includes the door support panel and the flange is continuously closed without gaps or openings so that there is no potential path for foam leakage during the foam-in-place injection process.
The chute side walls on the lower portion of chute form a rectangular cross-sectional chute having first and second generally parallel and opposed major walls that are longer than third and fourth generally parallel and opposed minor walls oriented generally perpendicular to the first and second walls.
On the outer surface of a first side wall and below the flange, a single elongated tab (or a plurality of short tabs) is located to extend outwardly from the wall and define a corresponding slot between the tab and the underside of the flange. The slot is arranged in a line that corresponds to the edge of the substrate aperture into which the structure will be mounted. When the chute is inserted into the aperture from the upper side of the instrument panel substrate, the slot becomes engaged with the edge of the aperture and holds the tapered edge of the flange adjacent thereto, against the upper surface of the substrate.
The third and fourth side side walls contain gussets or braces to provide support to the flange extending above those walls. The gussets are of the same flexible material as the remainder of the integrally molded chute and because they extend beyond the substrate aperture, are slightly deformed during the insertion process. Notches are provided in the upper portions of the gussets to accommodate the side edges of the aperture in the instrument panel substrate. When the chute is fully inserted into the aperture, the gussets resume their original shapes and the notches capture and hold the chute and the flange in place for maintaining the seal.
The second skirt wall contains a series of individual notches or depressions that extend substantially the length of the wall beneath the flange and are sized to accept tab like extensions from the aperture edge, when the chute is fully inserted into the aperture. These depressions, along with the notches in the side gussets, retain the three sides of the chute and maintain the seal between the flange edges extending from those three sides and the upper surface of the instrument panel substrate.
Therefore, it is an object of the inventive concept to provide an improved air bag deployment chute that is held in place within the instrument panel of an automotive vehicle by merely inserting the chute into a corresponding aperture in the substrate.
It is another object of the inventive concept to provide an improved air bag chute that is an integrated structure with a surrounding flange having a tapered edge that seals against the upper surface of the instrument panel to which the air bag chute is mounted prior to performing a foam-in-place process and an attachment configuration that maintains the seal without the need for additional components such as fasteners.
It is a further object of the inventive concept to provide an air bag chute structure used in an air bag deployment system of an automotive vehicle wherein the structure is configured to be installed in an aperture of an instrument panel substrate; the structure contains an upper portion with a flange surrounding the structure; the flange is formed to engage the upper surface of the substrate surrounding the aperture when the structure is inserted into the aperture; and retaining slots and notches are provided in the lower portion of the chute structure to engage and interlock with the edges of the aperture formed in the instrument panel substrate during its insertion therein and to permanently retain the chute in the aperture.
It is a still further object of the inventive concept to provide a method of retaining an air bag deployment chute structure in an aperture formed in the substrate of an automotive instrument panel as a result of inserting the chute into the aperture from the upper surface side of the substrate and subjecting the chute to downward pressure to engage the retaining mechanism. The steps include providing the chute structure with a flange that extends around a defined deployment door support panel sufficiently to exceed the dimensions of the aperture; providing the outer side skirt walls of the chute below the flange with notches and slots that will engage the edges of the aperture when inserted into the aperture; insert the air bag deployment chute structure into the aperture in the substrate so that the flange engages the upper surface of the substrate; and fully depress the flange against the substrate until all the notches and slots engage the edges of the aperture.
It is a still further object of the inventive concept to provide an air bag chute structure for use in an instrument panel air bag deployment system of an automotive vehicle, comprising: a generally planer deployment door support panel portion integrated in the structure and defined by a plurality of pre-weakened edges and a flexible hinge with an upper surface and a lower surface; a generally planar flange member portion with an upper surface and a lower surface extending from the area surrounding the door support panel; an air bag chute portion extending from an area adjacent the lower surfaces at a junction of the door panel and the flange for insertion into a corresponding aperture formed in the substrate of an instrument panel; a single elongated tab (or series of tabs) that defines a slot (or series of aligned slots) beneath the flange along the hinge side of the chute portion between the lower surface of the flange and having a slot width that is substantially equal to the thickness of the aperture edge to engage the aperture edge when the chute is inserted into the aperture; and a plurality of notches disposed below the lower surface of the flange on the other sides of the chute portion to engage portions of the aperture edge when the air bag chute is fully inserted into the aperture.
A more complete description of an embodiment of the inventive concept is presented below.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
FIG. 1 is a perspective view of the air bag chute structure of the present invention.
FIG. 2 is a perspective view of the same air bag chute shown in FIG. 1 , but rotated upwards to reveal the detail of the sidewall below the door support panel hinge.
FIG. 3 is a perspective view of the same air bag chute shown in FIG. 1 , viewed from the opposite side to reveal the detail of the sidewall below the door support panel opening edge.
FIG. 4 is a top plan view of the instrument panel substrate aperture into which the air bag chute of the present invention is inserted.
FIG. 5 is a cross-sectional view of the air bag chute of the present invention taken along lines 5 - 5 in FIGS. 2-4 as it is being inserted into the instrument panel aperture and having one side initially engaged with the instrument panel substrate.
FIG. 6 is a cross-sectional plan view of the air bag chute structure of FIG. 5 after it has been fully installed in the instrument panel substrate and subjected to the foam-in-place process.
DETAILED DESCRIPTION OF THE INVENTION
The perspective view of the air bag chute 100 of the present invention is shown in FIG. 1 with the forward or windshield side in the foreground and the rear or passenger side in the background. The air bag chute 100 is embodied as a unitary structure 110 that is molded of a plastic material preferably having some flexibility to prevent fracturing during air bag deployment in all expected temperatures of operation. The upper portion of the structure 110 includes a door support panel 120 that is defined by a pre-weakened seam 122 at the outermost (initially rupturing) edge and a pair of pre-weakened seams on side edges 121 and 123 . A hinge 124 defines the fourth side of the door support panel 120 .
When installed on the instrument panel of a passenger vehicle, the hinge is closest to the windshield of the vehicle and the initially rupturable seam 122 is located closest to the passenger seating position.
The air bag chute structure 100 is formed as a one piece molding of a flexible material such as Dexflex™ or other material that exhibits equivalent or superior ductility at very cold temperatures at least to −30° C. and good toughness at high temperatures at least to 90° C. Materials such as TPO (Thermoplastic Olefin), TPE (Thermoplastic Elastomer) or TEO (Thermoplastic Elastomer Olefin) could be substituted.
In the shown embodiment, door support panel 120 is surrounded by a mounting flange 108 that is generally rectangular in shape and has flexible and tapered edges 112 , 114 , 116 and 118 of mounting flange 108 . The tapered edges are formed to be biased slightly downward so that when installed in the aperture of an instrument panel substrate 50 , the flange will provide a compression seal with respect to the substrate surface.
A plurality of windows 150 and 154 with retainer tabs 152 and 156 are located on lower chute side walls 126 and 128 , and reinforcement bars 130 and 132 are located at the lowest edge of the chute walls 126 and 128 ( FIGS. 2 and 3 ). Retainer tabs 152 and 156 function to contact hooks extending through the windows 150 and 154 from the air bag container module (not shown) to reduce vibration/rattling in a conventional manner.
On sidewall 126 , a single tab like protrusion 140 is shown in FIG. 2 that runs over most of the sidewall length. The guide tab 140 is supported by a series of gussets 141 that are anchored to the side wall 126 between window locations. The guide tab 140 is located just below the flange 108 and above the windows 150 to form a slot 142 therebetween. The slot has a height measured between the guide tab 140 and flange 108 that is approximately equal to the thickness of the edge of the aperture 51 in the instrument panel substrate 50 . The guide tab 140 and slot 142 serve to engage the edge of the aperture 51 during insertion of air bag chute 100 therein. Following the completion of insertion of air bag chute 100 into the aperture 51 , the tab 140 functions to retain the air bag chute in aperture 51 .
Other features pertinent to the present invention include the support gussets 160 shown in FIGS. 2 and 3 . These support gussets are located on the outer sides of both side walls 127 and 129 to provide a degree of rigidity between the flange 108 and the sidewalls. Notches 162 are provided just below the flange 108 to have a size that corresponds to the thickness of and to engage the edges 55 and 56 of aperture 51 ( FIG. 4 ) when air bag chute 100 is inserted therein.
On the passenger side of air bag chute 100 , shown in FIG. 3 , a series of indented depressions 144 are formed in sidewall 128 in correspondence to the locations of tab like protrusions 53 extending from the edge of the aperture 51 in the instrument panel substrate 50 ( FIG. 4 ). The depressions 144 are spaced apart so that they are separated by the window openings 154 . This separation and location serves to retain the strength integrity of the sidewall 128 that may be compromised if the depressions 144 were to be located above the windows or were formed as a single continuous depression that extended over the windows 154 .
FIG. 5 illustrates how guide tab 140 and slot 142 of air bag chute 100 (taken along section lines 5 - 5 in FIGS. 2 , 3 and 4 ) are used to engage edge 52 of aperture 50 during the initial part of the installation of air bag chute 100 therein. As can be seen, the lower chute skirt made up of sidewalls 126 , 127 , 128 and 129 is inserted into aperture 51 from above. As the forward portion of flange 108 containing tapered edge 114 is pressed against substrate 50 , flange 108 is flexed upwards to allow edge 52 to slide into slot 142 . Once edge 52 is fully engaged in slot 142 , the passenger side of chute 100 is depressed into aperture 51 . During that depression, gussets 160 are flexibly deformed inwards by side edges 55 and 56 until slots 162 engage. When slots 162 engage, gussets 160 are restored to their normal shapes. Further depression of chute 100 into aperture 51 allows depression 144 in sidewall 128 to engage tab protrusions 53 (see FIG. 6 ). At that point, air bag chute 100 is fully inserted into aperture 51 and secured in instrument panel substrate 50 .
In FIG. 6 , a cross-sectional view of air bag chute structure 110 is shown taken along section lines 5 - 5 in FIGS. 2 , 3 and 4 , fully mounted on instrument panel substrate 50 . The drawing illustrates air bag chute 100 in its finished condition mounted on the instrument panel 50 and covered with a foam interlayer 70 and a “class A” outer skin 60 . It should be noted that many choices of outer skin layers or laminations can be used that are both conventional and yet to be invented. The actual materials used for the outer skin are not pertinent to the present invention except for the property of containing the initially injected foam in its liquid form, and later the foam flow back as it approaches its solid form during the foam-in-place process described above.
The air bag chute structure 110 is inserted into the aperture 51 defined in the instrument panel substrate 50 . Guide tab 140 is located under flange 108 and extends from the outside of side wall 126 towards the tapered outer edge 114 . Slot 142 is shown formed between guide tab 140 and the underside of flange 108 below and in the vicinity of hinge 124 . Slot 142 is only slightly larger than the thickness of the substrate 50 , at that location, and allows the chute structure to positively engage edge 52 of aperture 51 . When installed, the tapered edge 114 of flange 108 sealingly engages the upper surface of substrate 50 .
At the rear passenger side of the air bag chute structure 110 , depressions 144 formed in sidewall 128 below and in the vicinity of the leading edge 122 of the support door panel 120 are shown engaging edge tab protrusion 53 of aperture 51 . Tapered edge 112 of flange 108 sealingly engages the upper surface of substrate 50 . Although not shown, the other tapered edges 116 and 118 of flange 108 also sealingly engage the upper surface of substrate 50 . When installed, as shown in FIG. 6 , tapered edges 112 , 114 , 116 , 118 provide a complete seal of the opening 52 in substrate 50 without the requirement for masking tape or other add-on sealers.
An alternative embodiment of the present invention (not shown) duplicates the retention mechanism pictured on the passenger side of the air bag chute structure 110 on the forward or windshield. Instead of using a guide tab 140 below the underside of flange 108 in the vicinity of hinge 124 to define slot 142 , depressions 144 are formed in sidewall 126 below and in the vicinity of hinge 124 . Edge tab protrusions 53 of aperture 51 on the passenger side of the substrate aperture are duplicated on the forward side of the substrate aperture to accommodate and engage with the depressions on that side of the air bag chute structure 110 . Installation of this embodiment allows for a straight or angled insertion of the air bag chute structure 110 into the aperture 51 . Retention is completed when the tab protrusions 53 engage the depressions 144 in both side walls 126 and 128 .
It can be seen from the drawings and accompanying explanation, that the present inventive concept is a unique improvement over conventional air bag deployment support structures and methods of installation. And while the embodiments described here are preferred, they shall not be considered to be a restriction on the scope of the claims set forth below. | An integrated air bag chute structure that provides means for providing automatic interlocking attachment of the chute to the substrate of an instrument panel. By inserting the air bag chute into a substrate aperture and utilizing slots, depressions and notches formed in the chute structure beneath a surrounding flange, the aperture edges are captured and retained to thereby lock the chute in place. | 8 |
CROSS REFERENCE TO RELATED APPLICATION
This application is related to, and claims priority under 35 U.S.C. § 119 of, German Application No. 197 05 360.2, filed Feb. 12, 1997, the disclosure of which is expressly incorporated herein in its entirety by reference thereto.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a device and a process, particularly a press device and a pressing process. The device and process of the invention are for use on a fibrous web or fibrous pulp web, such as a cellulosic fibrous web or cellulosic fibrous pulp web, having a surface weight of about 100 g/m 2 or less, or under about 100 g/m 2 ; graphic papers are particularly preferred. The device and process of the invention are utilized for treating—e.g., for draining (particularly dewatering) and/or for smoothing—and particularly for pressing the indicated material, and for controlling its surface properties and sheet structure.
The device and process of the invention employ a press area which comprises or consists of at least one press nip. During operation of the device and practice of the process, the fibrous pulp web is fed through the press area at a speed of at least about 1200 m/min, while simultaneously being subjected to pressure.
2. Discussion of Background Information
Press devices of the type as discussed above, for the production of high-grade, graphic papers, usually are composed of compact presses, comprising or consisting of a press with 3 or 4 rolls, followed by at least one supplementary laying press. Such a relatively large number of essential roll openings, which is necessary due to the high operating velocity used in producing high-grade graphic papers, results in a large space requirement for these devices, because of the correspondingly large number of rolls needed. Despite this relatively high expenditure, only a limited draining capacity is attained because of the high operating velocity.
SUMMARY OF THE INVENTION
It is accordingly an object of the present invention to provide a press device and a pressing process of the type as mentioned initially above, but which have as small a space requirement as possible, while at the same time both displaying a high capacity for draining at high operational speeds, and also avoiding a loss of quality, such as from crumpling the paper web. This object is achieved by providing that the press area of the indicated press device and pressing process comprises at least two press zones in succession, and also providing that the device and process attain a K value of at least 2.5 kPa·s·m, or at least about 2.5 kPa·s·m. Preferably, the device and process of the invention attain a K value of at least 2.6 kPa·s·m, or at least about 2.6 kPa·s·m, or at least 2.8 kPa·s·m, or at least about 2.8 kPa·s·m, or at least 3.0 kPa·s·m, or at least about 3.0 kPa·s·m.
The indicated K value is the product of L 1 and I tot . L 1 is the length of the first press zone, measured along the direction in which the web runs, and I tot is the total press impulse operating on the fibrous pulp web in the entire press area.
With press devices of the prior art, usually the fibrous pulp web is first drained intensively with roll presses, with a high line force, and then drained gently with extended nip presses. Pressure peaks with large gradients accordingly appear at high velocities. As a result, large quantities of water are pressed out of the loosely bound, wet paper web in a short amount of time, so that the paper web can be damaged, for example by crumpling.
However, for the present invention, it is guaranteed that a sufficient pressing time in the first press zone, as well as a sufficient press impulse for as high a draining or dewatering capacity as possible, are provided for the fibrous pulp web. If the draining or dewatering is not gentle, then twosidedness increases; however, the use of gentle draining or dewatering has the desirable effect of minimizing twosidedness. A gentle draining or dewatering is achieved by means of the length of the first press zone as well as the total press impulse operating on the fibrous pulp web.
It is understood that twosidedness, with reference to a particular property or properties, pertains to a variation in that property or properties between the top side and the bottom side of the fibrous web, for example, paper or liner. If the difference between the top and the bottom side is small for a particular property, then twosidedness for that property is small.
For instance, twosidedness in ash content refers to a difference in ash content distribution, from the top to the bottom of the web or paper product; correspondingly, minimizing twosidedness in ash content means minimizing the difference in ash content distribution between the top side and the bottom side. Accordingly, twosidedness in filler content refers to a difference in filler content distribution, from the top to the bottom of the web or paper product; correspondingly, minimizing twosidedness in filler content means minimizing the difference in ash content distribution between top and bottom.
There is also twosidedness with respect to the properties of structure and roughness. Minimizing structural twosidedness means minimizing the difference in the structural arrangement of fibers between the top and bottom sides. Minimizing twosidedness as to roughness means minimizing the difference between the roughness of the surface of the top side and the roughness of the surface of the bottom side.
As indicated herein, gentle dewatering minimizes twosidedness generally. Among the specific properties for which gentle draining diminishes twosidedness are structural twosidedness, twosidedness in ash content, twosidedness in filler content, and twosidedness as to roughness.
Because the amount of fluid is highest at the point where the fibrous pulp web is fed into the press device, or where the fibrous pulp web is first subjected to the pressing process, significantly more fluid must be diverted at the beginning of the pressing than at the end of the pressing. Therefore, a gentle draining in the first press zone is especially important at the machine velocities which are necessary for treating graphic papers. Because of the length of the first press zone in accordance with the invention, and accordingly the extent of the time period during which the fibrous pulp web is inside this zone, the essential gentle draining is accomplished in the first press zone.
The pressure pries of the various press zones can be the same, or substantially or essentially the same. However, it is advantageous for various press zones to have differing pressure profiles. For example, after the first, gentle draining in the first press zone, there can follow a gentle draining in the second press zone, with the pressure profile of this second zone demonstrating a pressure gradient larger than that of the pressure profile of the first press zone.
In a preferred and advantageous embodiment of the invention, the press zones of the press area are formed by several presses, such as shoe presses, roll presses, and extended nip presses. Preferably a shoe press is used to form the first press zone, because the distinguishing features of the invention can be especially easily attained with a shoe press. Thus it is especially simple to adjust the essential, gentle draining in the first zone by means of a shoe press. The reason for this ease of adjust is that, on the one hand, long duration of the web in the zone, and on the other hand, a moderate increase in pressure via a corresponding length and shape of the press shoe as well as a corresponding impingement of the press shoe, can be achieved with pressure.
The present invention may employ two or two or more press zones, or three or three or more press zones. Assuming that the first press zone is formed by a shoe press or a part of a shoe press, the most diverse embodiments of the remaining press zones are conceivable. For example, the entire press area can encompass two press zones, whereby the first press zone is formed by a shoe press and the second press zone by a roll press or another shoe press. As another example, the press area can also comprise three press zones, whereby the first press zone is formed by a shoe press, and the second and third press zones by roll presses which successively follow the shoe press along the path of the web. In place of the second roll press, another shoe press can be provided.
As another possible embodiment, there may be at least two successive press zones formed by shoe presses which are arranged alternatively—specifically, situated on different, or opposite, sides of the fibrous pulp web, or of the path along which the web runs. The shoe presses may be configured so that in successive zones, pressure is alternatingly applied to opposite sides of the web.
To further reduce the amount of space required, the press area can comprise or consist of only two press zones, which are both formed by shoe presses arranged successively in the direction that the web runs. Preferably in this embodiment, the two shoe presses are equal, or at least substantially or essentially equal; specifically, they are preferably of the same, or at least substantially or essentially the same, mechanical configuration or design. In order to attain a final, intense draining at the end of the pressing, yet another roll press can be provided after both shoe presses in the direction that the fibrous pulp web runs.
As one embodiment of the invention, where the press area consists of only two press zones and the two zones are formed by successive shoe presses as indicated, and particularly where the two shoe presses are of the same, or at least substantially or essentially the same, mechanical configuration or design, the line forces {overscore (p)} 1 and {overscore (p)} 2 of the two press zones are equal, or at least substantially or essentially equal, but the lengths L 1S and L 2S of the press zones—i.e., the lengths of the shoes—as measured along the direction in which the web runs, are not equal. In other words, the running conditions of the two shoe presses are equal, or at least substantially or essentially equal, but the shoe designs are not equal.
As another embodiment of the invention, where the press area consists of only two press zones and the two zones are formed by successive shoe presses as indicated, and particularly where the two shoe presses are of the same, or at least substantially or essentially the same, mechanical configuration or design, the line forces {overscore (p)} 1 and {overscore (p)} 2 of the two press zones are not equal, but the lengths L 1S and L 2S of the press zones—i.e., the length of the shoes—as measured along the direction in which the web runs, are equal, or at least substantially or essentially equal. In other words, the running conditions of the two shoe presses are not equal, but the shoe designs are equal, or at least substantially or essentially equal.
As yet another embodiment of the invention, where the press area consists of only two press zones and the two zones are formed by successive shoe presses as indicated, and particularly where the two shoe presses are of the same, or at least substantially or essentially the same, mechanical configuration or design, the line forces {overscore (p)} 1 and {overscore (p)} 2 of the two press zones are not equal, and likewise the lengths L 1S and L 2S of the press zones—i.e., the lengths of the shoes—as measured along the direction in which the web runs, are not equal. In other words, both the running conditions of the two shoe presses, and the shoe designs, are not equal.
As still a further embodiment of the invention, where the press area consists of only two press zones and the two zones are formed by successive shoe presses as indicated, and particularly where the two shoe presses are of the same, or at least substantially or essentially the same, mechanical configuration or design, the line forces {overscore (p)} 1 and {overscore (p)} 2 of the two press zones are equal, or at least substantially or essentially equal, and also the lengths L 1S and L 2S of the press zones—i.e., the length of the shoes—as measured along the direction in which the web runs, are equal, or at least substantially or essentially equal. In other words, the running conditions of the two shoe presses are equal, or at least substantially or essentially equal, and also the shoe designs are equal, or at least substantially or essentially equal.
With regard to the foregoing, press zone line force {overscore (p)} is defined by the area encompassed by the pressure profile. It is also defined by the equation p _ = ∫ L p x
As discussed herein, in the present invention the individual press zones can be provided by different press mechanisms. However, it is also within the scope of the invention for the press area to be formed by a single press mechanism. This single press mechanism can be a long shoe press or an extended nip press, with a press area which is elongated in the direction that the fibrous pulp web runs. The press area, accordingly having a long configuration, is thereby separated into at least two successive press zones, and the necessary press dimensions can be adjusted therein.
With regard to the use of a long so press as the single press mechanism, it is noted that in the present state of the art, the maximum shoe length for a conventionally sized shoe press is about 300 mm. In the context of the present invention, it is understood that a long shoe press is one having a length of more than about 300 mm, as measured along the direction in which the web runs. An example of a long shoe press is one having a length of 500 mm, or about 500 mm.
In the present invention, the fibrous pulp web is preferably run at a velocity of at least 1200 m/min, or at least about 1200 m/min. In an advantageous embodiment of the invention, the transport velocity of this web is more preferably at least 1500 m/min, or at least about 1500 m/min. As a matter of particular preference, the velocity of the fibrous pulp web is at least 1800 m/min, or at least about 1800 m/min. It is also within the scope of the invention to run the fibrous pulp web at a velocity of at least 2500 m/min, or at least about 2500 m/min.
The value K, as discussed herein, is the product of the length L 1 of the first press zone, as measured in the direction that the fibrous pulp web runs, and of the total press impulse I tot in the entire press area affecting the fibrous pulp web. K is defined by the equation K = L 1 · I tot = L 1 · ∑ i = 1 n ( p m i · L i ) v = t 1 · ∑ i = 1 n p _ i
wherein:
n=the number of press zones;
L i =the length of the i-th press zone;
p m i =the medium pressure applied to the fibrous pulp web in the i-th press zone;
v=the velocity of the fibrous pulp web;
t 1 =the time that a point of the fibrous pulp web resides in the first press zone; and
{overscore (p)} i =the line force applied to the fibrous pulp web in the i-th press zone.
In other words, for a press device and a pressing process of the present invention, the product, of the time t 1 that a point of the fibrous pulp web resides in the first press zone, and of the sum of the line forces {overscore (p)} i applied to the fibrous pulp web in the isolated press zones, amounts to at least about 2.5 kPa·s·m.
Preferably, the total length L tot = ∑ i = 1 n
L i of the press area is at least about 250 mm. Also as a matter of preference, the total time t tot = ∑ i = 1 n
t i that a point of the fibrous pulp web resides in the press area is at least about 10 milliseconds.
The total line force operating in the press area p _ tot = ∑ i = 1 n p _ i
is preferably about 1800 kN/m or less. Also the total press impulse I tot operating on the fibrous pulp web is preferably at least about 25 kPa·s.
Yet additionally as a matter of preference, the characteristic number for the a draining capacity DC={overscore (p)} tot ·t tot is at least about 15 kN · s m .
And still further as a matter of preference, the characteristic number for gentle draining GD = p _ tot t tot
is about 63 MN m · s
or less.
The pressure applied to the fibrous pulp web in the first press zone is preferably lower than that employed in the one or more subsequent press zones. In this way, the essential, gentle draining can be advantageously achieved in the first press zone.
For the portions of the pressure profiles which indicate increasing pressure, the pressure profile in the first press zone can have a pressure gradient smaller than the pressure gradient of at least one of the one or more subsequent press zones. It is also due to this feature that the indicated gentle draining is taken into consideration in the first press zone.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention is further described in the detailed description which follows, in reference to the noted plurality of drawings by way of nonlimiting examples of preferred embodiments of the present invention, and wherein:
FIG. 1 is a graph showing different values for L 1 ·I tot , obtained with different press devices at three different web velocities;
FIG. 2 is a graph showing the pressure profile, over the length of the press area, for a press device having a shoe press followed by two successive or connecting roll presses;
FIG. 3 is a graph showing the pressure profile, over the length of the press area, for a press device having a shoe press, followed by a roll press, followed by another shoe press;
FIG. 4 is a graph showing the pressure profile, over the length of the press area, for a press device which employs, as the sole press mechanism, a shoe press of more than about 300 mm in length, as measured along the direction in which the web runs;
FIG. 5 is a graph showing the pressure profile, over the length of the press area, for a press device which employs an extended nip press as the sole press mechanism; and
FIG. 6 is a graph showing the pressure profile, over the length of the press area, for another press device which employs an extended nip press as the sole press mechanism.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows the different K=L 1 ·I tot values, measured as kPa·s·m, obtained with different press devices, at different web velocities. The different press devices are a conventional press consisting of three roll presses, a press consisting of two roll presses and a subsequent shoe press, a press consisting of a shoe press with two subsequent roll presses, and a press consisting of two shoe presses in succession.
For each of these four press devices, kPa·s·m measurements are calculated for web velocities of 1200 m/min, 1500 m/min, and 2500 m/min.
For the first, second, and third press zones in the press devices, medium pressures of p m1 =2 MPa, p m2 =3 MPa, and p m3 =5 MPa, respectively, were chosen. The lengths of the press zones which were formed by roll presses were L 1 =40 mm, L 2 =30 mm, and L 3 =30 mm, with the subscript denoting the position of that press zone within the press area, in relation to the other press zones. In this regard, a press area is formed by its successive press zones, with each press zone defined by the area in which its respective press operates; particularly, when the presses are press rolls, the press area is formed by the successive press rolls.
For the press devices with shoe presses, L 1S =150 mm, and L 2S =270 mm were chosen for the lengths of the press zones defined by their respective press shoes. Corresponding to the subscripts used for the roll presses, as discussed above, for these shoe presses the position of the press zone within the press area is likewise denoted by a supplementary subscript 1, 2, or 3.
The four following configurations were thusly obtained. The corresponding values for these configurations are shown.
1. Conventional Press (Press Zones L 1 , L 2 , L 3 )
For a web velocity of V=1200 m/min, the result is K = L 1 · I tot = L 1 · ∑ i = 1 n ( p m i · L i ) v = 40 mm · 2 MPa · 40 mm + 3 MPa · 30 mm + 5 MPa · 30 mm 1200 m / min = 0.64 kPa · s · m .
Correspondingly, for web velocities of V=1500 m/min and V=2500 m/min, the results are K=0.512 kPa·s·m and K=0.307 kPa·s·m, respectively.
With this press device, K values below the desired 2.5 kPa·s·m lower limit were obtained at web velocities of 1200 m/min and greater. It is accordingly evident that a conventional press device is not suitable for producing qualitatively high-grade, graphic papers at high operating velocities.
2. Press Device with Shoe Press Providing the Third Press Zone (Press Zones L 1 , L 2 , L 3S )
For this press device, values of p _ L = 800 kN m ,
p m =3 MPa, and V=1200 m/min result in a K value (K=L 1 ·I tot ) of 1.96 kPa·s·m. Web velocities of V=1500 m/min and V 2500 m/min result in K values of 1.57 kPa·s·m and 0.94 kPa·s·m, respectively. Accordingly, for this device also the K values are below the desired value of 2.5 kPa·s·m, and therefore beneath the area in FIG. 1 shaded in grey.
Became the shoe press is not used for the first press zone in this press device, the essential, gentle draining is not attained at the beginning of the pressing. Therefore, with this press device, treatment of graphic papers at the necessary high velocities does not provide the desired quality.
3. Press Device with Shoe Press Providing the First Press Zone (press zones L 1S , L 2 , L 3 )
This press device, with a shoe press providing the first press zone, yields a K value (K=L 1S ·I tot ) of 3.225 kPa·s·m for P _ L 1 = 200 kN m ,
p m1 =1.33 MPa, and V=1200 m/min. With a web velocity of V=1500 m/min, the resulting K value is 2.58 kPa·s·m. For P _ L 1 = 292.6 kN m ,
p m1 =1.33 MPa, and V=2500 m/min, K=2.76 kPa·s·m.
Thus, the K values for this press device are greater than the desired 2.5 kPa·s·m lower limit, and therefore within the area shaded in grey in FIG. 1 . Accordingly, with this configuration, a treatment of graphic papers at high velocities provides a treated paper web of high grade.
4. Press Device Consisting of Two Shoe Presses in Succession (Press Zones L 1S , L 2S )
With this press device, which comprises only two press zones, a pressure of 1.33 MPa was used as a basis for data in the first press zone, and a pressure of 3 MPa was used as a basis for data in the second press zone. Thereby, at a web velocity of V=1200 m/min, the resulting K value (K=L 1S ·I tot ) is 7.5 kPa·s·m; at V=1500 m/min and V=2500 m/min, the resulting K values are 6.0 kPa·s·m and 3.6 kPa·s·m, respectively.
It can accordingly be seen that through the application of two shoe presses in succession, the crucial lower limit of 2.5 kPa·s·m for the K value is thus in part markedly exceeded, as shown in FIG. 1 .
The gentle increase in pressure occurring at the beginning of the pressing in a shoe press is distinctly recognizable in the course of pressing 1, as shown in FIG. 2 . Therein is depicted the pressure profile of a press device in accordance with the invention; specifically, this press device has a shoe press for forming the first press zone, followed by two successive or connecting roll presses, which form the second and third press zones, respectively. The gentle draining of the fibrous pulp web, initiated within the first press zone, ceases after distance L 1 , at the end of the shoe press. The remainder of the draining thereafter occurs in the two following press zones. These zones are formed by roll presses of lengths L 2 and L 3 , respectively, under impingement by high pressure and larger pressure gradients.
The pressing represented by the pressure profile of FIG. 3 essentially correlates to that of FIG. 2, except for the respective third press zones. Whereas the third press zone for the FIG. 2 device is provided by a press roll, the device of FIG. 3 has a third press zone formed by a shoe press, with a pressing 3′ and a press zone length L 3S . Because of this, the FIG. 3 device also attains a gentle draining in the third nip at a simultaneously high total press impulse.
Even with this FIG. 3 press device, the K value (K=L 1S ·I tot ) is greater than 2.5 kPa·s·m, so that an optimal treatment, of graphic papers having a surface weight under 100 g/m2, is possible at high velocities.
FIG. 4 depicts the pressure profile 4 , of a press device in which both of the press zones, having lengths L 1 and L 2 respectively, are formed by one long shoe press—i.e., a shoe press which is more than about 300 mm in length, as measured along the direction in which the web runs. The length L 1 of the first press zone thereby extends from the beginning of the pressure profile to the point at which the increase of the pressure profile is at maximum, and thus defined, for example, by the position of the pressure profile turning point. The initial increase of the pressure profile is not taken into consideration here, because only a structural compression, without draining, occurs in this area.
The pressure profile illustrated in FIG. 4 essentially correlates to the pressure profile shown in FIG. 3, if the three nips forming the FIG. 3 pressure profile were concentrated into a single nip. For the FIG. 4 press device, the K value (K=L 1 ·I tot ) lies above the requisite 2.5 kPa·s·m lower limit.
FIG. 5 shows the pressure profile 5 of a press device having two press zones with lengths L 1 and L 2 , respectively. These zones are formed by one extended nip press, with the length L 1 being characterized by the turning point of the pressure profile 5 . While in the first press zone of the press area a relatively gentle increase of the pressure occurs along the pressure profile 5 ′, the pressure increases decidedly more sharply in the second press zone along the pressure profile 5 ″. Through this, a gentle draining is attained at the beginning of the pressure profile, on the one hand, whereby simultaneously at the end of the pressing, the remaining moisture is pressed out of the fibrous pulp web by means of the increased pressure as well as the heightened gradient of the pressure profile.
The K value (K=L 1 ·I tot ) lies above the essential 2.5 kPa·s·m lower limit with this FIG. 5 press device also.
The pressure profile 6 shown of FIG. 6 is distinguished from the pressure profile illustrated in FIG. 5 in that, for the FIG. 6 pressure profile, the increase of the pressure within the first press zone runs more steeply than in pressure profile of FIG. 5 . As with length L 1 for the first press zone in FIG. 5, the length L 1 of the FIG. 6 first press zone is correspondingly characterized by the turning point of the pressure profile 6 . At the end of the pressing, the pressure inside of the second press zone decreases abruptly.
Even with the press device of FIG. 6, the K value lies above 2.5 kPa·s·m, so that qualitatively high-grade, graphic papers can be treated by this device at high velocities.
The press devices of FIGS. 2 and 3 each includes three press mechanisms, and therefore both of these devices have three nips. Each of the press devices of FIGS. 4, 5 , and 6 employs a single press mechanism, and therefore these devices all have only one nip. Because of this single nip feature these latter press devices enjoy an advantage in efficiency over the FIG. 2 and FIG. 3 multiple nip devices.
In this regard, it is noted that the pressing which takes place with each press mechanism involves at least two steps. The first of these steps is structural compression; as indicated herein, with structural compression the web is compressed, but no draining, or dewatering, occurs. After a certain level of pressure is reached, the second step takes place, and draining occurs along with the compression.
After the pressure applied by the press mechanism reaches its apogee and begins falls back to zero, rewetting of the web occurs. And where there are multiple press mechanisms in the press device, efficiency is weakened for the following reasons.
Specifically, after pressure has fallen back to zero for the first press mechanism and the accompanying rewetting has occurred, pressure is applied by the next press mechanism, and the two or more step process is accordingly reiterated. The first step, as discussed, is the structural compression, and the corresponding lack of draining with this step is indicative of its inefficiency. As yet an additional inefficiency, at the point in this next mechanism's pressure profile where its pressure falls below the pressure at which draining occurs with the prior press mechanism, rewetting takes place again.
Both of these forms of inefficiency are repeated with each additional press mechanism. Accordingly, with multiple nips effective press length is lost from the press device.
However, with the single press mechanism devices, such as those of FIGS. 4, 5 , and 6 , there is no structural compression, without draining, to occur between nips, because there are no multiple nips; there is only the one nip for the device. Also, rewetting between press zones is practically nonexistent.
Accordingly, the two indicated forms of inefficiency which characterize multiple mechanism press devices are not found, or are greatly reduced, for the single nip press devices. These devices have increased effective press length.
It is noted that the foregoing examples have been provided merely for the purpose of explanation and are in no way to be construed as limiting of the present invention. While the invention has been described with reference to preferred embodiments, it is understood that the words which have been used herein are words of description and illustration, rather than words of limitation. Changes may be made, within the purview of the appended claims, as presently stated and as amended, without departing from the scope and spirit of the invention in its aspects. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein; rather, the invention extends to all functionally equivalent structures, methods and uses, such as are within the scope of the appended claims. | A press device for draining and/or smoothing, or shaping the surface and controlling the sheet structure of fibrous pulp webs with a surface weight of under 100 g/m 2 , such as the fibrous pulp webs used to make graphic papers. The device has a press area which includes at least one press nip through which, during operation, the fibrous pulp web is fed at a velocity of at least 1200 m/min, under simultaneous impingement by pressure. The press area includes at least two press zones subsequent to one another. The device is further characterized by a K value of at least 2.5 kPa·s·m. This K value is the product of L 1 and I tot . L 1 is the length of the first press zone, measured along the direction in which the web runs, and I tot is the total press impulse operating on the fibrous pulp web in the entire press area. | 3 |
TECHNICAL FIELD
[0001] This invention relates to luminaires, and in particular to systems for connecting luminaires together.
BACKGROUND
[0002] Spatial and design considerations can require two or more luminaires to be connected together in certain lighting environments. Systems for effectively connecting luminaires are desirable.
SUMMARY
[0003] The inventions described herein have many aspects, some of which relate to systems for connecting luminaries.
[0004] In one aspect, a system for connecting luminaires is provided. The system comprises: a first luminaire comprising an end face comprising a first slot; a second luminaire comprising an end face comprising a second slot; a first elongated joining member comprising first prongs. The first slot and second slot are in laterally aligned and joined relationship define a first joining member slot comprising a first wedged end, and the first wedged end is shaped to provide an interference fit with the first prongs wherein advancing the first prongs against the first wedged end forces the first slot and the second slot toward each other to tighten connection between the first luminaire and the second luminaire.
[0005] The first wedged end may comprise outwardly and downwardly angled surfaces that define a first angle equal to or greater than a second angle defined by the first prongs.
[0006] The first luminaire may comprise a first crossplate that at least partly defines the end face of the first luminaire, and the second luminaire may comprise a second crossplate that at least partly defines the end face of the second luminaire.
[0007] The first luminaire may comprise a pair of first sidewalls that at least partly defines the end face of the first luminaire, and the second luminaire may comprise a pair of second sidewalls that at least partly defines the end face of the second luminaire.
[0008] The first and second slots may be formed in the first and second crossplates.
[0009] The first slots may be formed in the first sidewalls and the second slots may be formed in the second sidewalls.
[0010] The first slots may be formed partly in the first crossplate and partly in the first sidewalls, and the second slots may be formed partly in the second crossplate and partly in the second sidewalls.
[0011] The first and second elongated joining members may extend into their respective joining member slots to a depth greater than half of the height of the sidewalls.
[0012] The system may comprise fastening means for fastening the first and second elongated joining members into their respective joining member slots. The fastening means may be selected from the group consisting of screws, snap clips and spring clips. The fastening means may comprise screws for fastening a flanged portion of the elongated first and second elongated joining members to the crossplates of the first and second luminaires.
[0013] A close tolerance may exist between a thickness of the first and second elongated joining members and a thickness of their respective joining member slots.
[0014] A loose tolerance may exist between a width of the first and second elongated joining members and a width of their respective joining member slots.
[0015] The system may comprise a plurality of opposing aligning slots formed in the end faces of the first and second luminaires, and a plurality of aligning members insertable in the aligning slots.
[0016] The first elongated joining member may be rigid and the first joining member slot may comprise a straight cross-section.
[0017] The first elongated joining member may be flexible and the first joining member slot may comprise a curved cross-section.
[0018] In another aspect a system for connecting luminaires is provided. The system comprises: a first luminaire comprising an end face comprising a first slot and a third slot; a second luminaire comprising an end face comprising a second slot and a fourth slot; a first elongated joining member comprising first prongs; and a second elongated joining member comprising second prongs. The first slot and second slot may be laterally aligned and joined relationship to define a first joining member slot comprising a first wedged end. The third slot and fourth slot may be in laterally aligned and joined relationship to define a second joining member slot comprising a second wedged end. The first wedged end may be shaped to provide an interference fit with the first prongs wherein advancing the first prongs against the first wedged end forces the first slot and the second slot toward each other to tighten connection between the first luminaire and the second luminaire. The second wedged end may be shaped to provide an interference fit with the second prongs wherein advancing the second prongs against the second wedged end forces the third slot and the fourth slot toward each other to tighten connection between the first luminaire and the second luminaire.
[0019] The first and second wedged ends may each comprise outwardly and downwardly angled surfaces that define a first angle equal to or greater than a second angle defined by the first and second prongs.
[0020] The first luminaire may comprise a first U-shaped crossplate comprising a pair of first legs that at least partly defines the end face of the first luminaire, and the second luminaire may comprise a second U-shaped crossplate comprising a pair of second legs that at least partly defines the end face of the second luminaire.
[0021] The first luminaire may comprise a pair of first sidewalls that at least partly defines the end face of the first luminaire, and the second luminaire may comprise a pair of second sidewalls that at least partly defines the end face of the second luminaire.
[0022] The first slots may be formed in the first legs and the second slots may be formed in the second legs.
[0023] The first slots may be formed in the first sidewalls and the second slots may be formed in the second sidewalls.
[0024] The first slots may be formed partly in the first legs and partly in the first sidewalls, and the second slots may be formed partly in the second legs and partly in the second sidewalls.
[0025] The first and second elongated joining members may extend into their respective joining member slots to a depth greater than half of the height of the sidewalls.
[0026] The system may comprise a fastening means for fastening the first and second elongated joining members into their respective joining member slots. The fastening means may be selected from the group consisting of screws, snap clips and spring clips. The fastening means may comprise screws for fastening a flanged portion of the elongated first and second elongated joining members to U-shaped crossplates of the first and second luminaires.
[0027] A close tolerance may exist between a thickness of the first and second elongated joining members and a thickness of their respective joining member slots.
[0028] A loose tolerance may exist between a width of the first and second elongated joining members and a width of their respective joining member slots.
[0029] A plurality of opposing aligning slots may be formed in the end faces of the first and second luminaires, and a plurality of aligning members may be insertable in the aligning slots.
[0030] The first elongated joining member may be rigid and the first joining member slot may comprise a straight cross-section.
[0031] The first elongated joining member may be flexible and the first joining member slot may comprise a curved cross-section.
[0032] The foregoing discussion merely summarizes certain aspects of the inventions and is not intended, nor should it be construed, as limiting the inventions in any way.
BRIEF DESCRIPTION OF DRAWINGS
[0033] The accompanying drawings illustrate non-limiting example embodiments of the invention.
[0034] FIG. 1 is a bottom isometric view of a system according to an embodiment of the invention, showing two luminaires about to be connected.
[0035] FIG. 2 is a top isometric view of the embodiment shown in FIG. 1 , showing two luminaires connected.
[0036] FIG. 3 is a cutaway partial side view of the embodiment shown in FIG. 1 showing insertion of a joining member into a joining member slot to secure connection between the luminaires.
[0037] FIGS. 4A to 4C are a close up internal partial side views of the embodiment shown in FIG. 1 showing stages of insertion of the joining member into the joining member slot.
[0038] FIGS. 5A and 5B show close up internal partial side views of a joining member and a joining member slot according to another embodiment of the invention.
[0039] FIGS. 6A and 6B show close up internal partial side views of a joining member and a joining member slot according to another embodiment of the invention.
DESCRIPTION
[0040] Throughout the following description, specific details are set forth in order to provide a more thorough understanding of the invention. However, the invention may be practiced without these particulars. In other instances, well known elements have not been shown or described in detail to avoid unnecessarily obscuring the invention. Accordingly, the specification and drawings are to be regarded in an illustrative, rather than a restrictive, sense.
[0041] This invention relates to luminaires, and in particular to systems for connecting two luminaires together. Embodiments of the invention of exemplary commercial application are systems for end-to-end connection of elongated, channel-shaped luminaires. Examples of elongated, channel-shaped luminaires include the luminaires sold under the name PROFILE™ by Fluxwerx Illumination Inc. of Delta, British Columbia. Embodiments of the invention are also applicable to connecting luminaires of other shapes and in other configurations where a secure and discreet connection between luminaires, with connection components confined within relatively limited internal spaces of the luminaires, is sought; non-limiting examples include luminaires with curved sidewalls when viewed from above and below; and non-channel-shaped narrow luminaires such as the luminaires sold under the name VIEW™ by Fluxwerx Illumination Inc.
[0042] Claims of the invention relate to systems comprising a pronged joining member insertable into a corresponding joining member slot with a wedged end formed by respective slots of adjacent luminaires, wherein interference fit between the pronged joining member and the wedged end of the joining member slot provide an effective connection between the luminaires that is secure, discreet, and minimizes leakage of light from the boundary between the connected luminaires.
[0043] FIGS. 1 to 4 show a system 10 for connecting elongated channel-shaped luminaires 12 and 14 together according to an embodiment of the invention.
[0044] FIG. 1 shows system 10 with aligning members 16 which insert into internal aligning slots 18 formed in end faces 20 of luminaires 12 , 14 allowing luminaire 14 to be connected to luminaire 12 , in for example the direction of arrow 22 , in an end-to-end manner. System 10 is shown with two aligning members 16 . Some embodiments may have only one aligning member 16 or more than two aligning members 16 , with a corresponding number of aligning slots 18 . In some embodiments, instead of having aligning slots 18 formed in end faces 20 of both luminaires 12 and 14 , aligning slots 18 may be formed in end face 20 of one of the luminaires, with aligning members 16 fixed to and projecting from the other one of the luminaires. In some embodiments aligning members 16 and aligning slots 18 may be absent. In some embodiments other suitable features with similar function may be provided. In some embodiments end faces 20 , including aligning slots 18 , may be at least partially defined by legs 24 of crossplates 26 and/or sidewalls 28 .
[0045] In some embodiments, plates 30 bridging the interior cavities of luminaires 12 , 14 may be provided. Plates 30 block light that may otherwise escape from the lit interior cavities of luminaires 12 , 14 to between the exterior connecting seam 32 between sidewalls 28 of luminaires 12 , 14 . Plates 30 also cover the internal connecting seam between luminaires 12 , 14 , providing an aesthetically pleasing joint.
[0046] FIGS. 2 to 4 show system 10 with joining members 34 and joining member slots 38 . Joining members 34 and joining member slots 38 may be formed of any strong and durable material such as stainless steel, aluminum alloys, or the like. Joining members 34 are insertable in direction 36 into joining member slots 38 to secure the connection between luminaires 12 , 14 . In some embodiments the joining members may be rigid, for insertion into joining member slots with straight cross-sections (such as those illustrated in the Figures), for example in luminaires with straight sidewalls. In some embodiments the joining members may be flexible (e.g. made of a material such as spring steel), for insertion into joining member slots with curved cross-sections, for example in luminaires with curved sidewalls.
[0047] Joining member 34 includes prongs 40 at one end, an elongated body 44 , and a perpendicular flange 42 at the other end. Flange 42 may include fastening means 46 for fastening joining member 34 to luminaires 12 , 14 once joining member 34 is fully inserted into joining member slot 38 . In the illustrated embodiment, fastening means 46 comprises a screw extending through an aperture in flange 42 for engagement with a threaded bore 48 in crossplate 26 of luminaire 12 or 14 . In some embodiments fastening means 46 may comprise two screws, each extending through a respective aperture in flange 42 and engaging a respective threaded bore 48 in crossplates 26 of each of luminaires 12 , 14 . In some embodiments, any other suitable fastening means 46 may be employed to secure joining member 34 within joining member slot 38 and, depending on the fastening means 46 , flange 42 may or may not be present. For example, a snap clip or a spring clip may be used to secure joining member 34 within joining member slot 38 .
[0048] In some embodiments the length L J of joining member 34 may be greater than 50%, or greater than 75%, or greater than 90%, of the height H L of luminaires 12 , 14 , in order to ensure a secure connection between luminaires 12 , 14 and also to block light that may otherwise escape from an interior of luminaires 12 , 14 and out connecting seam 32 between sidewalls 28 of luminaires 12 , 14 .
[0049] Joining member slot 38 is formed by lateral alignment and joining of slot 50 of luminaire 12 and slot 52 of luminaire 14 , as shown best in FIGS. 4A to 4 C. Joining member 34 is slidably insertable in joining member slot 38 . In some embodiments, a close tolerance exists between the thickness of joining member 34 and the thickness of joining member slot 38 , where thickness is defined as the dimension going toward and away from the drawing sheet with respect to FIGS. 3 and 4A to 4C . In some embodiments, a loose tolerance exists between a width 54 of joining member 34 and a width 56 of joining member slot 38 .
[0050] As joining member 34 is initially inserted, there is typically a gap 64 between slots 50 , 52 . Prongs 40 of joining member 34 eventually contacts sloped surfaces 58 of respective slots 50 , 52 and due to the configuration and interaction of these components, gap 64 closes, as shown in FIGS. 4A to 4C and described as follows.
[0051] Sloped surfaces 58 of slots 50 , 52 are angled outwardly and downwardly. Sloped surfaces 58 , upon lateral alignment and joining of slots 50 , 52 , form wedged end 60 . Wedged end 60 and prongs 40 are shaped to provide an interference fit between them, such that as prongs 40 advance downward in direction 36 , slots 50 , 52 are forced together in direction 62 to form joining member slot 38 , thereby tightening the connection between luminaires 12 , 14 and eliminating any gap 64 . In other words, as joining member 34 is pushed down slots 50 , 52 , the force (e.g. downward force) along direction 36 is translated to forces (e.g. lateral forces) along directions 62 to secure luminaires 12 , 14 together. Interference fit is provided by having angle 68 defined by wedged end 60 be equal to or greater than angle 66 defined by prongs 40 . In the illustrated embodiment, angle 68 is greater than angle 66 .
[0052] Slots 50 , 52 are formed in end faces 20 of luminaires 12 , 14 . As described above, end faces 20 may be at least partially defined by legs 24 of crossplates 26 and/or the ends of sidewalls 28 . Accordingly, in some embodiments, slots 50 , 52 may be at least partially formed in legs 24 of crossplates 26 and/or in the ends of sidewalls 28 . In the illustrated embodiment, slots 50 , 52 are formed in legs 24 of crossplates 26 . In some embodiments slots 50 , 52 , and therefore wedged end 60 , may be symmetrical. In some embodiments slots 50 , 52 , and therefore wedged end 60 , may be non-symmetrical.
[0053] Accordingly, reducing and eliminating gap 16 has the advantage of increasing the aesthetic appeal of luminaires 12 and 14 and giving them a seamless appearance. Placing joining member 34 into joining member slot 38 in the crossplates 26 and/or sidewalls 28 of luminaires 12 and 14 , where joining member 34 is not visible, also has this advantage.
[0054] In some embodiments, the interference fit may be provided by other suitable shapes and configurations of the prongs and the wedged ends. FIGS. 5A, 5B, 6A and 6B illustrate examples of such other shapes and configurations.
[0055] FIG. 5A and 5B show joining member 134 with prongs 140 , slots 150 , 152 (which join to form joining member slot 138 and round end 160 ) with sloped surfaces 158 curving outwardly and downwardly. The radius 168 defined by round end 160 is equal to or greater than the radius 166 defined by prongs 140 to provide an interference fit between round end 160 and prongs 140 .
[0056] FIG. 6A and 6B show joining member 234 with prongs 240 , slots 250 , 252 (which join to form joining member slot 238 and wedged end 260 ) with sloped surfaces 258 angling outwardly and downwardly. The angle 268 defined by wedged end 260 is equal to or greater than the angle 266 defined by prongs 240 to provide an interference fit between wedged end 260 and prongs 240 .
[0057] Where a component (e.g. joining fork, luminaire, etc.) is referred to above, unless otherwise indicated, reference to that component (including a reference to a “means”) should be interpreted as including as equivalents of that component any component which performs the function of the described component (i.e. that is functionally equivalent), including components which are not structurally equivalent to the disclosed structure which performs the function in the illustrated exemplary embodiments of the invention.
[0058] This application is intended to cover any variations, uses, or adaptations of the invention using its general principles. Further, this application is intended to cover such departures from the present disclosure as come within known or customary practice in the art to which this invention pertains and which fall within the limits of the appended claims. Accordingly, the scope of the claims should not be limited by the preferred embodiments set forth in the description, but should be given the broadest interpretation consistent with the description as a whole. | A system for connecting luminaires is provided. The system includes: a first luminaire having an end face having a first slot; a second luminaire having an end face having a second slot; a first elongated joining member having first prongs. The first slot and second slot are in laterally aligned and joined relationship define a first joining member slot having a first wedged end, and the first wedged end is shaped to provide an interference fit with the first prongs wherein advancing the first prongs against the first wedged end forces the first slot and the second slot toward each other to tighten connection between the first luminaire and the second luminaire. | 5 |
FIELD OF INVENTION
The present invention relates to a method of preparation of a novel, solid-phase reagent that is useful in combinatorial synthesis for the creation of libraries of compounds for lead identification. More specifically, the method produces phosgenated oxime resins.
BACKGROUND
The facile manipulation of reactive functionality is a key factor in the development of efficient, high-yielding methods for combinatorial syntheses. For example, activated carboxylic acid derivatives have served as reactive building blocks in the solid-phase preparation of a wide variety of oligomeric and small molecule libraries. In most cases, the solid-phase protocol allows reactions on a polymer-bound scaffold to be driven to completion by making use of large excesses of reagents in solution that can be easily filtered away from the polymer support. After the scaffold has been modified, an additional cleavage step then frees the small molecule from the polymer support into solution for isolation. An alternative approach is to support a reagent or catalyst that can be used in excess to induce a chemical transformation on other reagents in solution, and once again, simple filtration can serve as a means for product separation and isolation.
Isocyanates are well known in the art to be useful intermediates in the production of pharmaceuticals and agrochemicals. A typical preparation of isocyanates involves the phosgenation of primary amines. Phosgene is a very reactive reagent, and many compounds have functional groups in addition to the primary amine which would also be react with phosgene. Therefore, many highly functionalized compounds cannot be prepared from the amine as the starting point via the isocyanate as an intermediate. Similarly, unsymmetrical ureas with different groups on each of the nitrogen atoms adjacent to the carbonyl, are also difficult to directly synthesize without the use of laboriously prepared protecting groups. A need exists to develop simple syntheses to overcome these problems.
The reaction of oximes with phosgene in solution phase to produce oxime-derived chloroformates is known in the art. Itoh et al. (Organic Syntheses, 59, 1975, 95-101 and Bull. of the Chem. Soc. of Japan, 50, 1977, 718-721) have used the reaction of various oximes with phosgene as part of a scheme to prepare a t-butoxycarbonylating reagent, which is used in peptide synthesis. The chloroformate that is formed is in the solution phase and is never isolated, but rather is used in situ. The use of the chloroformates in syntheses has the disadvantage that it must be stored and used under an inert atmosphere since they are very reactive and decompose in open air liberating HCl.
DeGrado and Kaiser (J. Org. Chem. 1980, 45, 1295-1300 and J. Org. Chem. 1982, 47, 3258-3261) have used an oxime resin as a solid phase reagent for peptide synthesis. A C-terminal amino acid is anchored onto the oxime resin as its oxime-derived ester, allowing further amino acids to be added stepwise by standard peptide coupling. Once the desired peptide is assembled, it is cleaved from the oxime resin by treatment with nucleophile such as hydrazine to afford the peptide hydrazide.
A functionalized polymer to serve as a vehicle to deliver reactive functionality, such as an isocyanate, into the solution phase, would be highly useful in the development of combinatorial syntheses for ureas, carbamates, sulfonylureas, hydantoins and other heterocyclic systems of biological importance. High yields, high recovery with few or no undesired side reactions, stability, and a suitability for automation are requirements to satisfy the need in the field.
SUMMARY OF THE INVENTION
The invention comprises the production of the novel reagent by the reaction of a source of phosgene with the polymer-bound reagent ##STR1## wherein Z is the recurring part of a carbonaceous polymeric backbone or sidechain thereof, Y is a pendant group of the recurring part of a carbonaceous polymeric backbone, and EWG is an electron withdrawing group. The reagent is useful as a phosgene transfer reagent in the production of isocyanates. The resulting composition is of the formula ##STR2## wherein Z is the recurring part of a carbonaceous polymeric backbone or side chain thereof and EWG is an electron-withdrawing group.
Additionally, the invention includes a process for preparing a solid phase reagent of the formula ##STR3## wherein Z is the recurring part of a carbonaceous polymeric backbone or side chain thereof, EWG is an electron-withdrawing group and R 1 NH--is derived from an initial primary amine addition of the formula R 2 R 3 NH.
The invention also includes a process for preparing a non-symmetrical urea of the formula ##STR4## wherein R 1 and R 2 are independently selected from a group consisting of optionally substituted alkyl or optionally substituted aryl and R 3 is independently selected from a group consisting of optionally substituted alkyl or optionally substituted aryl or hydrogen. The non-symmetraical urea is produced by contacting the solid phase reagent of the formula ##STR5## wherein Z is the recurring part of a carbonaceous polymeric backbone or side chain thereof, EWG is an electron-withdrawing group and R 1 NH--is derived from an initial primary amine addition with an amine of the formula R 2 R 3 NH.
DETAILED DESCRIPTION OF THE INVENTION
Applicant has invented a method to prepare a novel phosgenated oxime resin. The resin is useful as a solid-phase phosgene transfer reagent to primary amines. In particular, it is useful for generating isocyanates upon thermolytic cleavage of the oxime-derived carbamate.
As used herein the following terms may be used for interpretation of the claims and specification.
scaffold--molecular framework on which functionality is presented
trapping amine--amine used to trap isocyanate
unsymmetrical urea--urea derived from two different amines
protic input--a molecule containing a heteroatom attached to a proton
The use of solid phase reagents can overcome the limitations of the prior art by serving as a vehicle to deliver reactive functionality, such as phosgene, onto desired sites of a compound. With one site, such as the isocyanate, attached to the solid-phase reagent, other sites can be manipulated at will. Cleavage from the solid support will then allow the isocyanate to be further reacted to the desired end product. The instant invention overcomes the problem of instability of the isocyanate by the immobilization of the chloroformate as part of the solid phase reagent, allowing it to be isolated, characterized and further reacted without the use of an inert atmosphere.
Since the method provides for high yields, high recovery with little or no undesired side reactions, high stability, and is suitable for automation, it is an effective tool in combinatorial synthesis.
The solid support used has the formula ##STR6## wherein Z is the recurring part of the carbonaceous polymeric backbone, Y is a pendant group of the recurring part of a carbonaceous polymeric backbone, and EWG is an electron-withdrawing group. Any polymer in which the oxime-derived carbamate functionality can be added may be used. Suitable polymers include polystyrene and polyethylene. Preferred is polystyrene, wherein Y is a pendant phenyl group of the polymer.
Any electron-withdrawing group (EWG) that is unreactive to phosgene may be used. Suitable groups include nitro, cyano, dinitro, trifluoromethyl, di-trifluoromethyl, and halogens. Preferred is a nitro group.
Phosgenation can be performed with any source of phosgene. Sources include phosgene gas and triphosgene, a commercially available solid trimer of phosgene.
The phosgenated oxime resin can be used to prepare unsymmetrical ureas where the substitutions on the nitrogens are independently selected from the group consisting of hydrogen, optionally substituted alkyl, and optionally substituted aryl. At least one of the four possible substituents on the nitrogen atoms must be hydrogen whose origin can be traced back to the primary amine used in the initial addition to the phosgenated oxime resin. In the preparation of unsymmetrical ureas, the trapping amine can be either primary optionally substituted alkyl or aryl or secondary optionally substituted alkyl.
The phosgenated oxime resin can also be used to prepare carbamates where an alcohol is used in the thermolytic cleavage trapping step instead of an amine.
The method of synthesis permits the scaffolding between the two inputs, namely the primary amine and the trapping amine in the case of unsymmetrical ureas, to be minimized. In this case, the central scaffolding of the product is essentially a carbonyl group whose origin is traced back to the phosgene. The high reactivity of phosgene is controlled by the polymer support, which may be beads, film or other form having a high surface area. This method provides a very versatile tool for the combinatorial chemist to tie protic inputs such as amines and alcohols) together on a relatively small molecular scaffolding.
One reaction path is as follows: ##STR7##
EQUIPMENT AND MATERIALS
Toluene was distilled from sodium benzophenone ketyl and dichloromethane was distilled from phosphorus pentoxide prior to use. The solid phosgene equivalents, triphosgene and trhiophosgene were purchased from Aldrich and used directly. Amines were also purchased from Aldrich and used directly without purification. The oxime resin was prepared using Biobeads® SX-1 (1 % crosslinked polystyrene) from Biorad (Hercules, Calif.). Microanalyses were carried out by Micro Analysis Inc. of Wilmington, Del. IR spectra were obtained with a Perkin-Elmer FT1600. Low resolution mass spectra were obtained with a VG Trio-2000 quadrapole mass spectrometer using the electrospray atmospheric pressure chemical ionization (APCI) technique. HPLC analyses were performed on a Hewlett-Packard 1090 liquid chromatography system using a photodiode array detector and a Zorbax SB-C18 column.
EXAMPLES
The meaning of abbreviations is as follows: "h" means hour(s), "min" means minute(s), "sec" means second(s), and "d" means day(s).
EXAMPLE 1
PREPARATION OF OXIME RESIN
The oxime resin was prepared by the method described in DeGrado, W.F.; Kaiser, E.T., J. Org. Chem. 1982, 47, 3258-3261. Before use, the resin was pre-swelled in dichloromethane (75 mL) under an atmosphere of nitrogen, then allowed to shake overnight at room temperature. 6.0 g (20 nunol) of triphosgene was weighed out in the drybox, dissolved in dichloromethane (75 mL) and added to 20 g (15 mmol, based on loading of 0.755 nunol/g resin) of the oxime resin. Filtration of the loaded resin into a solution of ethanol in dichloromethane (to quench the remaining phosgene) followed by washing with liberal amounts of dichloromethane (ca. 350 mL) and drying under vacuum overnight afforded the ketoxime chloroformate. IR (KBr) showed a strong peak at 1799 cm -1 corresponding to the chloroformate. Cl analysis indicated the loading to be 0.663 mmol/g resin corresponding to an 88% yield.
EXAMPLES 2-9
Examples were performed following the general procedures outlined below. Substrates, products and results are given in Table 1.
1ST AMINE ADDITION
Phosgenated resin (3.0 mmol) was weighed into a 60 mL bottle. Amine (H 2 NR 1 , 9.24 mmol, 3 eq.) was weighed out and dissolved in dry dichloromethane (50 mL). Addition of the dichloromethane solution to the resin resulting in swelling of the resin and the resulting mixture was sealed and vortexed overnight at room temperature. Filtration of the resin followed by liberal washing with dichloromethane and then methanol (ca. 500 mL total) and drying under high vacuum overnight afforded urea-functionalized oxime resin. Verification of complete addition was determined by loss of the chloroformate peak and presence of the carbamate carbonyl peak between 1750 and 1760 cm -1 in the IR spectrum. These resins were taken directly to the thermolytic cleavage without any further characterization.
THERMOLYTIC CLEAVAGE AND TRAPPING AMINE ADDITION
Primary amine-functionalized resin (0.5 mmol) was weighed into a 20 mL vial and swelled with dichloromethane until saturated (ca. 6 mL). Amine (NHR 2 R 3 , 0.55 mmol, 1.1 eq. of non-volatile amines or 2.0 mmol, 4 eq. of volatile amines) was added and the total volume was taken to 18 mL with toluene. The vial was then sealed and heated on a vortexor heating block to 75° C. overnight. The mixture was allowed to cool to room temperature and the resin was removed by filtration and washed with dichloromethane (20 ML) followed by methanol (10 mL) three consecutive times. The combined filtrates were evaporated to dryness to afford the urea product which was characterized by mass spectroscopy directly without any purification. The low resolution mass spectra were obtained with a VG Trio-2000 quadrapole mass spectrometer using the electrospray atmospheric pressure chemical ionization (APCI) technique. Yields were also determined on the unpurified product. Purity analysis was performed by HPLC on aromatic-containing urea products. HPLC analyses were performed on a Waters 2010 liquid chromatography system using a photodiode array detecotr and a Vydac C18 colum, 2.1×150 mm, starting at 100% water/0.01% TFA->100% acetonitrile/0.01 % TFA. Results are indicated in Table 1.
EXAMPLE 10
The reaction was performed as in the Examples above, except that a Nautlius 2400 automated synthesizer (Argonaut Technologies, Inc., San Carlos, Calif.) was used to examine the dependence of yield on cleavage temperature. The individual reactor temperature of the cleavage step was independently controlled from 50° C. to 120° C., and the yield plotted versus temperature. These results are shown in Table
TABLE 1__________________________________________________________________________Ex-am- Obs.ple H.sub.2 NR.sub.1 R.sub.2 R.sub.3 NH Product mw M + 1 Yield Purity__________________________________________________________________________ ##STR8## Et.sub.2 NH ##STR9## 193.25 194.1 67% 83%3 ##STR10## ##STR11## ##STR12## 207.23 208.1 72% 92%4 ##STR13## ##STR14## ##STR15## 221.26 222.2 72% 79%5 ##STR16## ##STR17## ##STR18## 212.29 213.2 81% --6 ##STR19## ##STR20## ##STR21## 226.32 227.2 89% --7 ##STR22## Et.sub.2 NH ##STR23## 206.29 207.2 92% 93%8 ##STR24## Et.sub.2 NH ##STR25## 250.30 251.2 92% 76%9 ##STR26## ##STR27## ##STR28## 291.4 292.2 62% 82%10 ##STR29## ##STR30## ##STR31## 294.4 295.2 86% 98%__________________________________________________________________________
TABLE 2______________________________________Isolated Yield of Cyclohexyl-4-Biphenylurea as aFunction of Temperature______________________________________ ##STR32##______________________________________ | This invention relates to methods for preparing novel, solid-phase transfer reagents, specifically phosgenated oxime resins and non-symmetrical ureas, that are useful as supports in combinatorial synthesis for the creation of libraries of compounds for lead identification. | 2 |
[0001] This application hereby claims the benefit of U.S. Provisional Applications Nos. 61/274,828 and 61/274,829 filed on Aug. 21, 2009 and U.S. Provisional Application No. 61/286,885 filed on Dec. 16, 2009.
SEQUENCE LISTING
[0002] This application contains a Sequence Listing that has been submitted via EFS-Web and is hereby incorporated by reference in its entirety. The ASCII copy, created on Dec. 15, 2009, is named 3201-200.txt, and is 53,851 bytes in size.
BACKGROUND OF THE INVENTION
[0003] A. Field of the Invention
[0004] The present invention provides a method to identify and remove pathogen infected animals from a group/herd to prevent the spread of infection and preserve the health of the animals. In particular, PCR screening, utilizing primers appropriate to the pathogen, of both the animals and their environs unambiguously identifies active infections.
[0005] B. Description of Problem and Prior Art
[0006] Pathogens that infect farmed animals affect both the health and survival of the animals as well as the income of the farmers who raise the animals. For many pathogens, antibiotics are administered to the animals on an intermittent or continuing basis. However, the presence of the antibiotics or their by-products in consumable food products has raised concern about their long-term effect on human and animal health. Immunization against some pathogens is another possible approach, but vaccines for many animal diseases are either not available or are not cost effective. Yet, for other pathogenic organisms no antibiotic or vaccine treatment is available. Early detection of the infection and elimination/removal of the infected animals is the only method that can be used. However, serologic detection methods vary in their sensitivity especially during the early days of infection and may only detect an infection after the animal has started to make antibodies to the pathogen and may, itself, already be infectious.
[0007] One pathogen for which there is no effective treatment and no available vaccine is the pathogenic mink Aleutian Disease Virus (mADV). This virus was first described in 1956. All mink Aleutian Disease Viruses are single stranded DNA viruses of the parvovirus family. There are many strains of the virus, but only one known non-pathogenic strain (strain G) while the others are typically fatal. The pathogenic viral strains are absolutely devastating to mink farmers spreading quickly through mink colonies and contaminating the farm site through contact with the mink and their urine and feces. These viruses typically elicit a hyperimmune response in the mink with lethality arising from macro immuno-antigen complexes. The hypergammaglobulinemia condition inflames circulatory filtering organs such as the kidneys (glomerulonephropathy), spleen, and liver causing failure of these organs and death from the complications.
[0008] Attempts to find treatments for parvovirus infections have been reported. Alvarez et al. in U.S. Pat. No. 5,785,974 suggests that an immunogenic peptide in conjunction with other immunogenic complexes can be used to make a vaccine that can protect dogs, cats, pigs, and minks. However, the vaccines are proposed to be useful only against another parvovirus infection in mink, Mink Virus Enteritis (MVE) not the Mink Aleutian Disease Virus (mADV). Barney et al. In U.S. Pat. No. 6,054,265 describe peptides that can be used both for screening for certain viruses and for possible treatment. Among other viruses are listed the Mink Virus Enteritis (MVE) and the Aleutian Mink Virus (strain G). The patent basically deals with HIV identification and possible treatment methods are suggested for clinical treatment of infected patients. No direct application to infection with the deadly form of the Aleutian mink virus is discussed. Elford et al. In U.S. Pat. No. 6,248,782 teach that polyhydroxy benzoic acid derivatives are useful in the treatment of diseases caused by retroviruses as well as in the treatment of diseases caused by DNA parvoviruses. No specific example of treatment for mink Aleutian disease is given. As far as is known, none of the above suggested approaches to containing a fatal mink Aleutian disease outbreak has been successfully employed.
[0009] The inventive methods disclosed in this patent document are exemplified by the detection and eradication of pathogenic mink Aleutian disease virus from a farmed mammalian herd.
[0010] However, the methodological approach taught here is applicable to detecting and eradicating pathogens from any farmed mammalian herd.
DESCRIPTION OF THE FIGURES
[0011] FIG. 1 shows the number of mink deaths per week on a Pennsylvania farm infected with Aleutian mink disease for the years 2006 through December 2008.
[0012] FIG. 2 is a photograph of a typical electrophoresis gel showing the locations of the GAPDH and mADV marker amplicons.
[0013] FIG. 3 is the contiguous partial sequence corresponding to the Stahl mADV strain starting at approximately 272 bp and ending at approximately 4440 bp of the G strain (SEQ ID NO: 17).
[0014] FIG. 4 shows the DNA sequence of the ADV G-strain (SEQ ID NO: 18) alongside the contiguous partial DNA sequence of the Stahl mADV strain (SEQ ID NO: 19) so far determined. The alignment was obtained using Clustal W alignment utility located at http:///www.ch.embnet.org/software/ClustalW.html. Primers that worked are shaded while primers that did not work are underlined. The hypervariable region is underlined and identified.
[0015] FIG. 5A is the amino acid sequence (SEQ ID NO: 20) of one protein specified by the Stahl mADV that does not include the hypervariable region. This protein is found at the same region of the genome as a protein found in the G strain.
[0016] FIG. 5B is the amino acid sequence (SEQ ID NO: 21) of a second protein specified by the Stahl mADV that does include the hypervariable region. This protein is found at the same region of the genome as a protein found in the G strain.
[0017] FIG. 6 is a comparison of the partial amino acid sequences of several known mink Aleutian disease viruses aligned (SEQ ID NOS 22-31, respectively, in order of appearance). The hypervariable region is boxed (boxed sequence in StahlX1 disclosed as SEQ ID NO: 32).
[0018] FIG. 7A is an outline of the screening method of the invention indicating the type of test applied at each stage and the disposition of animals that tested positive and negative.
[0019] FIG. 7B is an outline of an embodiment of the screening method of the invention in which PCR mADV screening, but not antibody detection, in blood is used.
[0020] FIG. 7C is an outline of a preferred embodiment of the screening method of the invention in which the herd is retested by PCR screening during the period roughly from December to February.
[0021] FIG. 7D is an outline of a preferred embodiment of the screening method of the invention in which additional PCR testing of fecal material is performed at the time of whelping.
[0022] FIG. 7E is an outline of a possible method to identify and place non-permissive animals into a breeding herd.
[0023] FIG. 8A is a photograph of an electrophoresis gel showing the result of a composite placental manure PCR identification of mADV infection.
[0024] FIG. 8B is a photograph of an electrophoresis gel showing on the left the result of PCR screening of the four females from the composite placental manure sample of FIG. 8A . None are mADV positive. The offspring of three of the four females were all mADV negative. On the right of FIG. 8B is the result of PCR screening of the 7 offspring of the fourth female from the composite placental manure sample of FIG. 8A . PCR identified three of the seven offspring as mADV negative while four of the seven offspring were PCR positive for mADV.
[0025] FIG. 9 shows the number of mink deaths per week on a Pennsylvania farm infected with Aleutian mink disease for the years 2006 through September 2009.
DETAILED DESCRIPTION OF THE INVENTION
A. Characterization of a Rampant Epidemic Infection and Need for a Solution:
[0026] The consequences of mADV infection, both in terms of animal survival and of economic survival of the farmer, are extreme and a solution to the problem is urgently needed. Just how extreme the consequences are is highlighted by the experience of the inventors. As noted above, deadly mink Aleutian Disease Virus (mADV) infection can quickly spread through a herd with devastating consequences. FIG. 1 shows the number of mink deaths per week on a Pennsylvania mink farm run by the inventors that had previously been virus free. Prior to June 2006 relatively few deaths occurred generally arising from environmental stress on the herd. Each lineage of minks had been raised on the farm for at least 35 years. In May 2007 health problems in the herd were first noted with some animals having bleeding gums and blood infused water cups. E. coli was ruled out and mink ADV was considered a remote possibility since the farm had been mADV free since a mild strain was eliminated by standard husbandry techniques alone in the late 1960's. However, CIEP (counterimmunoelectrophoresis) testing on Jun. 12, 2007 indicted that approximately 30% of barren females were mADV positive.
[0027] Despite an extensive testing and animal segregation program using a blood antibody detection procedure (LFIA dipstick—Scintilla Development, Bath, Pa.) the infection continued to spread. Emptied pens that had contained positive animals were disinfected with Kennel Care, reportedly a broad spectrum parvocide. However, animals later transferred to these pens had a 90% reinfection rate, and it was concluded that this parvocide was not effective against mADV. By the end of September and the beginning of November, 2007 approximately 130-150 animals were dying per day as illustrated in FIG. 1 . By the end of 2007, the herd had been reduced from roughly 14,000 members and 3,000 breeders to 7,000. At lest 50% of the mink died, another 30% were symptomatic, while 15-20% appeared asymptomatic. The disease spread was unstoppable.
[0028] One choice for the 2008 raising season was to dispose of all the animals and start the herd with imported healthy animals. However, this would have meant losing decades of selective breeding and a unique gene pool. In addition, important value would be gained by keeping the naturally resistant mink that survived the epidemic. Realizing the inadequacy of the testing methods, for the 2008 season only 3,000 asymptomatic female breeders were kept with no further testing. However, 1,000 of the 3,000 animals were lost by March, 2008 and about half of the remaining 2,000 females never produced surviving offspring. Of the other 1,000 females, 600 produced diminished litters of 3 or less and 400 produced litters of 4 or more. These 400 animals and their litters were kept but those that subsequently became symptomatic were removed. By late July 2008 it was obvious that an accurate method of virus detection was urgently needed.
B. Development of PCR Based Virus Identification:
[0029] The problem for herd management with known antibody testing methods is that the tests detect antibodies produced only after the animal has mounted an immune response some significant amount of time after infection. In addition, the virus persists outside of the animals. Three tests had been in common use in herd management. IAT (iodine agglutination test) is non-specific for mADV and detects only 16-65% of positive CIEP reactors. It is not possible to eliminate mADV from the herd by culling with this test (Gorham, Henson et al., Infection [ 1976] pp 135-158). CIEP sensitivity is uncertain below antigen titers of 8-16. However, a false negative window exists for at least one week post-infection, and CIEP will not determine if the virus was eliminated from the host. The best results for CIEP (0.5-3.2% positive reactors) were determined 1 year post test. (Cho, Greenfield, J Clinical Microbiology, January [1978] pp 18-22). If time and resources are available, post exposure antibodies can be detected at a fairly early stage using an ELISA assay (enzyme linked immunosorbent assay). Under farm conditions where a large number of animals (hundreds to thousands) need to be screened, a LFIA strip (lateral flow immunoassay) may be used in place of ELISA. Finally, ELISA is consistently more sensitive than CIEP (95% vs. 65% or less) (el-Ganayni, Pub Med, [ 1992] pp 134-151) and is a rapid cost-effective method of detecting exposure to mADV. However, there exists a false negative window for three weeks post-infection. Further, the false negative rate experienced with LFIA can range from 4-14%. The test will not determine if the virus was eliminated from the host.
[0030] If possible to implement, clearly the best alternative available would be testing the animals for the presence of the nucleic acid of the mADV virus using Polymerase Chain Reaction (PCR). PCR can detect virus days after infection and at a very low level (less than 1 femtogram—about 10 genomes of ADV DNA in 2.5 μL of serum (Durrant, Bloom et al., J Virology, February [1996] pp 852-861)). There is the possibility of false negatives due to sequestration of the virus, and, for this reason, the test will not determine if the virus was eliminated from the host. However, the ability to unambiguously detect the presence of the virus makes PCR the best choice for monitoring a herd and eliminating the viral infection.
[0031] Unfortunately, as of approximately July 2008 no laboratory was immediately available to perform a PCR test for mADV particularly on the scale required (several thousand animals) and at a non-prohibitive cost. Further, most importantly, at that time it was unknown whether a PCR test existed that could detect the strain of mADV infecting the inventors' herd.
[0032] (1) Discovery of Appropriate Primers:
[0033] In order to develop primers suitable for PCR testing of the infectious mADV, the nucleotide sequence of the non-pathogenic Aleutian mink virus G strain was examined. This sequence had been published by Bloom. The nucleotide sequence was obtained from PubMed.com (NCBI Reference Sequence NC — 001662.1). In addition, primers to a universal target, mink glyceraldehyde 3-phosphate dehydrogenase (mGAPDH), were developed. The mGAPDH nucleotide partial sequence (Gram-Nielsen, et al.) was obtained from PubMed.com (GenBank: AF076283.1). Multiplex PCR utilizes more than one set of PCR primers in the same reaction to allow simultaneous amplification of more than one target sequence. In such a controlled reaction, one pair of the multiplex PCR primers is used to detect the presence of the target in question while the other primer pair acts as an internal control to a universal target and assures that the quality of DNA extracted and PCR condition/technique is successfully implemented. Multiplex PCR was used for all testing for the mADV.
[0034] The entire G strain sequence was entered into PrimerQuest (Integrated DNA Technologies, idtDNA.com), and possible primers identified following suggestions by the Integrated DNA Technologies' on-line IDT SciTools application. Approximately 50 different primer pairs were suggested. A best guess was made for the first primer pair to be tried and the primers were ordered. Astoundingly, the first primer pair attempted, V3-F/V2R worked and yielded an amplicon of ˜378 bp. Because this amplicon size was too close to the GAPDH amplicon size to clearly resolve on the electrophoresis gel, another primer pair, V3-F/V3-R, was tried, and it also worked and yielded a large amplicon easily distinguished from GAPDH. Shortly after this success, primers that span the hypervariable region (which was previously known by Bloom) were sought in order to identify the particular mADV strain infecting the herd.
[0035] Once primers were identified that covered the hypervariable region, the sequence of the hypervariable region was obtained. It was quickly realized that the mADV strain on the inventors' farm did not correspond to any strain in the published literature and was, therefore, a novel strain. The sequence of the Stahl mADV genome was determined as indicated below in Section B (2). Subsequent to the initial identification of the first primer pairs, portions of the G strain sequence were entered into PrimerQuest and possible primers suggested. Selection of several primer pairs were made based on a judgment of what might work. Other primer pairs were tried over a course of about ten months in order to both identify the best primers to use to detect mADV and to identify primers having a sufficient coverage over the genome in order to sequence the entire virus genome. As is well known, primer selection is still an art and not an exact science and much trial and error was involved in determining useful primers. Some of the primer pairs worked while others did not, possibly due to mutual inhibition or to the inability of a particular region to anneal well. Primer pairs were suggested by PrimerQuest based on “relative abilities” to work as a primer based on the input sequence (or partial sequence). The remaining portions of the G-sequence were entered this way to find primers in the remaining untried regions. The oligonucleotide primers themselves were obtained from Integrated DNA Technologies. The DNA extraction conditions for PCR utilized by the inventors are set forth in Appendix “A”. The PCR reaction conditions utilized by the inventors are set forth in Appendix “B”.
[0036] Table 1 lists several of the primer pairs generated, tested, and used in mapping and diagnostic screening based on the G-strain sequence. Those with amplicon sizes listed indicate that the pair worked well. As shown below, five of the primer pairs that were tried and expected to work have zero size indicating the pair did not work. The start and end positions numbers referenced correspond to the G strain sequence positions.
[0000] TABLE 1 Primer Amplicon Start End Conserved Conserved (For/Rev) Size (bp) (bp position) (bp position) Match (forward) Match (reverse) V1/V0 0 18 381 ?/24 23/24 V1/V1 0 18 932 ?/24 23/24 V1a/V1a 954 273 1227 ?/24 23/24 V2/V2 934 895 1829 24/24 21/24 V3/V2 378 1451 1829 23/24 21/24 V3/V3 883 1451 2334 23/24 24/24 V4/V4 981 2064 3045 23/24 24/24 V4a/V5a 0 2356 3325 23/24 21/24 V4b/V5b 999 2525 3524 24/24 24/24 V5/V5 802 3022 3824 24/24 24/24 V6/V6 0 3742 4766 21/24 ?/24 V6a/V6a 881 3559 4440 23/24 ?/28 V7/V6 0 4223 4766 25/26 ?/24
The oligonucleotide sequences of some of the above primers used include:
[0000] V1a: (SEQ ID NO: 1) 5′ - TTA ACG ACG GTG AAG GAG TTG CCT - 3′ (forward) (SEQ ID NO: 2) 5′ - TCT TCT GGA GTA AAG CAA CCA ACG - 3′ (reverse) V2: (SEQ ID NO: 3) 5′ - TGG TTA CTT TGC TGC TGG TAA CGG - 3′ (forward) (SEQ ID NO: 4) 5′ - TCC TCT GTT TAA GTG GCT CTG CGT - 3′ (reverse) V3: (SEQ ID NO: 5) 5′ - ACC ATC CTA ACC AAG CAA GGT GGA - 3′ (forward) (SEQ ID NO: 6) 5′ - ACA CGT GTC TTG GAG CAC TTC TCT - 3′ (reverse) V4: (SEQ ID NO: 7) 5′ - TGC CAC AAC TGC CAC GAA GAA TAC - 3′ (forward) (SEQ ID NO: 8) 5′ - ATT GGG TTG GTT TGG TTG CTC TCC - 3′ (reverse) V4b/V5b: (SEQ ID NO: 9) 5′ - CAG CAC TGG CGG CTT TAA TAA CAC - 3′ (forward) (SEQ ID NO: 10) 5′ - ACT ACC CTG TAA CCC TGC TGG TAT - 3′ (reverse) V5: (SEQ ID NO: 11) 5′ - GGA GAG CAA CCA AAC CAA CCC AAT - 3′ (forward) (SEQ ID NO: 12) 5′ - TTC AAA GTG TGT GCC TGA AGC AGC - 3′ (reverse) V6a: (SEQ ID NO: 13) 5′ - CAA CCA AAG GTG CAG GTA CAC ACA - 3′ (forward) (SEQ ID NO: 14) 5′ - GGA AGT ACA CAG TAT TTA GGT TGT TCA C - 3′ (reverse)
The primer pair used for mGAPDH is:
[0000]
(SEQ ID NO: 15)
5′- AAC ATC ATC CCT GCT TCC ACT GGT - 3′ (forward)
(SEQ ID NO: 16)
5′ - TGT TGA AGTCGC AGG AGA CAA CCT- 3′ (reverse)
[0037] As noted above, an initial attempt at diagnosing the presence of mADV via PCR utilizing primer V3 forward paired with V2 reverse yielded an amplicon of 378 bp. The size of this amplicon was too similar to the mGAPDH amplicon of 250 bp to be reliably separated on the electrophoresis gel. Therefore we ultimately chose an alternative mADV primer pair (V5) which would yield a larger amplicon (802 bp). This resolution was sufficient to clearly distinguish the mGAPDH and mADV amplicons. FIG. 2 is a photograph of a typical electrophoresis get and shows that the GAPDH and mADV amplicons are well resolved and separated. In addition, the V5 primers spanned the hypervariable region of the mADV (Bloom, et al.). This not only yielded an amplicon distinguishable from the mGAPDH amplicon, but also enables the strain typing of the viruses by subsequent sequencing of this amplicon from different viruses The V5 primer pair represents the preferred enablement and is used routinely as the diagnostic screening tool of choice for mADV.
[0038] As will be readily evident to those skilled in the art, in addition to the primer pair sequences listed above, the reverse complement sequences of the above forward primers could also work as reverse primers (i.e. reverse complement of V5 forward equals V4 reverse). Similarly the reverse complement sequences of the above reverse primers could also work as forward primers (i.e. reverse compliment of V4 reverse equals V5 forward). (This is easily seen illustrated in FIG. 4 .) In both these examples, a new primer companion would have to be selected because the direction of amplification would now be different. All primers disclosed should also function properly if at least approximately 85% of the bases are identical to the primer sequences identified and appropriately matched with a primer pair under slightly different annealing temperatures. As is evident to those skilled in the art, the disclosed primers should also function properly if 1 or more bases were added to the 5′-end and 1 or more bases truncated from 3′-end and similarly when 1 or more bases were added to the 3′-end and 1 or more bases truncated from 5′-end (when referenced to the G-strain sequence). In addition, as will also be readily evident to those skilled in the art, any nested primers, being a subset of the target region of the described primers, are included in the scope of this disclosure as are other primer pairs that overlap or are immediately adjacent to the primers described in detail above.
[0039] (2) Sequencing of Mink Aleutian Disease Virus:
[0040] A novel mADV strain has been identified based on DNA sequences obtained from mADV amplicons produced from the PCR reactions using the above selected primers. Amplicons were sent to GeneWiz (GeneWiz, Inc., South Plainfield, N.J.) for DNA sequencing. Overlapping DNA segments were assembled using DNA Baser software (dnabaser.com) to form a contiguous sequence. This sequence was compared to the only published full-length sequence G-strain mADV (Bloom, et al.) obtained from PubMed.com (NCBI Reference Sequence: NC — 001662.1) by the use of Clustal W software (npsa-pbil.ibcp.fr) and determined to be a contiguous partial sequence that starts relatively around 272 bp and ends around 4440 bp out of the 4801 bp total.
[0041] Table 2 illustrates the relative alignment positions and sizes of the mADV amplicons used to sequence the mADV genome in relation to the G-sequence (vertical bars). Progression over time is indicated from top to bottom starting with V3/V2 and ending with V7/V7. Hatched trellis regions indicate the part of the mADV DNA sequence obtained using the different primer pairs. Region 2.8 kb (horizontal bars along the top of the table) indicates the relative hypervariable region (3096-3134 bp). The assembled mADV contiguous region is depicted in the bottom row and was obtained from overlapping DNA sequences (273-4440 bp). It was assembled without any gaps by the use of the overlapping amplicons designed by proper primer pair placements. This is considered a partial sequence in relationship to the entire G-sequence since approximately the first 272 bp at the 5′ end and 361 bp at the 3′ end have not yet been identified.
[0000] TABLE 2
The primer pairs that span the hypervariable region are V5-F/V5-R and V4b-F/V5b-R. The contiguous partial sequence of the Stahl mADV strain is presented in FIG. 3 . While the standard procedure of starting the numbering sequence at “1” has been utilized in FIG. 3 , as noted above, the Stahl mADV sequence is a contiguous partial sequence starting about 272 bp in from the start of the G strain sequence.
[0042] A comparison of the nucleotide sequences of the G-strain and the Stahl strain is shown in FIG. 4 . The alignment information shown in FIG. 4 was generated using the Clustal W alignment utility located at http://www.ch.embnet.org/software/ClustalW.html. The strain identifications, numbers, and primer designated sites have been added to the Clustal W comparison. The primers that worked are shaded, while the primers that did not work are underlined. The hypervariable region starting at 3096 (G-strain reference) is labeled and underlined. The mADV contiguous sequence was BLAST searched against all other published sequences and no other identical match found (PubMed.com). The mADV sequence shown in FIGS. 3 and 4 is the first time identification of the sequence of the highly infectious mADV virus has been determined. In particular, it will be appreciated by those skilled in the art that any primer pair that spans the hypervariable region falling within the V5 primer pair including the nucleotide sequence of the hypervariable region disclosed in this patent document will generate a PCR amplicon specific to the Stahl mADV strain. Further, since the hypervariable region specifies the strain type, use of such a primer pair that spans the hypervariable region with other ADV strains will permit an accurate strain typing that can be used to not only identify the strain but also to trace infections from place to place, herd to herd.
[0043] Thus, while other methods of performing PCR have been developed (such as rapid PCR techniques using fluorescence resonance energy transfer probes) that do not rely on electrophoresis gel determinations, any such technique that relies on the amplification or identification of the sequences disclosed in this patent document is considered to be encompassed by the present disclosure.
[0044] FIG. 5 shows the amino acid sequence of two proteins predicted from the partial nucleotide sequence determined for mADV. FIG. 5A shows the amino acid sequence of one protein specified by the Stahl mADV that does not include the hypervariable region. This protein is found at the same region of the genome as a protein found in the G-strain. FIG. 5B shows the amino acid sequence of a second protein specified by the Stahl mADV that does include the hypervariable region. This protein is found at the same region of the genome as a protein found in the G-strain. The sequences were generated using the ExPASy Proteomics Server, Swiss Institute of Bioinformatics (http://www.expasy.ch/tools/dna.html). FIG. 6 is a comparison over a limited span of the amino acid sequences of several mink viruses including the G-strain and the Stahl strain. To generate FIG. 6 , a nucleotide BLAST search was conducted using the Stahl strain nucleotide sequence as the query on PubMed.com (http://blast.ncbi.nlm.nih.gov). Several similar DNA sequences obtained were selected for translation using ExPASy. The resulting amino acid sequences were then aligned using a CLUSTAL W protein alignment utility (http://npsa-pbil.ibcp.fr/cgi-bin/npsa_automat.pl?page=/NPSA/npsa server.html). The comparative sequences span the hypervariable region (indicated by the box). The amino acid sequence of the Stahl strain clearly differs from the others in several locations. Several different single nucleotide polymorphisms (SNP's) were identified within the Stahl strain DNA sequence. The differences in the DNA base at these positions each produce a change in the corresponding coded amino acid. This type of variant is known as nonsynonymous because a different polypeptide is produced. Table 3 shows some SNP's identified by the DNA location and resulting change in coded amino acid.
[0000] TABLE 3 SNP location (bp) Nucleotide = Amino Acid 301 T > G = H > Q 412 A > G = I > M 575 T > C = F > L 908 T > A = C > S 1059 G > C = S > T 1068 C > T = T > I 1078 A > C = E > D
It is unknown at the time of drafting this patent document whether the identified changes are responsible for the virulence of the Stahl strain. There are indications in the literature that other sites along the amino acid chain may also be involved in determining the relative virulence of the viruses.
C. Procedure for Elimination of Pathogens from a Farmed Herd:
[0045] In order to eradicate a rampant epidemic infection from a herd, all testing methods available are used. In the case of a mink farm, both an antibody detection method (ELISA or LFIA) and PCR are used. However, even before animal inspection and testing can begin, a virus free clean facility needs to be created so that animals transferred out of the infected herd are not reinfected. Appendix “C” outlines the sanitation procedure used on the farm. Importantly, Oxine solution with and without added detergent has been found to be an effective parvovirus viracide. Before cleaning with any product, care should be taken to ascertain that product will inactivate the infecting pathogen. In particular, environmental PCR testing as described in Appendix “E” should be employed.
[0046] Once a clean facility has been obtained, animal selection and testing can begin. FIG. 7 shows in outline form the methodological sequence originally employed to identify and remove infected animals from the herd. Initially a visual examination of the animals is made to observe any animals showing clinical symptomology. Clinical signs such as lethargy, poor appetite, underweight, ventral staining, discharge from the mouth and bleeding gums are all indications but not proof of an infected animal. Considering the consequences of keeping a potentially infected animal in the herd, no consideration at this time on an infected farm is given to the actual clinical cause of the observed condition of the animals. These animals are immediately removed from the herd, and, in the case of mink, are pelted. Only visually asymptomatic animals are considered for testing. Urine samples are obtained from these animals. For mink, urine is collected from a suspended cup placed below the animal and above the manure pile. The urine is tested with an antibody detecting method (ELISA may be used but the use of a LFIA strip provides a quick result and is easily employed in the field). LFIA can only detect antibodies after the 14-21 days it takes for the animal to mount a sufficient immune response. However, a positive urine antibody test (using LFIA) on an asymptomatic animal indicates a prolonged and persistent viral infection and that sufficient renal damage (glomerulonephropathy) has already occurred from antibody/antigen complexes. Healthy animals will not excrete antibodies in urine unless the renal system has deteriorated. The antibody positive animals are removed from the herd, and, in the case of mink, are pelted.
[0047] An antibody negative urine animal is now a candidate for further antibody testing of its blood. ELISA or LFIA may be used. Again, as noted above, LFIA is more conveniently used. LFIA testing of blood is a more sensitive test and does not rely on extensive renal damage having occurred. Blood is collected for both antibody testing and PCR testing at the same time according to the method described in Appendix “D”. Whether the blood tests positive or negative for antibodies, the blood is still subjected to further PCR testing. In the case of an animal with antibody positive blood, it is possible that the animal has acquired a natural immunity to the virus and should be kept in the herd. If the blood PCR test indicates virus present in the antibody blood positive animal, the animal is removed from the herd. If the blood PCR test indicates no virus present in the antibody blood positive animal, the animal is kept in the herd and identified as antibody (+) virus (−). If the blood PCR tests positive for virus present in the antibody blood negative animal, the animal is removed from the herd. If the blood PCR test indicates no virus present in the antibody blood negative animal, the animal is kept in the herd and identified as antibody (−) virus (−). At this point in the selection process, both the antibody (+) virus (−) and the antibody (−) virus (−) animals are kept in the herd.
[0048] After some experience utilizing the above outlined protocol, it was appreciated that nothing was being gained by testing the blood for antibodies. The subsequent PCR test for viral presence is a necessary and sufficient selection criterion. PCR mADV positive blood tests indicate an infected animal and indicate that the animal should be removed from the herd. However, as in the earlier protocol where antibody positive PCR mADV negative animals were not removed from the herd (since the antibody presence probably resulted from the animal naturally mounting a sufficient immune response to the virus) in the revised protocol PCR mADV negative animals are kept in the herd. The preferred protocol embodiment of the invention is outlined in FIG. 7B .
[0049] As the animals are characterized and the infected animals removed or destroyed, the healthy animals are transferred to sanitized pens. For this transfer, the animal is caught with Oxine soaked gloves (500 ppm), placed in a small carrier and dowsed repeatedly in a 200 ppm solution of Oxine.
[0050] Into this solution is also added a small amount of dish washing soap to aid as a surfactant for the aqueous Oxine solution to penetrate the highly hydrophobic under wool. In this manner, the external surface of the animal is treated as completely as possible with Oxine. Oxine aids in the elimination of environmental virus on the mink. It has been discovered that it is possible to have a viral blood negative mink in a viral positive pen. Swabbing of the tops and bottoms of pens and analysis of the swabs by PCR revealed that the top of the pen was usually more contaminated than the bottom of the pen. In such a pen, a virally negative mink either was not yet infected or the viral load was not yet sufficient to cause an infection, but the virus may be carried on the outside of the body. When a mink from an infected pen is moved into a clean area, it may unknowingly cause a reinfection at a later date. Thus, passing the viral PCR tests is not sufficient to maintain a virus free herd without also sanitizing the exterior of the mink. The 200 ppm Oxine solution was not found to have any effect on the eyes or mucus membranes of the mink and is an effective tool for killing the virus in the mink's coat. Only after undergoing this cleansing methodology was a mink placed into a freshly sanitized, quarantined, windward area of the ranch.
[0051] However, it should be appreciated that it is possible that a recently infected animal may not be detected by PCR testing. Accordingly, retesting of the animals using the preferred PCR protocol may be required to either confirm the absence of the virus in the herd or to remove any remaining infected animals. Based on the inventors' experience, it is believed that the optimum windows for testing are December during pelting, late February prior to breeding, and whelping season. PCR retesting according to the protocol set out in FIG. 7C of the mink herd on the inventors' farm two months after the above described testing and selection process discovered that about 1.5% of the females and less than 1% of the males were still infected. In addition, the pens of these animals were resanitized and left dormant. As can be seen in FIG. 9 , the viral elimination protocols outlined above substantially reduced the mink mortality for 2009. It should be noted that a variety of causes unrelated to mADV infection result in some level of mink mortality as is reflected in FIG. 9 for 2009. However, it should also be appreciated that the viral elimination protocols and hygienic cleaning of the farm result overall in a much healthier herd.
[0052] Another method of monitoring the health of the herd has been discovered using placental manure screening that will be described below.
D. Procedures for Continued Monitoring of an Animal Herd:
[0053] In a large farm consisting of potentially many thousands of animals, the cost in time and expense of utilizing the protocols outlined above for eliminating a contagious infection from the herd is a relatively small fraction of the loss attributable to the decimation of the herd population. Once a relatively infection free herd is established, other ongoing monitoring protocols can be utilized.
[0054] (1) Placental Manure Sampling:
[0055] The females of many mammalian animal species, including mink, soon after giving birth devour the discharged placenta. Malformed or dead offspring may also be consumed. The reason for this behavior is not well understood but may be linked to the need for hormones to reduce uterine bleeding (in mammals). In the case of mink, shortly after consumption of the placenta, the female mink passes a black, tarry, and shiny stool. Typically the stool is found in a far corner of the pen or even on the ground. If deposited relatively soon prior to discovery, the stool is easily sampled by inserting a small diameter tube a fixed distance into the medium to collect a sample size of approximately 35 uL. This sample is placed in a labeled tube for submission for PCR. If the stool has been deposited for some time and the weather conditions are dry, a hard skin begins to form around the medium that must be broken for internal sampling.
[0056] Using PCR methods described above to analyze a sample of the stool, it has been discovered that mADV can be detected in animal manure as shown in FIG. 8A . The placental stool PCR mADV screening enables the removal from the herd of the affected dams and litters the day of whelp. Very importantly, this method provides a non-invasive and non-tactile method of screening that does not disrupt the mink during this period with unnecessary handling. In addition, the method minimizes the spread of the disease through contact and handling at the beginning of the spring and summer (the whelping season), the most contagious times of the year. When a positive manure sample is identified, the animals are removed from the herd, and, in the case of mink, euthanized. To reduce the likelihood of the spread of infection, the litters adjacent to the infected litter are removed to pens on the leeward side of the ranch for quarantining and observation as an extra precaution. All empty pens are then cleaned and resanitized as taught previously. Most importantly, since the stool contains material from all the offspring as well as the mother, analysis of the stool by PCR discovers infection in the offspring as well as the mother. Based on the discovery of pathogen detection by PCR in the placental manure of mink, detection of pathogen infection in the placental manure of other species in which the mother consumes the placenta may be accomplished by PCR analysis for a representative pathogen nucleotide sequence.
[0057] On a ranch where the virus has been substantially eliminated according to the protocol methods of the present invention, to reduce the number of manure samples to be analyzed by PCR, sampling of composite birth stools from several animals can be used as an economical and rapid method for virus detection. For example, it has been found that composite pooling of samples from four females where one sample is positive for the virus will reveal the entire composite to be positive. (See FIG. 8A .) FIG. 8A shows the results of PCR mADV analysis of 9 different pooled placental manure samples. As shown, the mADV virus was found in one pooled sample. Thus the dilution factor of the sample is not a concern due to the high sensitivity of the PCR method. Higher pooling numbers are possible but the limits have not been explored as of yet. It is very important to record all members of the pooled sample and the location of each of the members for future reference should PCR mADV analysis of individual samples be required. In all cases of a PCR mADV positive composite sample, the individual samples that made up the composite will have to be retested by themselves to find which of the pooled samples had the infection so that the positive animals associated with that sample can removed from the herd. Farms that have a history of the disease may not be able to afford high pool numbers due to the greater probability of positive samples.
[0058] Screening during the whelping season of the placental manure of all animals in the Pennsylvania herd after the elimination of infected animals according to the protocol methods of the present invention set forth above yielded some interesting results. Two composite placental manure samples (four dams in each composite) were PCR positive for mADV. As noted above, FIG. 8A shows the screening result for composite samples indicating that one composite sample was PCR positive for mADV. PCR analysis was then applied to samples from each dam and their offspring in the two PCR mADV positive composite pools (not shown). In the first positive composite pool, 3 dams and all of their offspring were PCR negative for mADV. The remaining dam and her offspring were PCR positive for mADV. Clearly, dilution by composite pooling did not affect the accurate PCR detection of mADV. The PCR mADV positive animals were removed from the herd.
[0059] PCR mADV analysis of animals in the second positive pool was surprising. The results of the individual screening for these animals is shown in FIG. 8B . FIG. 8B shows the PCR results for all four females (on the left of the central ladder column) and the seven offspring of one female (on the right of the central ladder column). All four females were found to be PCR mADV negative. Three of the four litters (18 offspring) were also PCR negative for mADV (not shown). The fourth PCR mADV negative female had a litter of 7 offspring in which 3 of the 7 were PCR mADV negative while 4 of the 7 were PCR mADV positive as shown on the right of the central ladder column of FIG. 8B . Two very important discoveries come out of this data. First, PCR testing of the placental manure picked up mADV infection in the offspring. Suprisingly, PCR mADV testing also revealed the presence of an otherwise healthy and PCR mADV negative female that carried the mADV virus and was capable of passing the virus on to her offspring. Screening by the composite sampling method permits not only the identification of infected animals that were kept in the herd having passed the initial screening tests, but, most importantly, also permits the identification of carrier animals that need to be removed from the herd in order to eliminate all infection from the herd. It is probable that the PCR mADV negative female animal was “non-permissive”; that is, the virus is unable to infect the animal's cells even though virus particles remain sequestered in the animal. The female apparently passed on her “non-permissive” genome to 3 of her offspring but not the other 4. Prior to this discovery, the relevant literature has taught that the vertical transmission of disease caused by mink disease virus was 100%. The results shown in FIG. 8B clearly indicate otherwise.
[0060] This is the first indication that there is some genetic variation in mADV susceptibility occurring between generations, and that there is a genetic basis that makes the animals non-permissive. Clearly, all the fetuses develop simultaneously in utero and are simultaneously exposed to the virus, but the virus does not affect some of the fetuses. Interestingly, antibody testing of the non-permissive dam also did not indicate any antibodies. Based on this example, there is a strong suggestion that a genetic solution to the mADV infection problem may be found. Not only is placental manure screening a cost and time effective way to monitor the health of the herd, it is particularly important as a way to identify non-permissive animals as early as the whelping day so that infected animals can promptly be removed from the herd before there is an opportunity for them to pass on the virus. The full screening protocol setting forth the most preferred embodiment is shown FIG. 7D .
[0061] In the future, the inventors intend to try to identify the genetic markers that are responsible for the “non-permissive” characteristic with the hope that, with knowledge of the gene sequence identifying the non-permissive characteristic, a whole herd can be created that is resistant to mADV. Alternatively, the identification of non-permissive animals using PCR for mADV on placental manure samples, also raises the interesting possibility of creating, by breeding, a herd of animals all of which possess a non-permissive genome. At this time it is unknown whether breeding non-permissive animals with other non-permissive animals will produce a stable gene line of non-permissive animals. A possible alternative scenario for establishing a breeding herd of non-permissive animals is set out in FIG. 7E . Instead of pelting the kits that are identified by a PCR mADV positive unpooled manure sample, the kits are individually retested by PCR for mADV. Some of the kits will test positive since they are the source of the positive manure sample. Any PCR mADV negative kits would be segregated and used to establish a non-permissive herd. At this point it would be unknown whether the kits harbor a sequester virus and would transmit the virus to their offspring. Any remaining PCR mADV positive kits as well as the PCR mADV negative dam that is now known to harbor the virus would be pelted. Repetitive identification and segregation of non-permissive animals in subsequent generations should establish a gene line that breeds true for non-permissive animals.
[0062] (2) Saliva Sampling:
[0063] Finally, for continued monitoring of the herd, an alternative saliva collection process for PCR can also be employed. Saliva can be collected from mink by allowing them to bite upon a thin plastic tube or string or absorbent material such that sufficient saliva is collected. No handling of the animal is required which lessens the transmission of the disease and speeds collection. Typically this sampling is best achieved just prior to feeding time for the animals as they are very aggressive towards objects placed through the wire cage. The chewing process on the tube or string or other material is sufficient to deposit enough saliva for nucleic acid detection. Return visits may be required for animals that are not compliant.
[0064] One caution for this method is that the sampling tube or string or other material may not touch the wire cage since environmental virus is likely to be included in the sample. Care must be taken at this point to ensure that no contamination results before the sample is safely placed in its labeled sampling container. As taught before with respect to sample acquisition for antibody testing (LFIA) and PCR testing, the sampling lid is opened and the portion of tube or string or other material is cut off allowing it to fall into the container and then the lid is closed. Specific duties of each hand are practiced as described in Appendix “D”.
[0065] (3) Demonstration of Elimination of Pathogen From a Herd:
[0066] The success of the screening method taught in this patent document can clearly be seen by examination of FIG. 9 which extends the data of FIG. 1 for the year 2009. It is immediately evident beginning in the late fall of 2008 that, after employing the testing and selection method taught in this patent document, the death rate had fallen at least to the levels observed before the mADV outbreak, if not even lower. The reason the death rate is never zero is due to the fact that some deaths naturally occur due to environmental stress and other factors. However, the method taught herein has clearly been successful in eliminating the mADV epidemic.
[0067] The method of the present invention has been exemplified by application to the elimination of mADV from a mink herd. The basic principles of screening using PCR detection of a pathogen's nucleic acid signature, with or without additional screening technologies such as antibody testing (ELISA or LFIA) to identify and remove infected animals from a herd has general applicability to a wide range of animals. The techniques may even be extended to populations of wild animals particularly through the PCR testing of manure.
[0068] The discovery of primers that can identify the lethal mADV permits the assembly of testing kits that may be employed on mink farms. Simple kits may contain just the primers for mADV with the users supplying reference primers and laboratory facilities. More advanced kits may contain not only the mADV primers but also the GAPDH or other internal reference marker primers along with the remaining materials required to screen by PCR.
Appendix “A”
DNA Extraction
[0069] Samples received for detection of mink Aleutian Disease Virus (mADV) were processed using RNase/DNase free microcentrifuge tubes and sterile pipette tips containing aerosol filters. Samples collected consisted of 2mL microcentrifuge tubes containing either:
[0070] 1. Blood soaked cotton swab
[0071] 2. Urine soaked cotton swab
[0072] 3. Environmentally obtained sample on wetted cotton swab
[0073] 4. Manure sample inside small diameter tube(s)
[0074] 5. Placental manure sample inside small diameter tube(s)
[0075] 6. Blood collected in heparinized glass or plastic capillary tube
[0076] 7. Blood collected from pipette tip
[0077] 8. Blood collected and dried onto Qiagen QIAcard
[0078] 9. Saliva collected on applicator
[0079] Total DNA from cotton swab and small tube samples was extracted and purified using Qiagen DNeasy Blood & Tissue Kit (Qiagen, Inc., Valencia, Calif.). The suggested manufacturer's protocol “Purification of Total DNA from Animal Blood or Cells (Spin-Column)” was performed. Minor changes were incorporated into the protocol for manure and placental manure samples. For samples containing more than one small tube, the Master Lysis Buffer volume was increased two fold, samples were applied to Spin Columns/Collection Tubes in 2 sequential loading applications (due to increased volume), 8000 rpm spins for 1 minute were increased to 9000 rpm for 3 minutes, and 13600 rpm spin for 3 minutes increased to 6 minutes. Total DNA from cotton swab, small diameter tube, capillary tube, pipette tip, QIAcard (excised 2.5 sq mm), and saliva applicator samples was extracted using Epicentre QuickExtract DNA Extraction Solution (Epicentre Biotechnologies, Madison, Wis.). The suggested manufacturer's protocol was performed with the following changes: for cotton swab and small diameter tube the volume of QE used was 100 uL and for capillary tube, pipette tip, QIAcard, and saliva applicator the volume of QE used was 50 uL. The final solution was diluted 1:4 with DNase free water (Boston BioProducts Inc., Worcester, Mass.). PCR methods including extraction methods and PCR techniques are undergoing rapid developments including advances in instrumentation. The processes described above and below are currently practiced on the inventor's farm. However, these methods should not be considered limiting and advanced PCR techniques can be employed in the overall method described in this patent document.
Appendix “B”
PCR Reaction Conditions
[0080] Extracted DNA, oligonucleotide primers, and GoTaq Green Master Mix (Promega Corporation, Madison, Wis.) were mixed together following Promega's suggested protocol for PCR. Mineral oil was added to samples before placing them in PerkinElmer 480 Thermocycler (PerkinElmer, Waltham, Mass.). Basically, the PCR steps included initial denaturation (95° C. for 2 minutes) followed by a 40 cycle loop of denaturation (95° C. for 30 seconds), annealing (see table below), and extension (72° C. for 1 minute), and then final extension (72° C. for 5 minutes) with a hold at 4° C. The following table summarizes primer and PCR conditions:
[0000]
TABLE 4
Swab
Multplex
GAPDH
ADV
Anneal
DNA
Small Tube
QE DNA:H2O
GAPDH
(uM)
(uM)
(° C.)
(uL)
DNA (uL)
1:4 (uL)
V1a
No
—
0.1
57
3
—
—
V2
No
—
0.6
55
5
—
—
V3
Yes
0.2
0.4
57
10
—
—
V4
No
—
0.1
55
5
—
—
V4b/V5b
No
—
0.4
57
6
—
—
V5
Yes
0.2
0.4
57
10
5
5
V6a
No
—
0.1
57
10
—
—
[0081] Completed PCR reactions were subjected to agarose electrophoresis. PCR products (amplicons) were visualized by UV fluorescence using GelRed Nucleic Acid Stain (Phenix Research Products, Candler, N.C.) incorporated in the agarose. The presence of the GAPDH amplicon (250 bp) in the sample indicated that (cellular) DNA was extracted correctly and PCR performed properly. Appearance of the mADV amplicon (802 bp for V5) indicated the presence of viral DNA in sample.
Appendix “C”
Cleaning/Sanitation
[0082] After removal of mink from the area, the first steps in cleaning are described as “dry cleaning” whereupon any remaining feed, manure, and other debris is scrapped from the pens and used bedding materials are removed from the boxes and allowed to fall to the ground. Next the manure, bedding and other materials are removed as much as possible and taken to a compost pile outside and downwind from the ranch. Spreading of this material is not recommended as virus may spread to feral animals and perpetuate the infection outside of the farm. Layering of manure and “quick lime” (Ca0) to this compost pile has been recommended to raise the pH to unfavorable levels for the AD virus to survive.
[0083] If boxes are removable from their pens, they are immersed in a 3% NaOH solution as well as any other wooden-ware associated. These are then cleaned typically with a cleaning machine delivering 4 GPM @ 3000 PSI @ 190 degrees F. The outside surfaces of the box are done first finishing with the inside surfaces. Other parts are cleaned similarly whereupon the box with its parts are removed from the shed and immersed in a 500 ppm solution of Oxine (Bio-Cide International, Norman, Okla.) and palletized in a way for air circulation for the natural drying of the Oxine solution from the boxes. Afterward they are stretched wrapped for protection and taken to clean storage until needed.
[0084] The next phase of cleaning addresses the wire pens and inside surfaces of the shed. In one method the pens are sprayed with a 3% NaOH solution with the optional addition of a foaming agent to enhance maximum contact to the extremely large surface area involved. While this is soaking, the inside roof and other areas are sprayed with a detergent [Complete Plus, (Camco Chemical, Madison, Wis.)], again with the optional use of a foaming agent. The 3% NaOH solution is not recommended on surfaces that are aluminum such as shed roofs so the use of a detergent is used instead. Rinsing of the inner roof surface and other structural parts of the shed is preformed with the same machine initially before the wire pens are done working in a top to bottom fashion. The pens are carefully rinsed in a manner that directs the spray to as many angles possible to minimize shadowed areas formed by the spraying action. The pens are then sprayed with a 500 ppm solution of Oxine and allowed to air dry. Again the addition of a foaming agent enhances the contact time and completeness of the sanitizing solution. The final step of preparing the shed is to broadcast CaO inside and outside of the shed by use of a garden pulled lawn broadcaster. The CaO is applied at the rate of approximately six pounds per square yard. The shed remains in this state until just prior to moving in PCR mADV negative animals. At that time, immediately before the shed is utilized, a second application of 500 ppm Oxine is applied to the pens to ensure sanitation before use. Under all circumstances, strict ranch hygiene is absolutely essential for the successful implementation of eradication of the disease. Animal testing alone will not ensure elimination of a pathogen without adherence to the highest levels of biosecurity.
Appendix “D”
Blood Collection Process for Antibody (ELISA or LFIA) and PCR Testing
[0085] To minimize the transmission of the disease during this procedure, a technique of using Oxine soaked handling gloves is employed as to provide a sanitizing surface for any bodily fluids from the animals to be neutralized upon contact. The gloves are soaked in a 500 ppm solution of Oxine until saturated and the handler first dawns a pair of latex gloves before the soaked catching gloves to protect his/her hands from the long term exposure to the Oxine solution. The mink are carefully caught as to avoid contact of the rear feet with the Oxine laden gloves as it was discovered that Oxine will produce a false positive reaction on LFIA test strips when incorporated with the blood sample (personal communication).
[0086] The handler holds the animal horizontal with the rear feet to him/her and extended beyond the pen with the fore feet placed firmly on the top part of the pen while gently rolling the animal to the left side to raise the right rear foot upward. The sampling person prepares to acquire the blood sample. Since a third hand is required, the mouth of the sampler may be used to hold the stem ends of the sterile cotton swabs while the right hand holds the clippers and is the only hand used to open and close sample containers. Reproducible non-cross contaminating sample acquisition is crucial at this stage. It is imperative that the sampler maintains a clean hand, usually the most dexterous one, and a sampling hand, one that is in repetitive physical contact with the animals. The two hands never exchange duties and maintain their respective operations.
[0087] The technique of blood collection is best preformed as follows. With the left hand, the sampler firmly grabs the elevated right rear foot of the mink such that the foot pad rests completely on the left thumb of the sampler. With the right hand, the sampler skillfully clips a toenail, preferably from the smallest, last digit, just above the quick line with a small pair of toenail clippers maintaining the grip with his left thumb and left fore finger of the left hand. Blood will flow momentarily or, if not, a second clipping may be required or a slight relaxation of the grip may allow the flow of blood to proceed. The sampler removes from his mouth a sterile cotton swab with his clean right hand and acquires first the sample for blood LFIA. The stem of the swab is transferred to the released left hand, the pre-labeled sample container lid is opened with the thumb and fore finger of the right hand and the cotton head of the blood soaked swab is cut with the clippers still held in the right hand just above the cotton head. The lid is closed with the right thumb and fore finger. The stem of the swab is discarded with the left hand and is then used to re-grip the animal's right rear foot as before. Secondly, the sample for blood PCR is acquired in the same fashion excluding any contact with anything other than free flowing blood from the toenail to avoid environmental virus contamination. This process is repeated using the same hands in the same fashion as previously described. Upon completion of acquiring samples from the animal, the clippers are wiped free of any blood with a paper towel using the left hand and exchanged with a second pair of clippers soaking in 500 ppm of Oxine. This second pair is carefully dried with a clean portion of paper towel using the left hand but not allowing the sampling fingers to touch any part of the clipper's cutting surface. Layers of clean towel are maintained between the left fingers and cutting surface and the handles are held by the right hand. The purpose of this drying action is to eliminate false positive LFIA that may arise with Oxine present in the blood sample. In practice, the used towel is not discarded until used to remove blood from the next clipping action prior to immersion in Oxine. A fresh towel is only used for the pair of clippers immediately removed from the Oxine.
[0088] Blood collection can also be taken using 1.0 to 1.1 mm ID Na heparinized plastic capillary tubes commonly used in CIEP (counterimmunoelectrophoresis) testing, (Globe Scientific, Paramus, N.J.). The mink is similarly handled and hygiene observed as above only the use of a capillary tube instead of cotton swab acquires the sample. By this method, volumes of samples can be accurately established due to the constant capillary diameter and length of tube filled. For instance a half-filled capillary tube is approximately 35 uL in volume. In some sampling procedures, the contents of the capillary tube are expelled by the use of a capillary bulb into a pre-labeled/bar coded sampling vial with a snap top or into a pre-labeled/bar coded 48 or 96 well plate suitable for extraction and/or PCR.
[0089] Yet another collection process that has been successfully used is the spotting, spreading, and drying of a drop of blood onto a QIAcard (QIAGEN, Valencia, Calif.) and is useful for sample archiving. Punched out portion of the dried, spotted area yields sufficient sample for analysis and it has been found that cross-contamination is not a factor to be considered by the protocol outlined by the manufacturer. Samples are stored at −20° C. until ready for testing for PCR and LFIA samples are stored at 4° C. until testing.
Appendix “E”
Environmental Collection Process for PCR
[0090] Unlike other testing methods currently available, the use of PCR technology allows testing of the environment for mADV presence. This is particularly important to eliminate the possibility of recontamination of the animals that are returned to the pens. Thus, environmental sampling is most useful after a cleaning procedure to determine the efficacy of the cleaning and sanitizing processes. Typically the method used is as follows. An area to be investigated is aggressively rubbed with a cotton swab that has been soaked in a Phosphate Buffered Saline (PBS, Boston BioProducts, Inc., Worcester, Mass.). The presoaking of the cotton swab aids in the acquisition and preservation of the sample. The sampling area can include, but is not limited to, the wire cages, wooden boxes and their parts, inside of the housing roof surfaces, and the ground to name a few of the more obvious and worthwhile sites. As previously stated, the use of proper hygiene while manipulating the sample is always important. The sample may be stored at 4° C. until the PCR process. | Animal husbandry has always been susceptible to the ravages of pathogenic infections. Poultry flus and cattle diseases are but two examples that have dire consequences for animals and adversely affect the economic fortunes of farmers. A testing and culling methodology is presented that can eliminate pathogens from an infected herd. The sensitivity of PCR to detect very low levels of nucleic acid of an infecting pathogen is utilized to identify infected animals. In addition, it has been discovered that PCR analysis of manure samples can accurately identify infected animals and offspring for those species that consume placental remains after birth. Mink Aleutian Disease Virus (mADV) is one of several deadly DNA parvoviruses that can quickly reach epidemic proportions in a mink herd. PCR primers have been developed that generate amplicons to detect and identify the mADV. In addition, a previously unidentified strain of mADV has been discovered, genomically sequenced, and substantially detailed. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to and more stack construction and means particularly to a stack pipe and derrick support therefor.
2. Description of the Prior Art
It has been common practice with tall stacks such as are used with flare gas burners in oil refineries and the like to employ a derrick of a tripod construction between the legs of which the stack is supported. In such structures it is common practice also to connect the tripod legs to the stack between the top and the bottom by braces which are rigidly held at their outer ends by the tripod legs and are slidably connected to the stack at their inner ends.
One tripod derrick which has been proposed is shown in the U.S. Pat. No. 3,233,567, to Goldfield.
In the U.S. Pat. No. to Bates, 2,009,378, a stack of ceramic material is shown in which individual sections of the stack are supported by counterbalancing utilizing cables extending over pulleys carried by a skeleton framework so that should breakage of one section occur the sections supported above it will not fall, and the sections can be individually replaced.
None of the tall stack structures heretofore proposed has proven wholly satisfactory both from the viewpoint of installation and maintenance.
SUMMARY OF THE INVENTION
In accordance with the invention tall stack constructions are provided wherein the stack pipe is supported by a tripod derrick with spaced supports intermediate the top and bottom comprising lateral support guy wires each extending over a pulley carried by one of the tripod legs, with their ends connected to a plate fastened to the stack pipe. The stack pipe can be rigidly supported with respect to the tripod at the top or at the bottom, as desired, with a slidable connection at or near the other end to accommodate expansion and contraction attendant upon change of temperature. Support wires may extend from the bottom of the stack pipe to the foundation. The pipe may rest on a disentrainment drum, removably connected if desired.
The principal object of the invention is to provide tall stack construction wherein the stack pipe may expand upwardly or downwardly in response to thermal expansion and contraction while being supported and without causing damage to the derrick.
A further object of the invention is to provide, in a tall stack construction, a simple but effective bracing employing cables connected to plates secured to the stack and extending around pulleys carried by the legs of the derrick.
A further object of the invention is to provide tall stack construction utilizing a disentrainment drum wherein the stack pipe may be lifted to replace the disentrainment drum by apparatus carried on the top of the derrick.
A further object of the invention is to provide a tall stack construction wherein a work platform may be provided at the top of the derrick.
Other objects and advantageous features of the invention will be apparent from the description and claims.
DESCRIPTION OF THE DRAWINGS
The nature and characteristic features of the invention will be more readily understood from the following description taken in connection with the accompanying drawings forming part hereof, in which:
FIG. 1 is a side elevational view of one embodiment of a tall stack construction in accordance with the invention;
FIG. 2 is a horizontal sectional view taken approximately on the line 2--2 of FIG. 1;
FIG. 3 is a sectional view, enlarged, taken approximately on the line 3--3 of FIG. 2;
FIG. 4A is a fragmentary horizontal sectional view, enlarged, taken at the location 4A on FIGS. 2 and 3;
FIG. 4B is a fragmentary sectional view, enlarged, taken at the location 4B on FIGS. 2 and 3;
FIG. 5 is a fragmentary sectional view, enlarged, taken approximately on the line 5--5 of FIG. 1;
FIG. 6 is a view similar to FIG. 1 but illustrating another embodiment of the invention;
FIG. 7A is a horizontal sectional view, enlarged, taken approximately on the line 7A--7A of FIG. 6;
FIG. 7B is a view similar to FIG. 7A showing another form of mounting;
FIG. 8 is a view similar to FIG. 1 but illlustrating still another embodiment of the invention;
FIG. 9 is a view similar to FIG. 1 but illustrating still another embodiment of the invention, and
FIG. 10 is a fragmentary view, enlarged, in partial section, of a portion of the structure illustrated in FIG. 9.
It should, of course be understood that the description and drawings herein are illustrative merely and that various modifications and changes can be made in the structure disclosed without departing from the spirit of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now more particularly to the drawings and FIGS. 1 to 5, inclusive, one embodiment of the tall stack construction is illustrated which includes a tripod 10 composed of three legs 11 rigidly secured at their bottom ends to foundation plates 12 which are secured by any suitable means to the ground G.
The legs 11 are preferably fabricated of hollow steel tubing, extend upwardly and converge inwardly with upper converging connecting members 15 secured to the legs 11 and to a collar 20 to which the stack pipe 21 is secured.
The stack pipe 21 may be utilized to carry waste products upwardly for dispersal or be provided with a burner tip (not shown) for combustion of waste products in a well known manner.
The pipe 21, at the bottom has a flange 22 thereon for connection to a source (not shown) of waste products to be delivered by the pipe 21. Adjacent the flange 22 and for each of the legs 11 plates 25 are secured to the pipe 21 each of which has a guy wire 26 attached thereto and to the foundation plates 12, exerting a vertical downward force on the pipe 21 and restraining it from sidewise movement.
Above the plates 25, the tripod legs 11 are connected together by horizontal brace members 30 which aid in establishing the rigidity of the tripod 10.
Diagonal brace members 29 are also preferably provided for strength and for rigidity.
Above the plates 25 a plurality of support assemblies 32 are provided each with three plates 33 rigidly secured to stack pipe 21, such as by welding. Adjacent the upper ends of plates 33 as seen in FIG. 1 and 4A, U-shaped clips 34 are provided retained in pivotal engagement with the plates 33 by pins 35 and cotter pins 36.
The clips 34 each has one end of a guy wire 37 attached thereto by retainers 38 of well known type with the guy wires 37 passing over pulleys 40 which are pivotally engaged with plates 41 carried on the tripod legs 11.
The guy wires 37 are secured at the ends opposite to clips 34 to bolts 42, of adjustable turn buckles 45 and retained thereto by retainers 38 of well known type. The turn buckles 45 are adjustable to provide tension on the guy wires 37 which turn buckles 45 are secured to the plates 33 above pins 35 by bolts 47 and nuts 48.
The support assemblies 32 by reason of the tension placed on guy wires 37 exert a restraining force on the pipe 21 permitting limited vertical expansion and contraction of the stack pipe 21 without substantially altering the restraining effect of the guy wires 37.
Referring now more particularly to FIGS. 6 and 7A of the drawings, another embodiment of the tall stack construction is illustrated which includes tripod legs 110 rigidly secured to foundation plates 101 which are attached to the ground G and have members 107 connecting the legs 100. The tripod legs 100 extend upwardly, converge inwardly and have angularly inwardly extending connecting members 102 connected thereto and to a triangular frame 103 which frame includes three angle members 104 secured together at their ends with pairs of plates 105 attached thereto at the intersections of the members 104. The plates 105 have spools 106 rotatably mounted therebetween by pins 110. The spools 106 are engaged with V-shaped plates 111 rigidly secured to a stack pipe 121, permitting vertical sliding engagement of pipe 121 but retaining the pipe 121 from sidewise movement. The stack pipe 121 is similar to pipe 21 in construction at the bottom, is provided with a flange 122 for connection to a source (not shown) of waste products to be burned above or merely discharged through pipe 121 for dispersal. Above the flange 122 the pipe 121 is retained in a collar 125 to which it is rigidly connected. The collar 125 has three arms 126 connected thereto and to the tripod legs 100 with additional diagonal bracing members 127 connected to the arms 126 and legs 100 for support of the arms 126. The collar 125 restrains the pipe 121 from sidewise movement and provides a support for the pipe 121.
In FIG. 7B another form of guide and support for the stack pipe 121 is shown in which, in addition to the V-shaped plates 111 and the spools 106 movable therealong, the shaft 105 carries additional rollers 112 which engage with angle plates 113 secured to the stack pipe 121. The plates 113 have flanges engaged by the rollers 112 to restrain the stack pipe 121 against radial displacement.
Above the collar 125 the pipe 121 has a plurality of support assemblies 132 engaged therewith similar to the assemblies 32 each of which includes three plates 133 secured to the pipe 121 at spaced locations therearound. Each of the plates 133 adjacent its top has one end of a guy wire 134 fastened thereto by bolt 135 with the cable passing over a pulley 136 rotatably mounted to a plate 137 which is secured to one of the tripod legs 100. The guy wire 134 at its end opposite to bolt 135 is secured to the plate 133 and provided with turn buckles (not shown) similar to turn buckles 45 to permit detachment of the guy wires 134 and adjustment of the tension on wires 134.
Referring now to FIG. 8 of the drawings, another embodiment of the tall stack construction is illustrated which includes tripod legs 200 rigidly secured to foundation plates 201 which are secured to the foundation F in any suitable manner. The tripod legs 200 are held in assembled relation by horizontal brace members 202 which are connected at their ends to the legs 200, diagonal stiffeners 203 also being provided as in the tripods previously described.
The legs 200 extend upwardly, converge inwardly and have angularly related connecting members 210 connected thereto at their upper ends which in turn are connected to a triangular frame 211 similar to frame 103 of FIGS. 6 and 7 which frame 211 has plates (not shown) and spools (not shown) which engage V-shaped plates (not shown) which are secured to a stack pipe 212.
The stack pipe 212 of conventional type is connected at its lower end to a disentrainment drum 215 of conventional type to provide for separation of slugs, water vapor and other heavy particles which settle out from the waste products to be discharged from stack pipe 212.
The drum 215 is detachably connected to foundation F by bolts 216 and nuts 217.
The drum 215 is provided with a drain connection 220 at its bottom to permit removal of the material which separates from the waste products passing through the drum 215.
A flange 221 is connected to the side of drum 215 for connection to a source of waste products (not shown) to be discharged from pipe 212.
Above the drum 215 a plurality of support assemblies 232 are provided similar to assemblies 32 and 132 with plates 233 connected to the pipe 212 and with guy wires 234 connected to the top and bottom of the plates 233 in the manner described for assemblies 32 and 132. The guy wires 234 are carried on pullyes 235 rotatably mounted to plates 236 which are fastened to the tripod legs 200 and which guy wires have turn buckle assemblies (not shown) attached thereto similar to assemblies 45 to provide tension on guy wires 234 for restraining sidewise movement of the stack pipe 212.
Referring now to FIGS. 9 and 10, still another embodiment of the tall stack construction is illustrated which includes tripod legs 300 rigidly secured to foundation plates 301 which are fastened to the foundation F in a conventional manner.
The legs 300 are held together in the tripod arrangement by a plurality of horizontal connecting members 302 which are secured at their ends to the legs 300 and with diagonal braces 303. The legs 300 extend uwpardly, converge inwardly and have angularly related connecting members 305 connected thereto and to the jacking plate 306 of a work platform 307. The jacking plate 206 extends around and retains a stack pipe 310 therein in vertical slidable engagement with a mounting similar to that shown in FIGS. 6, and 7A or 7B.
The jacking plate 306 has a plurality of hydraulic jacks 312 thereon with centering pins 313 which can be engaged with a plate 314 welded to the pipe 310 which plate 314 has reinforcement plates 315 welded to it and to the pipe 310.
The jacks 312 preferably operated together from a single pressure source, are utilized to raise the pipe 310 for purposes to be described.
The stack pipe 310 which is of conventional type has a flange 325 at its bottom end which is normally engaged with a flange 326 of a disentrainment drums 330.
The drum 330, which can be of conventional type can be secured to the ground or foundation F by a plurality of bolts 331 which extend downwardly into engagement with nuts 332 anchored below the surface of the ground thus permitting the sidewise movement of the drum 330 without obstacles.
The drum 330 is similar to drum 215 and is provided with a flange 335 connected to a source of waste products (not shown) to be discharged therefrom through the pipe 310.
The drum 330 is provided with a drain 336 to permit removal of material such as slugs and water from the waste products that settle out in the drum 330.
When it is desired to remove the drum 330, the flanges 325 and 326 are disconnected and the pipe 310 is raised by the hydraulic jacks 312 and plate 314. Another drum 330 can be provided and the flanges 325 and 326 can be reconnected when the pipe 310 is lowered.
The pipe 310 above the flange 325 is provided with a plurality of support assemblies 332 similar to support assemblies 32, 132 and 232 and which each includes three plates 333 welded to the pipe 310, cables 334 attached to the top and bottom of the plates 333 extending over pulleys 335 rotatably mounted on plates 336 carried by the tripod legs 330, with turn buckles (not shown) as previously described.
It will thus be seen that structure is provided with which the objects of the invention are acheived. | A tall stack construction which may be used for the discharge of products of combustion or may be used as a flare stack with a burner at the top end for combustion of waste products from oil refineries or other chemical processes, the stack pipe being supported by a derrick in the form of a tripod with lateral support guy wires each extending over a pulley carried by one of the tripod legs and with their ends connected to a plate on the stack pipe. Additional stability is obtained by diagonal guy wires in tension extending from the bottom of the stack to the foundation in one embodiment. The stack pipe may be fixed to the derrick at the top or the bottom, may have a disentrainment drum at the bottom and may be supported in slidable engagement at the top of the derrick for expansion and for separation of the disentrainment drum. | 4 |
FIELD OF THE INVENTION
The invention is directed to a guide bar arrangement for a warp knitting machine wherein the guide bar is axially displaceable by a displacement arrangement and is held by an axially non-displaceable holding means suitably attached to the swinging shaft via an intermediately placed compensating arrangement.
BACKGROUND OF RELATED ART
In a known guide bar arrangement of this type, DE GM 185 710 0, the displacement arrangement comprises a pusher rod controlled by a cam plate against which the guide bar is held by means of a return spring. The smoothing arrangement, which enables the displacement of the guide bar with respect to levers attached to the swinging beam, is provided by a plurality of guide bolts which are held in axial bearings provided in roller bearing boxes.
In order to drive the warp knitting machine at greater speeds, the guiding by the axial bearings must be substantially free of play. This leads to a larger amount of friction and a corresponding consumption of energy, which is converted into heat and thus to an undesired expansion of the guide bar. The high frictional forces also considerably bias the transfer elements of the displacement arrangement and also cause friction. At high working speeds, larger acceleration and deceleration forces also come into play.
An object of the present invention is to provide a guide bar arrangement of the foregoing type having a substantially simpler construction and only negligible frictional losses.
SUMMARY OF THE PRESENT INVENTION
In accordance with the illustrative embodiments demonstrating features and advantages of the present invention, there is provided, a guide bar arrangement for a warp knitting machine having a swinging shaft. This arrangement includes a guide bar and a displacing arrangement for axially displacing the guide bar. Also included is a holding means having an intermediating compensating arrangement for supporting the guide bar. The holding means is axially fixed and attached to the swinging shaft. The compensating arrangement and the displacement arrangement include a plurality of bending transducers, each having one end attached to the holding means and another end attached to the guide bar. The bending transducers are deflectable under the influence of an electrical control signal.
An improved smoothing arrangement and displacing arrangement can thereby be formed with bending transducers which are attached at one end thereof in the holding means and the other end thereof carrying the guide bar and are deformed under the influence of a control signal. In such an arrangement, it is no longer necessary to utilize the various elements of the displacement arrangement (for example pattern cam disk, pattern chain, setting motor and the like). Also unnecessary are all of the axial bearings of the smoothing arrangement. Rather all of the functions of the displacement arrangement and the compensating arrangement may be taken over by the bending transducers.
The number of required bending transducers is determined by the machine production level or the expected requirements of servicing. Even with two bending transducers, a parallelogram is formed together with the holding means and the guide bar in such a manner that even with deformation of the bending transducers, the guide bar is still held parallel to the holding means.
The change in height of the guide bar during the conventionally occurring displacement arrangement is so small that for practical purposes, it can be ignored. In practice however, a larger number of bending transducers are utilized, on the one hand to give the guide bar a higher stability despite axial movement and on the other hand to provide the bending deformation with a sufficient displacing force.
It should be noted that the displacing force is held to be substantially less than was utilized heretofore since it is unnecessary to utilize a return spring in order to achieve a force transferring contact between the displacing arrangement and the guide bar. Furthermore, it should be noted that the additional mass on the guide bar due to the bending transducers is substantially less than the additional mass thereto provided by the axial bearings so that a higher rate of working speed may be obtained.
It is particularly advantageous if the holding means on the lever attached to the swinging shaft comprises a holding rail and that the bending transducers are distributed over the entire length of the guide bar. By utilizing a holding rail, the bending transducer groups may be located at a comparatively small distance from each other so that the holding points of the guide bar are comparatively close. This permits the guide bar to have a smaller cross-section and thus to be provided with a lower mass which again leads to a higher working speed.
It is further advantageous to provide the bending transducers in mutually attached groups which are provided with a common header for fastening onto the holding means and a common footing for fastening onto the guide bar. In this manner, it is possible to insert and remove groups of bending transducers, which is very useful for assembly and repair.
Suitably, the bending transducers are piezoelectric transducers which have an active layer of piezoelectric material in strips either on one side or on both sides. Such bending transducers may be readily activated by a control potential and react very readily to such control potentials. It is thus possible to operate with conventional high working speeds and even achieve yet higher working speeds. However, the invention may include the use of other bending transducers, for example, electromagnetic or magnetostrictive or otherwise activated transducers.
It is preferred to provide the strip-shaped carrier with a protrusion at its foot end extending beyond the active layer. This non-activatable layer increases displacement of the guide bar so that the displacement path of several millimeters may be achieved.
It is advantageous to make the strip carriers of a carbon fiber composite, that is, a polymer filled with carbon fibers. This yields a particularly light, but stable construction to the bending transducer.
It is particularly advantageous if the provision of the control current causes the bending transducers to move from a neutral position either to the left or the right, as desired. Thus, if there is applied a positive control potential and another time a similar negative control potential to the bending transducer, there are provided three equidistant positions of the guide bar so that, for example, a tricot base fabric can be knitted. By utilization of different potentials, it is also possible to provide different displacement movements.
In a preferred embodiment, the strip formed carriers are made out of an electrically isolating material and on both sides are provided with a coating comprising an inner electrode, an active layer and an outer electrode, wherein the inner electrode is connected to the power source and the outer electrode to ground. Such a bending transformer has the further advantage that it may be safely touched since the outermost electrodes are grounded.
It is also advantageous to provide a displacement control arrangement, which provides the control current to the bending transducers in predetermined size as well as in accordance with the predetermined program. In this manner, the displacement arrangement can be so carried through that no excessive acceleration or deceleration occurs. Further details may be found in Applicants' copending application DE P 44 11 528.8 (corresponding to U.S. Ser. No. 08/412,167) which is incorporated herein by reference.
It is furthermore advantageous to provide stops to limit the displacement path of the guide bar. It is possible to achieve displacement targets very rapidly, however it is still advantageous to provide definite end points. Furthermore, these stops can be moved by a drive means such as a setting motor. It is thus possible to drive the guide with very different displacement steps.
In a further embodiment of the invention, the guides themselves may be displaceable by piezoelectric deflecting transducers carried by the guide bars and individually influenceable by control potentials. In this manner, guide bar may be both displaceable by bending transducers and equally acts as a jacquard controlled guide bar because of deflecting transducers.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention may be further illustrated in its preferred embodiments by the following figures.
FIG. 1 is a vertical cross-sectional view through the working region of a warp knitting machine provided with the guide bar arrangement of the present invention;
FIG. 2 is a vertical cross-sectional view of one of the two right-hand guide bar arrangement of FIG. 1;
FIG. 3 is a vertical front view of the guide bar arrangement of FIG. 2;
FIG. 4 is a cross-sectional view of the left-hand guide bar arrangement of FIG. 1;
FIG. 5 is a group bending transducers set up for assembly in the machine of FIG. 1;
FIG. 6 is the upper mounting location of a bending transducer of FIG. 5;
FIG. 7 is a graph showing applied potential of the control signal of FIG. 1 against time;
FIG. 8 is a partial sectional view of a bending transducer that is an alternate to that of FIG. 6.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
FIG. 1 shows the working area (1) of a warp knitting machine having a needle bar (2) carrying needles together with the appropriate sliders on slider bar (3), a stitch comb bar (4) and a knock-over bar (5) over whose upper edge finished fabric (6) may be pulled. Two guide bars (7 & 8) with guides (9 & 10), respectively form the fabric ground. A guide bar (11) having jacquard control guides (12) provides the patterning.
The several guide bars have interposed bending transducers (13, 14 and 15) that are held by a holding means, shown herein as holding rails (16, 17 and 18) and swing lever (19). These latter are held fast on swinging shaft (20) and may be moved to and fro in the direction of arrow (21) wherein the-guides (9, 10 and 12) may be moved from the illustrated overlap situation into the underlap position and back again.
Under the term "bending transducers," there are included in the first instance elements made out of a bendable material which, under the influence of an outside force, suitably electrical or mechanical is deformed through bending. For the presently required purpose, these elements are preferably in strip form.
Referring to FIGS. 2 and 3, holding rail (18) stretches over the entire length of right-hand guide bar (8). Eight piezoelectric bending transducers (15) are put together in groups (22 and 22a), which have a header (23 and 23a) and a footing (24 and 24a), respectively. The piezoelectric bending transducers (15) are connected with the header (23) and the footing (24). Screws (25) which grasp through holes (26) serve to attach the header (23) to the holding rail (18). Screws (27) grip through holes (28) and serve to affix the footing (24) to the guide bar (8). The latter generally carry leads (29), which are attached by means of screws (30) and themselves carry a plurality of guides (10).
Two signal leads (32 and 33) are attached to control arrangement (31) over which the electrical potential of a control signal may be led to the depending transducers (15) as is further illustrated in FIGS. 5 and 6. The holding rail (18) is grounded at (34). By providing the control potential, the lower ends of the bending transducers (15) are displaced in one or the other direction so that the guide bar (8) can provide a displacement (X1).
Stops (35 and 36) serve to limit the extent of travel of the displacement movement and thus provide an exact setting for guides (10) during their swing through the needle gaps between the needles.
In FIG. 3, a composite displacement (X) is illustrated. The stops (35 and 36) can be further displaced by the setting motors (drive means 37 and 38) receiving signals through leads (39 and 40) connected to the control arrangement (31) .
FIGS. 4 and 5 show the left-hand guide bar arrangement of FIG. 1 with guide bar (11) and holding rail (16) . Furthermore, groups (41) of bending transducers (13) are connected at their upper end with header (42) and at their lower end with footing (43) which, similarly to what is shown in FIGS. 2 and 3, are connected with holding rail (16) by means of screws, for example screws (44).
The bending transducer (13) comprises, as shown in FIG. 6 a strip-formed carrier (45) of electrically insulating material, for example, reinforced glass fibers. On one side of carrier (45) there is a layer comprising: inner electrode (46), the piezoelectrically activated layer (47), and outer electrode (48). On the other side of carrier (45) is a layer comprising: inner electrode (49), piezoelectrically active layer (50), and outer electrode (51).
The two inner electrodes (46 and 49) are connected with signal leads (32 and 43). The two outer electrodes (48 and 51) are grounded via the potential of the mass of the machine, whereby the header (42) and the holding rail (16) and are grounded. For this purpose the header (42) is provided with comb-like grooves (52) in which the upper end of the bending transducers (13) can be slid and there clamped or affixed by other means. The strip-formed carrier (45) possesses a protrusion (53) extending beyond the active layers (47) and (50) and whose lower end is set in a slit in footing (43).
Commencing at a neutral position of bending transducer (13), upon the application of a control potential to the inner electrode (46), the footing (43) moves to the left and by the provision of a control potential to the right inner electrode (49) it moves to the right. The displacement distance is substantially proportional to the loading on the bending transducer and thus is proportional to the applied DC voltage potential. By successive applications of equal potentials, displacements of equal size will occur, which without any difficulty may be set to be equal to one or a plurality of the spacings between the needles. In this manner, it is possible to control the displacement in a pattern conforming manner.
Furthermore, as is shown in FIG. 7, in the course of a work cycle A, the control potential in volts DC follows a curve (k) in which: segment (a) corresponds to the overlap displacement; segment (b) follows the swing-through into the underlap position; segment (c) shows the underlap displacement itself; and segment (d) shows the swing back of the guide bar (11) into the overlap position. The individual segments may run in straight lines, however in between them advantageously, there are transition steps. In this way at the beginning one seeks a modification of the acceleration of guide bar (11) and modification of the deceleration at the end of the cycle. There are here no excessive counter forces so that there is provided a trouble free mode of proceeding.
The guides (12) are attached to carrier strips (54) on piezoelectric deflecting transducers (55), which in turn are affixed to header (56). This is attached to guide bar (11) by means of screws (57). Electrical leads (58) are connected to control arrangement (31). In this way guides (12) may be displaced in the manner of a jacquard control. With respect to further specific questions of such jacquard control with piezoelectric bending transducers, reference is made to Applicant's prior German patent applications, namely P 42 26 899 (U.S. Ser. No. 08/1 04,369); P 43 16 396, P 44 14 876 (U.S. Ser. No. 08/426,887), and P 44 18 714 (U.S. Ser. No. 08/412,167), whose disclosure is incorporated herein by reference. The construction of the piezoelectric bending transducers described in the foregoing applications may be similarly utilized for bending transducers (13 through 15) of the present application.
This structure may also apply as well to the provision of a second bending transducer in the region of the extension (43 of FIG. 1) which can bend in a direction opposite to that of the first bending transducer. By means of the second bending transducer, the lower end of the strip-formed carrier is displaced parallel to itself during the bending formation. The loading of the carrier on the attachment point on the guide bar side is therefore minimal.
FIG. 8 illustrates the upper end of the bending transducer (59). A strip-formed carrier (60) is made of a synthetic material strengthened with carbon fibers, which makes it electrically conductive. On one side, it carries a layer of piezoelectrically active material (61) having an outer electrode (62) and on the other side there is coated a piezoelectrically active layer (63) having an outer electrode (64). The outer electrode (62) is connected with signal line (32) and the outer electrode (64) with signal line (33). The electrically conductive carrier (60) is grounded at point (34). Such a bending transducer can be very light in weight, and still be made with very high stability.
It is to be appreciated that various modifications may be implemented with respect to the above described preferred embodiments. For example, in many cases it is sufficient if the holding means comprises the swinging lever (19). The holding rails (16, 17 and 18) may no longer be required.
Obviously, many other 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. | A guide bar arrangement for a warp knitting machine has at least one guide bar, which is axially displaceable by means of a displacing arrangement and is carried, suitably on an axially rigid holding arrangement attached to a swinging shaft, through the intermediation of a compensating arrangement. The compensating arrangement and the displacement arrangement include bending transducers, which are attached at one end thereof on the holding arrangement (a lever 19 holding rails) and on the other end thereof on the guide bar and are bendably deformed under the influence of a direct current control signal. This leads to a simple construction of the guide bar arrangement with little frictional loss. | 3 |
RELATED PATENT APPLICATION
This invention is a continuation-in-part application of patent application Ser. No. 680,279, filed Dec. 10, 1984, now U.S. Pat. No. 4,587,931.
BACKGROUND OF THE INVENTION
Most automotive internal combustion engines have a coolant system which includes fluid conduits within the engine and adjacent the engine, and a heat exchanger through which coolant liquid flows.
For the protection of the internal combustion engine against overheating, an alarm, audible, and/or visual, to the operator should be activated if the temperature of the engine becomes excessive.
One major consideration in the protection of an internal combustion engine is that the coolant fluid in the coolant system must remain substantially in liquid form and should not be permitted to boil. The boiling point of the coolant liquid depends upon the composition thereof and also depends upon the pressure applied to the coolant liquid within the coolant system.
A coolant system of an internal combustion engine usually is a closed system in which a pressure cap closes the passage through which the coolant liquid is introduced into the coolant system. The pressure cap is designed to maintain a predetermined operating pressure within the coolant system. If a predetermined operating pressure in the coolant system could always be precisely maintained, the problems involved with regard to protection of the engine against excessive temperatures would be significantly reduced. If a predetermined operating pressure were always maintained in the coolant system, monitoring of the temperature of the engine would be the principal requirement for protection of the engine.
However, as a practical matter, the pressure in the coolant system cannot be properly or effectively controlled. This is due to the fact that the pressure cap is customarily one which has a pressure tolerance range. Also, an aging pressure cap permits a change in the operating pressure maintained in a coolant system. Furthermore, an aging coolant system becomes increasingly subject to leakage.
Most engine protection devices sense only the temperature of the engine, and a temperature alarm condition is established based upon an anticipated operating pressure within the coolant system. In such systems a temperature alarm may be energized at a time in which temperature conditions do not justify an alarm, or an alarm may not be energized at a time in which the engine is subjected to damage by excessive heat.
A coolant system which maintains less than an expected operating pressure permits the coolant liquid to boil at a temperature less than that for which the danger signal is designed to operate. Under such conditions, the coolant liquid may boil away and be lost from the coolant system without causing the alarm signal to be energized.
For these reasons, inter alia, devices which have been designed to protect an internal combustion engine against overheating have not been effective.
Thus, it is understood that in order to properly protect an internal combustion engine against overheating, it is necessary to sense both the temperature and the pressure within the coolant system of the internal combustion engine.
It is an object of this invention to provide a switch unit for protection of an internal combustion engine in which the switch unit senses both the temperature and pressure of the liquid in the coolant system and which operates as a function of a combination of the temperature and pressure conditions of the liquid within the coolant system.
Another object of this invention is to provide such a switch unit which is capable of operating and compensating as a function of both the temperature and pressure of a specific liquid in the coolant system.
Another object of this invention is to provide such a switch unit which has relatively long life and which may be produced at relatively low costs.
Other objects and advantages of this invention reside in the construction of parts, the combination thereof, the method of production and the mode of operation of the switch unit as will become more apparent from the following description.
BRIEF DESCRIPTION OF THE VIEWS OF THE DRAWINGS
FIG. 1 is a side sectional view of a switch unit of this invention, as the switch unit is installed in association with the engine coolant system of an internal combustion engine. This figure illustrates the switch unit in a de-actuated condition.
FIG. 2 is a side sectional view, similar to FIG. 1, and illustrates the switch unit in an actuated condition.
SUMMARY OF THE INVENTION
A pressure compensated temperature switch unit of this invention comprises a housing adapted to be mounted within an opening in a wall of a conduit of a coolant system of an internal combustion engine. The housing has a cavity therein. Within one end portion of the housing is a support member of non-conductive material, such as a plastics material or the like. Attached to the support member is an expansible-contractible member in the form of a bellows, which extends from the support member and into the cavity of the housing.
Within the housing enclosing the cavity and separating the coolant system from the cavity in the housing is a flexible wall in the form of a bellows.
Within the cavity of the housing and encompassing the expansible-contractible member and filling the space in the cavity which is not occupied by the expansible-contractible member is a liquid, which is a good heat transfer medium, which is incompressible, and which has good dielectric characteristics.
Also attached to the support member and extending therefrom is a pair of electric conductor elements, which form a portion of an electric circuit.
Thus, the bellows members and the liquid within the cavity of the housing are subject to pressure and temperature conditions which exist within the coolant fluid which flows in the conduit system. When any combination of temperature and pressure conditions exist within the coolant system and within the cavity of the housing which indicates that a dangerous condition exists, an electric alarm circuit is created through the electric conductor elements. Thus, the temperature of the engine at which an alarm is energized is compensated by the pressure in the coolant system of the engine.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 illustrates a switch unit 10 of this invention as it is mounted in a fluid conduit 14 which is formed by a wall 12 and a wall 13. The conduit 14 is a part of a coolant system of an internal combustion engine. Engine coolant liquid flows through the conduit 14, through the engine, not shown, and through a heat exchanger, not shown.
The switch unit 10 comprises a housing 20 which is mounted within the wall 12. The housing 20 has a cavity 22 therein. An opening 30 in the housing 20 leads to the cavity 22 and is in fluid communication with the conduit 14.
Supported by the housing 20 at one end portion thereof opposite the opening 30 is a support member 36 which is made of non-conductive material. Supported by the support member 36 and positioned within the housing 20 is an expansible-contractible member 40, herein shown as being a bellows type of member which has a tubular base portion 42 which is closed by a closure element 44. The tubular base portion 42 is shown as being threadedly attached to the support member 36. However, of course, other means of attachment may also be satisfactory. The expansible-contactible member 40 also has an engagement, end portion 40e at the end thereof opposite the base 42. The expansible-contractible member 40 is made of electrically conductive material.
A limited quantity of vaporizable liquid is contained within the expansible-contractible member 40. Preferably, the liquid within the expansible-contractible member 40 has substantially the same composition as the composition of the liquid in the conduit 14 and within the entire coolant system of the engine.
Also, supported by the support member 36 and extending into the housing 20 is an electric conductor member 52, which has a part encompassing the base 42 of the expansible-contractible member 40 and in firm contact therewith.
A cap member 60, attached to the housing 20 and positioned within the opening 30, encloses the cavity 22. The cap member 60 has bellows wall portions 60b and is therefore expansible and contractible in length. Within the cavity 22 and encompassing the expansible-contractible member 40 is a liquid 62, which is retained within the cavity 22 by the cap member 60. The liquid 62 is a good dielectric, is incompressible, and has good thermal conductivity.
Extending through the support member 36 is another electric conductor member 70. The conductor member 70 extends into the cavity 22 and extends along the expansible-contractible member 40. The conductor member 70 has an engagement portion 70e adjacent the engagement end portion 40e of the expansible-contractible member 40.
OPERATION
During operation of the engine having the conduit 14, coolant fluid flows through the conduit 14. A portion of the coolant fluid flows into the opening 30 and encompasses the cap member 60.
Under normal conditions the engagement portion 40e of the expansible-contractible member 40 is spaced from engagement with the engagement portion 70e of the electric conductor 70, as shown in FIG. 1.
The wall 12, the cap 60, and the housing 20 serve as heat transfer agents between the coolant fluid flowing in the conduit 14 and the liquid 62 within the cavity 22 of the housing 20. Therefore, the temperature of the liquid 62 within the cavity 22 of the housing 20 is substantially the same as the temperature of the engine and the coolant fluid flowing through the conduit 14.
Obviously, some of the fluid which flows in the conduit 14 also flows within the opening 30. Therefore, the bellows walls 60b of the cap 60 expand and contract in accordance with the pressure of the coolant fluid flowing through the conduit 14 and through the coolant system of the engine. The pressure of the coolant fluid which is applied to the cap 60 is transmitted through the cap 60 to the liquid within the cavity 22 as the bellows walls 60b of the cap 60 expand and contract. Therefore, the pressure of the liquid 62 within the cavity 22 of the housing 20 is substantially the same as the pressure of the coolant fluid flowing through the conduit 14.
Thus, the pressure and temperature of the liquid 62 within the cavity 22 of the housing 20 are applied to the expansible-contractible member 40 within the cavity 22. As stated above, the expansible-contractible member 40 contains a liquid which has substantially the same composition as the coolant liquid flowing through the conduit 14. Therefore, the liquid within the expansible-contractible member 40 responds to temperature in the same manner as the coolant fluid in the coolant system of which the conduit 14 is a part. Therefore, the expansible-contractible member 40 expands and contracts in length in accordance with both the temperature and pressure of the coolant fluid in the conduit 14.
The temperature and pressure conditions in the coolant fluid flowing through the conduit 14 may be such that the expansible-contractible member 40 is expanded in length until the engagement portion 40e of the expansible-contractible member 40 engages the engagement portion 70e of the electric conductor 70, as illustrated in FIG. 2. When this engagement occurs, an electrical circuit is established between the electric conductor 52 and the electric conductor 70. Thus, an alarm, not shown, is energized to warn the operator of the engine that temperature and pressure conditions within the coolant system of the engine are such that dangerous conditions may exist in the engine. The alarm may be audible and/or visible. For example, the temperature of the coolant fluid may become so great that the pressure within the expansible-contractible member 40 overcomes the pressure exterior of the expansible-contractible member 40. When this occurs, the expansible-contractible member 40 expands to the extent that the engagement portion 40e of the expansible-contractible member 40 engages the engagement portion 70e of the electric conductor 70.
Thus, it is understood that an alarm is energized in accordance with both the temperature and pressure conditions within the cooling system of an internal combustion engine. It is to be understood that there is effectively an infinite number of pressure-temperature conditions at which the expansible-contractible member 40 expands to the position in which the engagement portion 40e of the expansible-contractible member 40 engages the engagement portion 70e of the electric conductor 70.
Also, for example, as a result of leakage, substantially all of the coolant fluid in the cooling system of the engine may be lost. When this occurs, the pressure in the conduit 14 and the pressure in the cavity 22 and the pressure upon the expansible-contractible member 40 is low. Therefore, as the engine operates and creates heat in the coolant system, the liquid within the expansible-contractible member 40 readily expands and the expansible-contractible member 40 readily expands in length and the engagement portion 40e engages the engagement portion 70e of the electric conductor 70. Thus, an alarm is energized.
Furthermore, when the pressure in the coolant system is significantly high, the temperature of the coolant fluid in the cooling system must become significantly high in order for the expansible-contractible member 40 to expand for engagement between the engagement portion 40e of the member 40 and the engagement portion 70e of the electric conductor 70.
Thus, it is understood that the switch unit of this invention functions in accordance with a combination of the temperature and pressure of coolant fluid within the cooling system of an internal combustion engine.
Although the preferred embodiment of the engine protective switch unit of this invention has been described, it will be understood that within the purview of this invention various changes may be made in the form, details, proportion and arrangement of parts, the combination thereof and the mode of operation, which generally stated consists in an engine protective switch unit within the scope of the appended claims. | A pressure compensated temperature switch for the protection of an internal combustion engine or the like. The switch unit includes a housing, a portion of which is positioned within a passage in the cooling system of the internal combustion engine. Within the housing is a pressure sensitive member. The pressure sensitive member senses both the temperature and the pressure of the coolant fluid in the coolant system of the internal combustion engine. A visual and/or audible alarm device, which is connected to a switch unit of this invention, thus operates when temperature conditions exist within an engine which are harmful to the engine. | 7 |
The invention broadly relates to security gates for children and pets, and is specifically directed to mounting apparatus for use with such security gates that can be used to insure that the gate will not be moved in any manner when it is in place.
Security gates provide an important function in the home where doors do not exist to keep children from leaving a safe area, as well as to prevent them from entering a dangerous area (e.g., a stairwell). These gates also find useful application in preventing pets from leaving areas in the house designated for the pet and from entering areas where the pet should not go.
Among various types of security gates available, most have relatively movable parts which enable it to expand laterally and increase its effective width. Frictional bumpers are provided on opposite sides of the gate for frictionally engaging opposite sides of a door jamb, and expansion of the gate places it under compression within the door jamb. In this state, the bumpers frictionally engage the door jamb and firmly hold the gate in place under most circumstances.
Although this approach lends itself to portability of security gates that are capable of functioning safely in the vast majority of cases, it has been difficult to use such security gates in conjunction with wrought iron railings, particularly where the opening leads to a stairwell. Here, the risk that the security gate can be dislodged increases, which precludes the gate from accomplishing its intended purpose.
In addition, consumers' safety groups have recently placed standards on security gates of this type, requiring them to withstand certain minimum forces that are imposed laterally on the gate. Where the gate can withstand such lateral forces, it is extremely difficult for a child or pet to dislodge the gate from its intended position.
This invention is the result of an endeavor to provide a mounting device for portable security gates that exceeds all applicable safety standards while at the same time being inexpensive to purchase and simple to use.
The inventive mounting device consists of a small socket defining member that is easily mounted on a door jamb, wall or other flat surface as well as onto the vertical post of a wrought iron railing. Each socket defining member is constructed and arranged to receive and retain a frictional bumper member on the security gate in such a way that the gate cannot be laterally moved or dislodged in any way.
Two specific types of socket defining members are used. The first is for door jambs and other flat surfaces, and it includes a rectangular base with front and back faces, the back face of which is flat to correspond to the flat surface upon which it is mounted. In the preferred embodiment, the back face includes a shallow recess in which a double-faced adhesive backing member is placed. The backing member itself has adhesive properties sufficient to hold the mounting member and gate in place to exceed safety standards. The socket for the mounting member is defined by a U-shaped rib that projects forwardly from the front face, and is adapted to receive and retain a circular friction bumper. Other configurations are obviously possible, although circular friction bumpers are most prevelant.
The socket-defining mounting member for wrought iron rails is structurally similar to that for flat surfaces, but also is provided with rearwardly projecting sides that overlie the sides of the wrought iron post. Because wrought iron railing posts are available in a variety of sizes, the back base of the mounting member is also provided with groups of frangible members that can be selectively broken away to define a mounting channel corresponding in size to the width of the vertical post. The adhesive back on the mounting member, coupled with the vertical sides and frangible members, cause the mounting member to be held rigidly in place under virtually all circumstances.
Although the adhesive back is entirely adequate for the vast majority of mounting situations, each of the socket-defining mounting members is also provided with a screw mounting that can be inserted into the door jamb, wall or wrought iron post to provide additional strength and stability.
Each of the socket-defining gate mounting members is structurally simple and can be fabricated by plastic molding. As such, the plastic mounting members are inexpensive to purchase and easily installed. For example, the security gate user may choose to purchase several different sets of mounting members for different doorway openings in the same house.
By virtue of their unique construction, the inventive mounting members are capable of receiving and holding in place any security gate of the adjustable width type having friction bumpers in any doorway or similar opening, including stairwells and those defined in whole or in part by wrought iron railings or similar rails.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded fragmentary perspective view showing a security gate installed with the invention;
FIG. 2 is an enlarged perspective view showing a first embodiment of an inventive mounting socket as viewed from the front side thereof;
FIG. 3 is an enlarged perspective view of the inventive mounting socket of FIG. 2 as viewed from the backside thereof;
FIG. 4 is an enlarged perspective view of a second embodiment of the inventive mounting socket viewed from the front side thereof;
FIG. 5 is an enlarged perspective view of the inventive mounting socket of FIG. 4 from the rear side thereof; and
FIG. 6 is an enlarged sectional view taken along the line 6--6 of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
With initial reference to FIG. 1, a child/pet security gate represented generally by the numeral 11 is intended for mounting at the head of a stairwell between a wall 12 and a wrought iron railing 13 using inventive mounting apparatus described in further detail below.
The child/pet security gate 11 is of the type disclosed in U.S. Pat. No. 4,607,455, which issued on Aug. 26, 1986 for an "Adjustable Gate for Doorways", and which is commonly owned by the assignee of this application and invention. Gate 11 includes relatively slidable gate sections 14, 15 that slide relatively to approximate the width of the doorway in which the gate 11 is to be mounted, and locking means (not shown) thereafter force the gate sections 14, 15 apart into a compressing relation with the doorway defining members and lock the gate 11 in this position. Small circular rubber bumpers 16 on the outside edges of the gate sections 14, 15 frictionally engage the door or wall surface to hold the gate 11 in position.
Reference is made to U.S. Pat. No. 4,607,455 for further details as to the structure and operation of the gate 11. However, it is to be understood that gate 11 is shown here for exemplary purposes only, and the inventive gate mounting devices may be used in conjunction with child/pet security gates of varying construction.
Wall 12 as shown in FIG. 1 is of conventional construction, defining a flat surface that the gate 11 may engage. Similarly, the wrought iron railing 13 is of conventional construction, including a top rail 17, bottom rail 18 with vertical members 19 welded therebetween. As shown in FIG. 1, the wrought iron railing 13 includes a corner section defined by larger vertical members 21 that extend to the floor and are rigidly secured thereto by bolts. It is important to mount the gate 11 on the floor mounted corner section of the wrought iron railing 13 since mounting it to the side of a longitudinal section of the railing 13 would not provide adequate backing.
With reference to FIGS. 2 and 3, a gate mounting device for walls, door jambs and similar flat surfaces is represented generally by the numeral 22. Device 22 is preferably molded from plastic, and comprises a rectangular base 23 the backside of which (FIG. 3) is flat for mounting on the flat surface of wall 12, a door jamb or the like. A shallow rectangular (square) recess 24 is formed in the rear flat face of the base 23 and is adapted to receive a square section 25 of a backing sheet that has an adhesive face on both sides covered by a protective sheet 26. The backing sheet 25 is slightly thicker than the depth of the recess 24 in order for the backing sheet to be adhesively secured to a backing surface.
The front face of device 22 is also flat, but has a U-shaped rib 27 projecting forwardly therefrom to define a socket, with the open part of the "U" facing upward. The radius of curvatuve of the U-shaped rib 27 is sized to receive one of the rubber bumpers 16 on gate 11. To facilitate entry of the bumper 16, the U-shaped rib 27 is flared outwardly at the top of each leg, as shown by the reference numeral 27a.
A mounting hole 28 is formed through the full thickness of base 23 near its top to receive a mounting screw 29, which typically would be a wood screw.
With reference to FIGS. 4-6, a mounting device for the wrought iron railing 13 is represented generally by the numeral 31. Device 31 is also preferably molded from plastic, and also comprises a rectangular base 32 having a flat backside 33. A square shallow recess 34 is formed in the backside 33 to receive a backing sheet 40 with a protective cover 41 on each side.
The front side of base 32 is also flat and includes a forwardly projecting U-shaped rib 36 identical to the rib 27, including flared portions 36a. A mounting opening 37 is formed through the rectangular base 32 near its top to receive a sheet metal screw 37.
Mounting device 31 is different from device 22 in that it is formed with a pair of spaced, parallel sides 38 that project rearwardly from each side edge of the rectangular base 32 (FIG. 5).
Also projecting from the rear face 33 of base 32 are four integrally formed frangible pegs 39 that are arranged in pairs, with each pair disposed in parallel relation to the sides 38.
The mounting posts 21 of conventional wrought iron railing are generally square in cross section, the sides of which are typically 1 inch, 11/8 inches or 11/4 inches in size. The sides 38 and pegs 39 are spaced to accommodate any of these sizes. Thus, the inside lateral spacing between the pairs of pegs 39 is slightly greater than one inch, the inside dimension between each pair of pegs 39 and the farthest side 38 is 11/8 inches, and the inside dimension between the sides 38 themselves is 11/4 inches. The pegs 39 are frangibly constructed (i.e., they can be broken away as shown in FIG. 5), and selected removal of one or more pairs of pegs 39 thus accommodates any of the sizes of posts 21.
In the example shown in FIGS. 5 and 6, the wrought iron corner post 21 has a mounting side that is 11/8 inches in size, and accordingly, one pair of the pegs 39 is removed (FIG. 5) to accomplish the necessary spacing for the device 31 to fit onto the corner post 21.
In mounting the gate 11, four mounting devices 22 or 31 are necessary, two for each side of the gate 11 corresponding to the number of rubber bumpers 16. In this particular installation, since the gate 11 is intended to close the space between the wall 12 and wrought iron railing 13, two mounting devices 22 are used for the wall 12, and two mounting devices 31 are used for the railing 13.
Placement of the devices 22, 31 must of course be based on the spacing of the lower bumpers 16 relative to the bottom of the gate 11 and the space between the lower and upper bumpers 16. Placing the lower mounting devices in the correct position will insure sufficient clearance between the bottom of the gate and the floor while avoiding excessive clearance.
With this initial dimension in mind, one side of the protective sheeting 26 is removed from one of the backing sheets 25, and the sheet 25 is placed into the shallow recess 24 of one of the wall mounting devices 22. The other protective sheeting 26 is now removed, and the mounting device 22 is placed in the lower position as shown. While the adhesive backing sheet 25 will itself sufficiently hold the wall device 22 in place, additional mounting strength may be obtained by drilling a pilot hole in the wall 12 through the hole 28 and inserting a wood screw 29.
The upper wall device 22 is now placed directly above the lower wall device 22 in the same manner, the spacing therebetween being based on the spacing between rubber bumpers 16.
On the opposite side, a rail mounting device 31 is prepared for the corner post 21 by first removing four, two or none of the pegs 39, depending on the size of the corner post 21. As pointed out above, the width of the corner posts 21 where the rail device 31 will be mounted is 11/8 inches in width, thus necessitating the removal of two of the pegs 39 as shown in FIG. 5. If a burr is left from this removal, it may be filed off to insure that the rear face 33 will fit flush against the corner post 21.
The backing sheet 40 is now placed in the shallow square recess 34 by removal of one of the protective sheets 41, and following removal of the other protective sheet 41, the wall device 31 is adhesively pressed into place on the corner post 21 at a height above the floor corresponding to that of the lower wall devices 22. If further mounting strength is desired, a pilot hole may be drilled in the corner post 21 and a sheet metal screw 37 inserted. The upper rail device 31 is now placed on the corner post 21 in the same manner and at the same height as the upper wall device 22.
With the four mounting devices 22, 31 in place, the gate 11 may now be removably mounted in the stairwell opening. This is accomplished by initially placing the gate 11 between the mounting devices 22, 31, expanding the gate 11 by sliding the relatively movable sections 14, 15 apart to the approximate opening space, and thereafter lockably expanding the gate 11 and locking it through the means shown in U.S. Pat. No. 4,607,455. In this mounted position, a child or pet is safely prohibited from moving past the gate 11. The locking mechanism of the gate cannot be operated by a child or pet, and the mounting devices 22, 31 offer further security because they preclude any lateral force on the gate 11 from causing it to be dislodged or moved in any manner.
Notwithstanding the strength and security offered by the mounting devices 22, 31, the gate 11 is easily removed when necessary by releasing the gate locking mechanism and sliding the gate sections 14, 15 together.
It is to be reiterated that the mounting sockets 22 and/or 31 may be used with frictional bumpers 16 on any type of security gate if the width of the gate is adjustable to conform to the width of the opening to be secured. There are many types of security gates commercially available for this purpose having a variety of approaches to width adjustment.
Further, although the bumpers 16 are circular in this embodiment, it is possible for the bumpers and devices 22, 31 to be of different configurations without departing from the scope of the invention, so long as they are of complementing shape.
It is also possible to mount the security gate 11 through the use of hinges on one side and mounting devices on the other, also to the extent the width of the gate is capable of being adjusted. An example of such mounting is shown in U.S. Pat. No. 4,607,455, to which reference is made.
It will be appreciated from the foregoing that the inventive mounting devices 22, 31 permit the gate 11 to be mounted safely and securely in a variety of environments without concern that the gate 11 will be dislodged or moved in any manner. | A mounting device is disclosed for a portable, expansion-type security gate for children or pets. The expansion gate has a variable width with frictional bumpers on each side that frictionally engage a door jamb or other doorway defining member. The mounting device consists of a socket defining mounting member for each frictional bumper that is secured to the door jamb and is configured to receive and retain the frictional bumper. One type of mounting member is configured to mount on flat surfaces such as door jambs and walls. Another mounting member is constructed to mount on a wrought iron railing. Both types rigidly support the security gate and prevent it from being accidentally dislodged. | 4 |
This is a continuation of application, Ser. No. 08/589,272, filed Jan. 22, 1996, abandoned.
BACKGROUND OF THE INVENTION
The invention relates to a drive unit, specifically for a motor vehicle, including an internal combustion engine, a transmission and a hydrodynamic retarder including a rotor and stator.
Such a drive unit is known from DE 37 13 580 C1.
Retarders are employed primarily in heavy vehicles to absorb the kinetic braking energy accruing notably in braking actions at high speed of travel (adaptation braking) and to convert it to heat. But retarders are suited well also for required sustained braking outputs, for instance at a constant speed of 30 km/h on an incline of 7%. Oil serves normally as the operating fluid. The heat transferred in the retarder to the operating fluid must be delivered, by means of a heat exchanger, to the coolant or ambient air.
The retarder described in U.S. Pat. No. 3,720,372 is integrated in the engine of the drive, permanently joined to the crankshaft and constantly flooded by the coolant of the cooling system. The rotor of the retarder serves as circulating pump, instead of utilizing a separate coolant pump. The purpose of this system is to cause heating of the coolant by means of the retarder for heating the passenger compartment. The same purpose serves also a control system arranged on the retarder, which controls merely the distribution of the coolant, depending on its temperature in a bypass line through the radiator.
Also known, from DE-PS 33 01 560, is a retarder which by way of a clutch is connected to the crankshaft of the drive engine and to the driven wheels of the vehicle. But the purpose of the retarder is not absorbing and converting high kinetic braking energy of the vehicle to heat. The retarder is operated exclusively as a heater, with the heating output meant to be controlled with a view to an available operating energy input. The coolant of the engine is likewise the operating fluid of the retarder.
A retarder described in DE-AS 1 946 167 (U.S. Pat. No. 3,650,358) is powered by the crankshaft of an internal combustion engine whose coolant serves also as operating fluid for the retarder. The advantage of this mode of operation is that the accruing heat develops directly in the coolant passed to the radiator and that a heat exchanger between two fluids is not needed. The rotor is mounted on an antifriction bearing and the seal between frame and rotor shaft is established by two lip seals.
The desire with drive units of this type is to keep the axial overall dimension and the weight as low as possible, especially when the drive unit is intended for a motor vehicle. With the drive units known heretofore, this was not achieved to a desirable degree.
SUMMARY OF THE INVENTION
The objective underlying the invention is to fashion a drive unit in such a way that the axial overall dimension and the weight will be less than with prior drive units.
In accordance with the present invention, the rotor of the hydrodynamic retarder is mounted either on the engine shaft or on a crankshaft journal coaxial therewith, and the stator is disposed, in the axial direction, between the crankcase and rotor. The following advantages result from a drive unit in accordance with the present invention:
The cantilevered mounting of the retarder rotor makes unnecessary a separate bearing, or in some cases two separate bearings, for the rotor of the retarder. This reduces the axial length.
Also with a given internal combustion engine the space between the fan and crankcase, in front of the engine, can be utilized for the retarder, without requiring an appreciable modification of the crankcase and fan.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is more fully explained with the aid of the drawings, which in detail show the following:
FIG. 1, a drive unit in side elevation and partly in axial section along line A--A of FIG. 2;
FIG. 2, the same drive unit in plan view toward the engine shaft, with the fan wheel removed; the fly circle of the fan wheel indicated by dash-dot line;
FIG. 3, an enlarged sectional view along line B--B of FIG. 2;
FIG. 4, the retarder 4 in a plan view in the direction of the engine shaft;
FIG. 5, in a view analogous to FIG. 2, an intermediate body between crankcase and retarder;
FIG. 6, an enlarged section of FIG. 1;
FIG. 7, an enlarged section of FIG. 2 along line C--C; and
FIG. 8, an enlarged section of a portion of FIG. 1.
DETAILED DESCRIPTION
FIG. 1 depicts only a few parts of the engine, among others, the crankshaft 1, connecting rod 1.1, a crankshaft journal 1.2 screwed to the end face of the crankshaft 1, and a crankcase 1.3. Located to the left of crankcase 1.3, in FIG. 1, are a retarder 2 and fan 3.
The retarder 2 includes a rotor impeller wheel 2.1 and a stator impeller wheel 2.2. Rotor impeller wheel 2.1 is mounted in a cantilevered fashion on the crankshaft journal 1.2. The retarder includes a housing which is structured of a bell 2.3 surrounding the stator impeller wheel 2.2 and a cover body 2.4. The crankshaft journal 1.2 also supports a damper device 2.5 joined to the crankshaft journal 1.2 in rotationally fixed fashion.
Fan 3 is rotated by the crankshaft 1 of the engine by way of a gearset, which is illustrated only in part. As can be seen, fan shaft 3.2 extends parallel to crankshaft journal 1.2.
The arrangement is such that retarder 2 occupies virtually the entire space bounded by the end face of crankcase 1.3 facing retarder 2 or the gearset driving fan 3, additionally by fan shaft 3.2 and, lastly, the rear edge of fan wheel 3.1. Retarder 2 with cover body 2.4 is contained, in plan view relative to FIG. 2, within the fly circle of the fan wheel 3.1. Thus, the space is utilized optimally.
A very decisive advantage of this arrangement of retarder 2 in the space between crankcase 1.3, fan shaft 3.2 and fan wheel 3.1 is that the air flow generated by fan wheel 3.1, due to the spatial proximity between fan wheel 3.1 and retarder 2, removes from the outside surfaces of the latter heat generated by braking action. Thus, the requirements of a heat exchanger coordinated with the retarder are reduced substantially.
With retarder 2 located directly in front of the engine (cold side of engine cooling), the mass of water contained between the retarder inlet and the radiator, along with the mass of the engine oil and, prorated, with the metal mass of the cooling system including the engine, can be utilized for capacitive energy absorption. The heat capacity available to the retarder is increased thereby and the braking output can briefly be greater than the continuous heat dissipation of the vehicle radiator.
The compact arrangement according to the invention reduces the piping to a minimal length. This also minimizes the problems which in conventional drive units derive from relatively long piping paths.
The cover body 2.4 serves several functions:
It forms part of the retarder housing by enclosing the rotor impeller wheel 2.1.
As a hollow body it forms a collecting chamber with three ports, namely two inlets and one outlet for the medium, which due to the configuration of this drive unit is simultaneously a cooling medium and an operating medium (so-called water pump retarder); drawing cooling water from the vehicle radiator, one of the three ports, namely 2.8, which draws cooling water from the vehicle radiator, is illustrated in FIG. 1, and the two other ports 2.9 are shown in FIGS. 3 and 4.
The cover body 2.4 bears on the crankcase 1.3, either directly or via the bell 2.3, or otherwise on the fixed surrounding structure, thus forming a torque support.
The cover body 2.4 is joined to the stator housing or bell 2.3. It thus supports stator housing 2.3 or, vice versa, the stator housing 2.3 supports the cover body 2.4. Additionally, it serves as a centering element for stator housing 2.3, or the stator housing for the cover body, thus being able to center at the same time the mechanical seal between stator housing 2.3 and crankshaft journal 1.2.
The cover body 2.4 supports the stator impeller wheel 2.2, and is joined to it by a slip-on joint and rests axially on the joining surfaces 2.7.
The advantages resulting from this arrangement are manifold. Primarily the design and arrangement of the cover body contributes to the compactness of the design. The entire drive unit is service-friendly, since removal of the fan wheel 3.1 and the cover body 2.4 provides free access to all major parts.
While in the illustrated embodiment no separate crankshaft journal 1.2 is used, this is possible, of course. In the example, the crankshaft journal 1.2 is fashioned to the crankshaft 1, the crankshaft journal 1.2 and crankshaft 1 forming a single component.
FIG. 3 depicts once more the major components, as far as these relate to the structure of the retarder. Specifically, it illustrates that cover body 2.4 connects to the relevant piping ports in slip-on fashion. As follows from the above, the rotor 2.1 of the retarder 2 is preferably mounted in a cantilevered fashion; it is thus supported by the crankshaft bearing.
There is provided in a particularly skillful manner an intermediate body 4, which is located between crankcase 1.3 and fan 3, mounted on crankcase 1.3 and borders directly on cover body 2.4. Intermediate body 4 supports a plurality of elements, such as a complete fan assembly 3 including its shaft 3.2 and impeller wheel 3.1. Additionally, it centers the housings 2.3 and 2.4 of the retarder 2 and it can support additional units, for instance, thermostats.
The silhouette of intermediate body 4 can be seen in FIG. 5--indicated there by heavy lines. Visible, in detail, are the inlet port 4.9 for the coolant to the engine and the outlet port 4.10 from the crankcase. Further visible is an idler pulley 4.11 for the V-belt of the accessory machines and attachment points 4.12 for a console 4.13 supporting auxiliary units. Located at the upper right in FIG. 5 is an outlet port 4.8 for coolant flowing to the radiator.
FIG. 6 shows the environs in the area of the fan shaft 3.2. Visible, in detail, are again the intermediate body 4, crankcase 1.3, a thermostat housing 4.1 as well as one of the thermostats 4.2, and a duct 4.4 as a short-circuit connection for fluid to the retarder 2.
FIG. 7 shows among others a housing part 4.5 as a gear closure, along with the gears 4.7 for driving the fan 3, fan shaft 3.2, and shows as well the slip-on joint 2.9.
FIG. 8 depicts the retarder 2 in a more detailed fashion. As can be seen, the stator impeller wheel 2.2 is contained between crankcase 1.3 and rotor impeller wheel 2.1. Expressed differently, stator impeller wheel 2.2 is in relation to the engine near, while the rotor impeller wheel 2.1 is away. The cover body 2.4 is firmly screwed to bell 2.3.
The rotor impeller wheel 2.1 features on its back, near the cover body 2.4, pump blades 2.10. Hence, the rotor impeller wheel 2.1 exercises not only its function as rotor of the retarder 2, but at the same time also that of a pump. Naturally, the necessary packings are provided between the components rotating relative to one another, for example, packings 2.11 and 2.12 between rotor impeller wheel 2.1 and cover body 2.4.
While this invention has been described as having a preferred design, the present invention can be further modified within the spirit and scope of this disclosure. This application is therefore intended to cover any variations, uses, or adaptations of the invention using its general principles. Further, this application is intended to cover such departures from the present disclosure as come within known or customary practice in the art to which this invention pertains and which fall within the limits of the appended claims. | A drive unit for a motor vehicle including an internal combustion engine, a transmission and a hydrodynamic retarder. The retarder includes both a rotor and a stator wherein the rotor is mounted on the engine crankshaft or crankshaft journal and the stator is disposed between the crankcase and rotor. | 5 |
BACKGROUND
The present invention is related generally to testing apparatus for integrated circuit chips (“IC chip” or “chip”), and more particularly to an assembly for regulating the temperature of an IC chip while the chip is mounted on a testing board so that it can be tested under predetermined temperature conditions.
Current IC chips can be designed to include hundreds of thousands of transistors, and those transistors require testing before the IC chip is delivered to a customer. Typically, each IC chip is incorporated into an integrated circuit module (IC module), and then the IC-chip in the IC-module is tested with a “burn-in” test, a “class” test, and a “system level” test. Electrical terminals are provided on the substrate which are connected by microscopic conductors in the substrate to the IC chip. The “burn-in” test thermally and electrically stresses the IC chips to accelerate “infant mortality” failures. The stressing causes immediate failures that otherwise would occur during the first ten percent of the chips' life in the field, thereby insuring a more reliable product for the customer. The burn-in test can take many hours to perform, and the temperature of the IC chip typically is held in the 90 degree C. to 140 degree C. range. Because the IC chips are also subjected to higher than normal voltages, the power dissipation in the IC chip can be significantly higher than in normal operation. This extra power dissipation makes the task of controlling the temperature of the IC chip very difficult. Further, in order to minimize the time required for burn-in, it is also desirable to keep the temperature of the IC chip as high as possible without damaging the IC chip.
The “class” test usually follows the burn-in test. Here, the IC chips are speed sorted and the basic function of each IC chip is verified. During this test, power dissipation in the IC chip can vary as the IC chip is sent a stream of test signals. Because the operation of an IC chip slows down as the temperature of the IC chip increases, very tight temperature control of the IC chip is required throughout the class test. This insures that the speed at which the IC chip operates is measured precisely at a specified temperature. If the IC-chip temperature is too high, the operation of the IC chip will get a slower speed rating, resulting in the IC-chip being sold as a lower priced part.
The “system level” test is the final test. In the system level test, the IC chips are exercised using software applications that are typical for a product that incorporates the IC chips. In the system level test, the IC chips are tested over a temperature range that can occur under normal operating conditions, i.e. approximately 20 degree −80 degree C.
During each of these tests, it is important to control and be able to test the chips under a variety of temperature ranges. Currently, to control the temperature of the chips during testing, large and expensive machines have been constructed such as those available from Delta Designs of Poway California, for example the ETC handlers (see www.deltad.com). These machines can cost up to four hundred thousand dollars or more. The temperature control of such machines requires larger volumes to be heated or cooled, and require large allocations of space and capital to operate. The present chip testing technology is in need of a low cost, efficient method of controlling the temperature of an IC chip under test.
SUMMARY OF THE INVENTION
The present invention is a small, lightweight cooling/heating chamber that can be used to test IC chips at a controlled temperature on a bench for device characterization and evaluation. This chamber can be retrofitted for use with existing test equipment and be incorporated into current test protocols without significant modification of the test equipment. The thermal chamber of the present invention is a block that has at least one inlet for a hot or cold fluid to circulate through a closed channel to heat or cool the chip, thereby reducing preheating/precooling, or “soak” time. There is also a second flow path that directly cools or heats the chip while testing. The cooling/heating chamber is designed to mate with a workpress (also referred to as a device nest or device plunger) and a docking interface plate to enclose the IC chip for testing purposes. The chamber can be designed with a ball valve or similar mechanism that controls the input of fluid into the chamber.
A clamp is also disclosed for use in securing the chip to the workpress, having a lever and pair of linkages that drive the workpress through the docking interface plate and against the chip/socket arrangement. The clamp includes spring mounted inside a block that connects to the workpress that yields a compliance for connecting to the chip. This compliance allows the downward force of the chip with the socket to be lessened, thereby reducing PCB wear and socket wear.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is perspective view of a first embodiment of the chamber of the present invention;
FIG. 2 is a cross-section of the chamber of FIG. 1 ;
FIG. 3 is a view of the chamber of FIG. 1 mounted on a docking interface plate;
FIG. 4 is a reverse view of the docking interface plate of FIG. 3 showing the workpress;
FIG. 5 is a cross-sectional view of the chamber showing the ball valve;
FIG. 6 is a view perspective view of a clamp for use with the thermal chamber in testing an IC chip;
FIG. 7 is another perspective view of the clamp of FIG. 6 showing the thermal chamber and IC chip mounted thereto; and
FIG. 8 is a perspective view, partially cut away, of the clamp assembly and the cooling chamber.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention is a thermal chamber that can be used to control the temperature of an IC chip under test. The temperature control uses a flow of fluid, which is preferably a cooled or heated gas such as air, nitrogen, or the like. The thermal chamber is designed to hold a chip socket, that itself contains an IC chip to be tested. The thermal chamber is mounted to a docking interface plate that includes a thermal insulator surrounding the thermal chamber. A work press engages a valve actuator on the thermal chamber to introduce fluid across the socket/chip surface.
FIG. 1 is a perspective view of the thermal block 10 that defines the thermal chamber. The thermal block 10 has a top side 12 and a bottom side 14 , and front 16 and rear 18 walls along with first and second side walls 20 , 22 . An aperture 24 in the interior of the block 10 allows a chip socket 26 to be inserted and held therein. The front wall 16 of the block 10 includes first and second nozzles 28 , 30 that serve as ports for the introduction and exit of a fluid such as a heated or cooled gas. Nozzle 28 serves as the port for the temperature controlled fluid to enter the block 10 , and nozzle 30 is the exhaust port where the temperature controlled fluid exits the block 10 . The rear wall 18 also includes two nozzles 32 a,b that connect to two channels 33 that are fed from a opening 31 in the block at the aperture 24 , the two channels 33 leading to the rear wall 18 and the nozzles 32 a,b, and can channel the fluid out of the block 10 from the aperture 24 . There are two fluid flow paths that are defined in the thermal block 10 , a first channel 34 that internally extends around the block 10 , entering at the first nozzle 28 and exiting through the second nozzle 30 on the front wall 16 . A second path flows the fluid through the first nozzle 28 and into a first pathway (not shown) that leads to the aperture 24 , where the fluid flows across the aperture 24 , into the opening 31 and through the two channels 33 that lead out to the two nozzles 32 a,b on the rear wall 18 . A ball valve 36 is disposed on the first nozzle's 28 entrance to govern the flow of the fluid either through the first path or the second, as set forth more fully below.
FIG. 2 shows a cross-section of the block 10 illustrating the two paths of the fluid flow. When the ball valve 36 is in a first position, the flow of the fluid entering through the nozzle 28 is directed entirely through the channel 34 , around the block 10 , until the fluid exits the exhaust nozzle 30 after having completed a path around the entire block (depicted as arrows 42 ). The fluid flowing through the channel 34 will heat or cool the entire block, thereby shortening any pre-heating or pre-cooling, also referred to as “soak.” A chip and socket disposed in the aperture 24 can be brought to the desired temperature during the soak period as the fluid circulates through the block 10 .
During the actual testing, the ball valve can be moved to a second position by depressing the actuator 38 , which blocks or partially blocks the flow path into the channel 34 while opening a flow path through the channel that leads to the aperture 24 . With the socket and chip disposed in the aperture 24 , the fluid can flow directly over the chip (depicted as arrows 48 ) to maintain even greater control on the temperature of the chip during the testing procedure. The relatively small mass of the chip will predominantly assume the temperature of the flowing gas over its surface during the test, ensuring a more accurate temperature response. The fluid flowing over the gas exits the aperture area through the opening 31 and through the channels 33 and out the nozzles 32 a,b.
The gas or temperature controlled fluid can also be directed to flow in both paths by letting the ball valve occupy a position that blocks neither the channel 34 nor the path across the socket/chip. In some embodiments, this will be the mode for normal testing, with both flow paths employed. To control the amount of flow between the two flow paths, a flow control valve 40 may be located at the end of the channel 34 that controls the area of the exit exhaust nozzle. By reducing the area, more flow will be directed in the second flow path across the chip (indicated by arrows 48 ) and less flow will be directed around the channel 34 (indicated by arrows 42 ).
FIGS. 3 and 4 illustrate how the thermal chamber can be incorporated into a testing set-up. In FIG. 3 , a docking interface plate 44 has mounted on it a thermal insulating material 46 on a first surface to prevent heat loss or heat gain into the system during the testing. The insulating material has a depth that is approximate to the thickness of the block 10 , and surrounds the block 10 while providing a pathway 47 for conduits that couple to the nozzles 28 , 30 to extend therefrom. Inside the block 10 is a socket 26 that mounts in the aperture 24 , and an IC chip 50 is mounted in the socket 26 . With the socket 26 and chip 50 in the block 10 , heating or cooling fluid such as air can be passed directly over the face of the chip while it is being tested, thereby providing an efficient method of testing the chip under a variety of different temperature conditions without using large, expensive equipment for this purpose.
FIG. 4 illustrates the reverse view of FIG. 3 , showing the underside of the docking interface plate 44 with the nozzles 32 a,b, exposed. A workpress 52 is mounted to the underside of the docking interface plate 44 , as is well known in the industry. As FIG. 4 illustrates, the thermal chamber is incorporated directly into the workpress/docking interface plate assembly without inhibiting the testing function of the chip or the testing set-up. Hot or cold air, nitrogen, or other gas can be introduced through nozzle 28 and allowed to flow over the chip 50 while the chip is being tested, and while the block 10 is temperature controlled by the same fluid.
The workpress, which can be for example a TCWP Titan Compliant workpress, can be installed in a handler or other automation equipment. The workpress picks up the chip from a tray and delivers it to the socket and thermal chamber assembly. The socket/thermal chamber may then be installed on a printed circuit board (PCB) fixture, which is mounted on a tester equipment or plugged into testing equipment. In the present set-up, the chip is seated in the socket and engaged for electrical testing before the ball valve is fully depressed for full airflow. An important feature is that the airflow will not blow the chip off of the workpress as it is being presented to the socket. That is, as the chip is being removed from the socket, the ball valve closes the airflow, preventing airflow from separating the chip from the workpress. This is important because, if the chip falls off the workpress vacuum, the machine stops and an operator must remove the chip and reset the machine, causing downtime. This feature is unique to the present set-up.
FIG. 5 illustrates the ball valve 36 at the entrance to the channel 34 , and also the flow control valve 40 at the exit of the channel 34 . The flow control valve can be a screw member 40 that blocks or partially blocks the exit 54 of the channel 34 , such that rotation of the screw member 40 in a first direction entirely blocks the exit, forcing the fluid to flow entirely through the second path 48 across the block. Conversely, rotation of the control valve 40 in the opposite direction opens the path out of the channel 34 through exit 54 (which leads to nozzle 30 ), such that more of the fluid will follow the first path through channel 34 since there is less resistance along this path. The ball valve 36 includes an occluding member 58 that blocks the path across the aperture 24 in the unbiased condition due to the force of the spring member 56 . However, when the pin 38 is depressed, the occluding member 58 compresses the spring as it lowers, exposing a channel through the block leading to the aperture 24 and across the block 10 .
FIGS. 6-8 illustrate a clamp 70 that may be used in conjunction with the thermal chamber in a manual mode. The clamp 70 works with the workpress 52 to allow for manual operation without using a large automated handler or other expensive equipment. The clamp 70 mounts on the docking interface plate 44 as shown in FIG. 6 . The clamp 70 has a manual lever 72 that pivots to open and close a pair of linkages 74 , 76 in a scissor motion, which in turn drives a base 78 that secures the workpress 52 . The workpress 52 moves vertically down through the hole in the docking interface plate 44 and against the socket 26 and chip 50 , secured on the underside of the docking interface plate 44 . The lower surface of the workpress 52 depresses the ball valve actuator 38 to direct the flow across the chip 50 as discussed above, and when the lever 72 is rotated back, the workpress 52 disengages the docking interface plate 44 and the ball valve actuator 38 springs back to the original position.
Traditional workpresses have no compliance or spring; rather, the traditional workpress includes a plunger gap of approximately one millimeter and then bottoms out. The lower portion of the workpress, (referred to sometimes as a “bladepak”), pushes directly on the chip mounted in the workpress. FIG. 8 illustrates a new workpress 52 that has compliance due to an internal spring 82 that allows resilient pressure on the chip 50 . The workpress 52 is mounted to the base 78 at a lower platform. A plunger 98 is coupled to the spring 82 , decoupling the plunger's vertical motion from the cover of the workpress. The spring may have a force of between seven and twenty seven pounds in a preferred embodiment, although the spring may be chosen to meet the needs of the particular application. The compliance can be in the range of about one millimeter, depending upon the selected spring and the tolerances desired, which provides for a chip thickness variation of up to 0.5 mm. The lower platform preferably rides on guides that allow the workpress to slide vertically, but allow some play in the vertical position to prevent damage to the chip.
The spring provides some tolerance with respect to the force of the workpress, which helps to prevent wear on the PCB and the socket by reducing the force on the socket and load boards. The compliance also has an important feature with respect to the thermal chamber. As a chip 50 is seated in the socket 26 and engaged for electrical testing before the workpress 52 engages the ball valve actuator 38 , air will be flowing around the block 10 but not across the chip 50 . It is important that the airflow does flow across the chip until the workpress is fully seated against the socket. Otherwise, the airflow can blow the chip 50 off of the workpress 52 as it is being presented to the socket 26 . As a result of the compliance in the clamp 70 , as the chip 50 is being removed from the socket 26 , the ball valve 36 closes the airflow, preventing blowoff.
The cooling/heating block 10 can take other configurations and the illustrated embodiment is meant to be exemplary only. For example, the number and placement of the nozzles can vary depending upon the requirements of the system without departing from the spirit of the invention. Similarly, the shape of the block is not critical and can take other shapes that make it convenient for the workpress and docking interface plate if necessary. Therefore, the preceding descriptions and embodiments should not be interpreted to limit the invention in any manner other than where expressly stated herein, and that the invention's scope should properly be interpreted based on the appended claims, in view of the foregoing but wherein the words of the claims are given their ordinary meaning. | A thermal chamber and system for influencing the temperature of an IC chip under test including a thermal block that receives a chip socket, the thermal block adapted to be disposed between a docking interface plate and a workpress. The thermal block receives a flow of heated or cooled gas, and causes an IC chip to become heated or cooled prior to and during a test of the chip. The thermal chamber and system allows an IC chip to be testing under specific temperature conditions without using an expensive handler costing hundreds of thousands of dollars. | 5 |
RELATED APPLICATION DATA
[0001] The present application is related to, and claims the benefit of, commonly-assigned and co-pending U.S. Provisional Application Ser. No. 61/905,132, entitled HIGH POWERED VACUUM MACHINE, filed on Nov. 15, 2013, U.S. Provisional Application Ser. No. 62/064,307, entitled HIGH POWERED VACUUM MACHINE, filed on Oct. 15, 2014, and is related to, claims the benefit of, and is a continuation in part of, commonly-assigned and co-pending U.S. application Ser. No. 29/472,851, entitled SERRATED CUTTING BLADE FOR INSULATION VACUUM MACHINE, filed on Nov. 15, 2013, which applications are incorporated herein by reference in their entireties.
TECHNICAL FIELD
[0002] The present invention relates to high-powered vacuum machines.
BACKGROUND ART
[0003] Vacuum machines are used by contractors and homeowners to recycle and/or remove undesirable material (such as insulation, leaves, twigs, and other debris) from the interior and exterior of houses and other buildings. Recycle of insulation is popular when contractors are installing loose fill insulation into walls of new buildings; removal may be required due to damage to the structure, such as from flood or fire, or may be desired during a renovation. Vacuums may also be used to pick up leaves and other yard debris when cleaning yards in autumn. Some vacuums may be used in reverse as blowers to move unwanted items such as leaves and twigs from lawns and streets. In either event, using a vacuum machine provides a safe and efficient method to recycle or remove unwanted items such as insulation from an attic or a floor on which it was over-sprayed and scrubbed off, or debris such as leaves and twigs from a yard. A hose is connected to an inlet of the machine, the other end of which is moved about in the undesirable material to be removed. Rotating vanes or blades on a flywheel within a shroud are connected to the shaft of an engine in the machine to create a suction to pull the undesirable material through the hose and into the machine. The undesirable material is then sent into a collection receptacle, either directly or through another hose connected to an outlet of the machine.
[0004] Frequently, debris may be concealed within the undesirable material and not seen by the operator of the machine. If the debris is small enough, it will pass through the machine without incident. However, larger debris, such as scrap wood left during construction, may be small enough to be pulled through the hose but too large to pass through the machine. Typically, then, the debris will enter the impeller in the shroud area. As a result, one or more impeller blades may bend or break creating an unbalanced impeller which, due to its high revolution speed, causes the vacuum to immediately vibrate with catastrophic failure occurring in seconds. Other times the debris may jam between the impeller and vacuum housing causing the impeller to stop which also creates a catastrophic failure. The catastrophic failures typically are a broken engine shaft, often combined with a broken shroud, and irreparable impeller. Repairing a broken engine shaft generally is not done; either a is replacement vacuum is purchased (typical), or a new engine is purchased to replace the current one with additional purchases of a new shroud and impeller. These repairs cannot be done in the field causing significant downtime for the vacuum user.
SUMMARY OF THE INVENTION
[0005] Current vacuum machines are (a) limited in vacuuming power due to placement of the impeller directly on the engine axle, (b) prone to costly catastrophic failures when operated in typical conditions, and (c) limited in function to either vacuum only or blow only, thereby often requiring multiple systems to complete a task. The present invention removes these limitations and provides safeguards to make for a vacuum machine that is more powerful, more robust, and more versatile than what is offered in today's market.
[0006] The present invention provides a vacuum machine, comprising: an engine having an engine shaft; a vacuum housing having an inlet and an outlet, the inlet having an inlet filter comprising a circular frame with an inner opening and a set of cross-pieces across the inner opening; an impeller within the vacuum housing. The impeller comprises: an impeller base, either circular in shape or space-aged shaped with six sides alternating between straight or radius ends for three sides, to half moon convex radius for alternating three sides, to reduce weight while providing structural support; an impeller shaft secured to the impeller base, the impeller shaft having first and second end sections with a first diameter and a middle section between the first and second end section with a second diameter larger than the first diameter, the impeller shaft allowing for any length to completely fit the hub assembly of any height of impeller; and a plurality of impeller blade modules spaced apart around, and secured to, the impeller base. Each impeller blade module comprises: a pie-piece shaped flat plate, which may or may not have a triangular piece cut out for weight savings, having two edges; and a side piece extending perpendicularly from each edge to the edge. Each side piece comprises; a back edge; a flat top edge perpendicular to the back edge, which may or may not be flat in two or more planes; and a sloped inner edge. The lower of the planes on the flat top edge may have one or more support piece(s)—circular or any shape—connecting each of the impeller blade modules. The vacuum machine further comprises a is break-away coupler connecting the engine shaft with the second end section of the impeller shaft, the coupler may be solid or a break away coupler; and a hub assembly secured to the vacuum housing around the impeller shaft. The hub assembly comprises: a first set of tapered roller bearings overlapping a portion of the first end section and abutting a first end of the middle section of the impeller shaft; a second set of tapered roller bearings overlapping a portion of the second end section and abutting a second end of the middle section of the impeller shaft; and first and second bearing mounts supporting the first and second tapered roller bearing sets.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] FIG. 1A is a side view of an embodiment of a vacuum machine of the present invention;
[0008] FIG. 1B is a front perspective view of the vacuum machine of FIG. 1A ;
[0009] FIG. 2 is a side view of a break-away coupler and hub assembly that may be used with the vacuum machine of FIG. 1A ;
[0010] FIG. 3 is an exploded view of a portion of the break-away coupler of FIG. 2 ;
[0011] FIG. 4A is a side view of the hub assembly of FIG. 2 ;
[0012] FIG. 4B is a close-up top perspective view of the hub assembly of FIG. 2 ;
[0013] FIG. 5 is a cut-away view of the hub assembly of FIG. 2 ;
[0014] FIG. 6 is a top view one embodiment of an impeller that may be used with the vacuum machine of FIG. 1A ;
[0015] FIG. 7 is a perspective view of an impeller blade module that may be used with the impeller of FIG. 6 ;
[0016] FIG. 8A is a top view another embodiment of an impeller that may be used with the vacuum machine of FIG. 1A ;
[0017] FIG. 8B is a perspective view the impeller of FIG. 8A ;
[0018] FIG. 9 is a perspective view of still another embodiment of an impeller that may be used with the vacuum machine of FIG. 1A ;
[0019] FIG. 10A illustrates a front view of an inlet filter that may be used with the vacuum machine of FIG. 1A ;
[0020] FIG. 10B illustrates the inlet filter of FIG. 10A in place on the vacuum machine is of FIG. 1A ;
[0021] FIG. 11A illustrates another embodiment of a vacuum machine of the present invention having a rotatable shroud shown in a first position;
[0022] FIG. 11B is a close up view of one embodiment of an outlet module attached to the shroud of FIG. 11A in the first position; and
[0023] FIG. 12 illustrates the shroud of FIG. 11A in a second position with an alternative embodiment of an outlet module.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0024] The described features, structures, or characteristics of the invention may be combined in any suitable manner in one or more embodiments. In the following description, numerous specific details are provided to provide a thorough understanding of embodiments of the invention. One skilled in the relevant art will recognize, however, that the invention can be practiced without one or more of the specific details, or with other methods, components and so forth. In other instances, well-known structures, materials, or operations are not shown or described in detail to avoid obscuring aspects of the invention.
[0025] FIGS. 1A and 1B are side and perspective views of a high-powered vacuum machine 100 of the present invention. The machine 100 includes an engine 110 and a vacuum housing 200 . The vacuum housing 200 has an inlet 202 and an outlet 204 . An impeller 210 ( FIG. 5 ) connected indirectly to an engine shaft is within the housing 200 and, when rotated by the engine 110 , creates suction to pull debris through a hose (not shown) connected to the inlet and release it through the outlet into a collection receptacle (not shown), such as a bag. For convenience, the machine 100 may be mounted on a wheeled frame 102 .
[0026] FIG. 2 illustrates the connection of the impeller 210 (within the housing or shroud 200 ) to the engine 110 . An engine shaft 112 is connected to one end of a coupler, such as a break-away coupler 120 . A shaft 212 , which is connected to the impeller 210 , extends through the housing 200 and through a hub assembly 300 and is connected to the other end of the break-away coupler 120 . FIG. 3 illustrates two sections of the coupler 120 . One outer section 122 connects to the impeller shaft 212 . An inner section 124 is designed to break if the torsional force on one of the shafts 112 or 212 exceeds a predetermined amount, such as if debris jams the impeller. A second outer section 126 connects to the engine shaft 112 , as shown in FIG. 2 .
[0027] Because the engine and impeller shafts 112 and 212 rotate at high speed, such as approximately 3600 RPM, it is critical that there be no wobble or “play” in the shafts 112 , 212 ; any such imbalance creates a high risk of damage to the impeller 210 , the engine 110 , or the shafts 112 , 212 . Consequently, the vacuum machine 100 of the present invention provides a hub assembly 300 around the impeller shaft 212 between the impeller housing 200 and the break-away coupler 120 . The hub assembly 300 supports the impeller shaft 212 , as illustrated in FIGS. 4A , 4 B, and 5 . The hub assembly 300 may be bolted onto the impeller housing 200 . In the FIGs., the end of the shaft 212 that is connected to the impeller 210 has been labeled 212 (A), the end that is connected to the coupler 120 has been labeled 212 (B), and the middle section of the shaft 212 that is within the hub assembly has been labeled 212 (C). Within the hub assembly 300 , the shaft section 212 (C) has a diameter slightly larger, such as ⅛ inch, than the diameter of the impeller shaft sections 212 (A), 212 (B) outside the hub assembly 300 . The impeller shaft 212 passes through the hub assembly 300 and is supported at both ends of the hub assembly 300 by tapered roller bearings 304 A, 304 B. One set of tapered roller bearings 304 A overlaps a portion of one impeller shaft section 212 A and abutting against one end of the middle section 212 (C); the other set of tapered roller bearings 304 B overlaps a portion of the impeller shaft section 212 B and abutting against the other end of the middle section 212 (C). Thus, the tapered roller bearings 304 A, 304 B are held in position by both the bearing mounts 306 A, 306 B and the larger shaft section 212 (C). As a result, the impeller shaft 212 is held securely and is prevented from moving in any direction other than rotational. That is, the hub assembly with shaft 212 supports the heavy weight, at times up to 40 lbs, of the impeller while connecting to the engine 110 and removing all torsional loads that may otherwise take place on the engine shaft 112 if it were not for this hub assembly 300 , shaft 212 , and break-away coupler 120 .
[0028] FIGS. 6 and 7 illustrate an embodiment of an impeller 210 that may be used with the vacuum machine 100 of the present invention. The impeller 210 may include an impeller base 214 and two or more precision engineered impeller blade modules, three of which 220 A, 220 B, 220 C are shown in FIG. 6 . FIG. 7 illustrates one blade module 220 A which may be formed as a pie-piece shaped flat plate 230 with two side pieces 222 A, 222 B folded perpendicular to the flat plate 230 . Alternatively, the side pieces 222 A, 222 B may be formed separately from the flat plate 230 and secured, such as by welding, perpendicular to the flat plate 230 . Each side piece 222 A, 222 B has a flat top edge 224 A, 224 B, which is parallel to the flat plate 230 , a sloped inner edge 226 A, 226 B, and a back or outer edge 228 A, 228 B, which is perpendicular to the flat top edge. The blade modules 220 A, 220 B, 220 C are symmetrically spaced apart around the flywheel 214 and may be bolted or welded, or a combination of bolted and welded, onto the flywheel 214 . In the event that a blade is damaged during use, such as from large debris being pulled into the machine 100 , it is relatively easy and inexpensive to remove and replace a blade module. And, because no balancing is necessary due to the precision engineered and formed blade modules, the repair may be performed in the field with little down time. If desired, all of the modules may be replaced at the same time.
[0029] To improve the performance of the vacuum machine 100 , the sloped inner edges 226 A, 226 B of the blades may be serrated ( FIG. 7 ). Serrations on the inner edges 226 A, 226 B allow the vacuum machine 100 to more thoroughly cut insulation and small debris before it is ejected through the outlet 204 . Such cutting may also reduce the risk that debris will jam the impeller 210 .
[0030] FIGS. 8A , 8 B are top and perspective views, respectively, another embodiment of an impeller 800 that may be used with the vacuum machine of the present invention. The impeller 800 may include an impeller base 802 and two or more precision engineered impeller blade modules 804 (three of which are shown in the embodiment of FIGS. 8 a , 8 B) symmetrically space apart around the impeller base 802 . The impeller base 802 may be a six-sided shape having three straight sides 802 A alternating with three concave sides 802 B to reduce weight, herein referred to as “space-aged shape”. The impeller modules 804 may be solid (as in the embodiment of FIG. 7 ) or may have material removed creating triangular openings 804 A for further weight reduction without reducing strength. In an alternative embodiment, the impeller base 802 may have material removed rather than material being removed from the blade modules 804 .
[0031] FIG. 9 is a perspective view of still another embodiment of an impeller 900 that may be used with the vacuum machine of the present invention. The impeller 900 includes at least one structural support for the impeller blades 902 . An inner ring 904 is secured to each impeller blade 902 at a radial location close to the sloped inner edges. An outer ring 906 is secured to each impeller blade 902 at a location close to the outer radius of impeller 900 . The rings 904 , 906 can be secured to the blades 902 by various means including welding, precision machining of a receiving and mating end, fasteners, or a combination of these methods. It will be appreciated that the rings 904 , 906 may be replaced with other shapes and configurations to provide structural support for the blades 902 and provide even weight distribution.
[0032] Referring back to FIG. 7 , the serrated inner edges 226 A, 226 B of the blade modules 220 A, 220 B reduce the risk that small debris will damage the impeller 210 . However, an inlet filter 400 ( FIGS. 10A and 10B ) secured to the inlet 202 of the vacuum housing 200 may be used to prevent larger pieces of debris, such as pieces of 2×4 lumber, from entering the inlet 202 . The filter 400 may have a annular frame 402 with an inner opening 404 having a diameter approximately the same as the diameter of the inlet 202 . A set of cross-pieces 406 within the inner opening 404 will prevent the larger pieces of debris from passing into the inlet 202 . The entire inlet filter 400 (frame 402 and cross-pieces 406 ) may be formed from a single piece of material. Alternatively, frame 402 and cross-pieces 406 may be formed separately with the cross-pieces 406 being bolted or otherwise secured to the frame 402 . The cross-pieces 406 are shown in the FIGs. as being perpendicular two bars intersecting at the center of the opening 404 . However, it will be appreciated that other configurations may also be used.
[0033] FIGS. 11A , 11 B, and 12 illustrate another embodiment of a vacuum machine 500 of the present invention having an impeller shroud or housing 502 that is rotatable about the engine/impeller shaft. The outlet 504 of the shroud 502 may thus be moved into different positions, allowing a single vacuum machine 500 to be deployed in different markets, such as commercial insulation, retail, rental, and lawn is and garden. In FIGS. 11A , 11 B, the outlet 504 is shown in a first position on one side of the machine 500 and in FIG. 12 , the outlet 504 is shown in a second position on the opposite side of the machine 500 after being rotated approximately 180°. Preferably, the outlet may be locked in any of a number of positions between the first and second positions. A spring-loaded latch pin 506 , biased toward the impeller shaft, is attached to the shroud 502 and locks the shroud 502 in place when the latch pin 510 is in a locked or released position. The latch pin 506 may be pulled outward into an unlocked position by a machine operator against the spring from the locked position to release the shroud 502 . For convenience, the latch pin 506 may have a handle 508 on the outer end. When the latch pin 506 is in the outward, unlocked position, the shroud 502 and latch pin 510 are free to rotate about the impeller shaft. The operator may then move the shroud 502 into a desired position and release the latch pin 506 . When released, the inner end of the pin 506 engages one of several notches 510 radially spaced around the perimeter of an orbital disk 512 secured to a stationary part of the vacuum machine 500 , such as on the frame, thereby locking the shroud 502 in place at that location. The spring-loaded pin 506 and corresponding notches 510 represent one method of locking the rotatable shroud 502 . It will be appreciated that the shroud 502 may be locked in place using other appropriate means.
[0034] The outlet 504 may be fitted with a variety of interchangeable outlet attachments, depending on the use to which the machine 500 is to be put. For example, FIG. 11B illustrates the shroud 502 with one type of outlet notches 512 to which a collection bag may be attached. FIG. 12 illustrates the shroud 502 with a different type of outlet notches 514 , which is more appropriate when the machine 500 is used as a blower, such as to remove leaves or other debris from a lawn.
[0035] The description of the present invention has been presented for purposes of illustration and description, but is not intended to be exhaustive or limited to the invention in the form disclosed. For example, although the description and accompanying figures are primarily directed towards a vacuum machine used to remove insulation from structures, the features described and illustrated herein may be incorporated into any high-powered vacuum machine. Further, many is modifications and variations will be apparent to those of ordinary skill in the art. The embodiment was chosen and described in order to best explain the principles of the invention, the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated. | A vacuum machine is provided, comprising: an engine secured to a frame and having an engine shaft; an impeller coupled to the engine shaft; a shroud surrounding the impeller and having an inlet and an outlet; a disk secured to the frame between the engine and the shroud, the disk having a plurality of spaced-apart notches around its perimeter; and a spring-loaded latch pin secured to the shroud and configured to engage one of the notches when in a first, locking position, and to disengage from the notch when in a pulled-back, unlocked position, thereby permitting the shroud to rotate about the impeller and lock in any of a plurality of positions corresponding to the plurality of notches. | 5 |
BACKGROUND OF THE INVENTION
Macrophages play a central role in host defense through a variety of effector mechanisms involving both membrane related and secretory events (Gordon et al., Curr. Opin, Immunol. 4, 25, 1992; Fuller, Brit, Med. J., 48, 65, 1992). Phagocytosis, chemotaxis and antigen presentation are membrane related processes involved in immunologic defense mechanisms necessary for host survival. The importance of macrophages in defense against microbes, immune surveillance, destruction of tumor cells, and in the clearing of senescent erythrocytes has been documented in man and in animal models characterized by the selective elimination of macrophages (Claassen et al., J. Immunol Meth, 134, 153, 1990). Macrophages also contribute to host defense through secretion of bacteriostatic and bactericidal proteins, cytokines and lipid mediators, as well as oxygen and nitrogen reactive intermediates. The secretory capacity of the macrophage is central to its function as these cells secrete over 100 distinct mediators and are located in every organ (Nathan, J. Clin. Invest., 79, 319, 1987).
while aberrant activation of macrophage functions is associated with autoimmune diseases as well as both chronic and acute inflammatory processes, the reciprocal condition, suppression of macrophage effector functions, is associated with reoccurring infections of both opportunistic and non-opportunistic pathogens and contributes to increased morbidity and mortality. Populations associated with an immunocompromised state include burn patients, transplants, HIV infected individuals, cancer patients undergoing chemotherapy and surgical patients, notably those with a higher risk of infection as observed in thoracoabdominal patients.
Current therapeutic approaches to these patients includes the use of intravenous infusion of macrophage derived cytokines notably the colony stimulating factors G-CSF, GM-CSF, and M-CSF (Nemunaitis, Transfusion 33: 70, 1993). Supportive therapy with antibiotics and fluids is also used however the limitations of these approaches are demonstrated by the continued problems of infection in immunocompromised patients and the emergence of more deadly strains of antibiotic resistant organisms. Furthermore, infections of immunocompromised patients with opportunistic pathogens including Pneumocystis and Cryptococcal infections remain significant and result in complications despite various antibiotic protocols. Clearly, novel therapeutics which can selectively enhance macrophage effector functions to augment host defense would play a central role in the clinical management of these patients.
Estrogen has been reported to increase select macrophage effector functions including Fc mediated phagocytosis, class II antigen expression, and IL-1 secretion. These observations coupled with the known propensity of women to be more resistant to a variety of infections (Ahmed et al., Am, J. Path., 12, 531, 1985) suggests that estrogen-like compounds may enhance macrophage effector functions and thus be beneficial in disease states associated with depressed host defense.
SUMMARY OF THE INVENTION
This invention provides methods for increasing macrophage function comprising administering to a human in need thereof an effective amount of a compound of formula I ##STR3## wherein R 1 and R 3 are independently hydrogen, --CH 3 , ##STR4## wherein Ar is optionally substituted phenyl; R 2 is selected from the group consisting of pyrrolidino, hexamethyleneimino, and piperidino; and pharmaceutically acceptable salts and solvates thereof.
Also encompassed by the invention is a method of treating an immunocompromised human comprising administering a compound of formula I to said human.
DETAILED DESCRIPTION OF THE INVENTION
The current invention concerns the discovery that a select group of 2-phenyl-3-aroylbenzothiophenes (benzothiophenes), those of formula I, are useful for Increasing macrophage function. It is believed the benzothiophenes disclosed increase macrophage function, including class II antigen expression, (hence antigen presentation), Fc mediated phagocytosis, and/or cytokine release. The therapeutic and prophylactic treatments provided by this invention are practiced by administering to a human in need thereof a dose of a compound of formula I or a pharmaceutically acceptable salt or solvate thereof, that is effective to increase macrophage function.
The term "increasing macrophage function" is defined to include enhancement or augmentation of macrophage function or activation rate so as to augment a human's defense.
The compound of formula 1 should be useful in the treatment, both prophylactic and therapeutic, in immunocompromised persons, and in particularly in thoracoabdominal surgical infections, myeloid depressed patients following chemotherapy, burn patients, HIV infected individuals, and transplant patients undergoing immunosuppressive therapy. Additional uses would include prophylactic and therapeutic uses for reoccurent bacterial, protozoan, and fungal infections, as well as in patients with Myelodysplastic syndrome and aplastic anemia in which myeloid cells are largely non-functional. It is anticipated that in any clinical entity in which Colony Stimulating Factors are being used, the compounds of formula 1 would also be useful.
Raloxifene is a preferred compound of this invention and it is the hydrochloride salt of a compound of formula 1 wherein R 1 and R 3 are hydrogen and R 2 is 1-piperidinyl.
Generally, at least one compound of formula I is formulated with common excipients, diluents or carriers, and compressed into tablets, or formulated as elixirs or solutions for convenient oral administration, or administered by the intramuscular or intravenous routes. The compounds can be administered transdermally, and may be formulated as sustained release dosage forms and the like.
The compounds used in the methods of the current invention can be made according to established procedures, such as those detailed in U.S. Pat. Nos. 4,133,814, 4,418,068, and 4,380,635 all of which are incorporated by reference herein. In general, the process starts with a benzo b!thiophene having a 6-hydroxyl group and a 2-(4-hydroxyphenyl) group. The starting compound is protected, acylated, and deprotected to form the formula I compounds. Examples of the preparation of such compounds are provided in the U.S. patents discussed above. The term "optionally substituted phenyl" includes phenyl and phenyl substituted once or twice with C 1 -C 6 alkyl, C 1 -C 4 alkoxy, hydroxy, nitro, chloro, fluoro, or tri(chloro or fluoro)methyl.
The compounds used in the methods of this invention form pharmaceutically acceptable acid and base addition salts with a wide variety of organic and inorganic acids and bases and include the physiologically acceptable salts which are often used in pharmaceutical chemistry. Such salts are also part of this invention. Typical inorganic acids used to form such salts include hydrochloric, hydrobromic, hydroiodic, nitric, sulfuric, phosphoric, hypophosphoric and the like. Salts derived from organic acids, such as aliphatic-mono and dicarboxylic acids, phenyl substituted alkanoic acids, hydroxyalkanoic and hydroxyalkandioic acids, aromatic acids, aliphatic and aromatic sulfonic acids, may also be used. Such pharmaceutically acceptable salts thus include acetate, phenylacetate, trifluoroacetate, acrylate, ascorbate, benzoate, chlorobenzoate, dinitrobenzoate, hydroxybenzoate, methoxybenzoate, methylbenzoate, o-acetoxybenzoate, naphthalene-2-benzoate, bromide, isobutyrate, phenylbutyrate, β-hydroxybutyrate, butyne-1,4-dioate, hexyne-1,4-dioate, caprate, caprylate, chloride, cinnamate, citrate, formate, fumarate, glycollate, heptanoate, hippurate, lactate, malate, maleate, hydroxymaleate, malonate, mandelate, mesylate, nicotinate, isonicotinate, nitrate, oxalate, phthalate, teraphthalate, phosphate, monohydrogenphosphate, dihydrogenphosphate, metaphosphate, pyrophosphate, propiolate, propionate, phenylpropionate, salicylate, sebacate, succinate, suberate, sulfate, bisulfate, pyrosulfate, sulfite, bisulfite, sulfonate, benzene-sulfonate, p-bromophenylsulfonate, chlorobenzenesulfonate, ethanesulfonate, 2-hydroxyethanesulfonate, methanesulfonate, naphthalene-1-sulfonate, naphthalene-2-sulfonate, p-toluenesulfonate, xylenesulfonate, tartarate, and the like. A preferred salt is the hydrochloride salt.
The pharmaceutically acceptable acid addition salts are typically formed by reacting a compound of formula I with an equimolar or excess amount of acid. The reactants are generally combined in a mutual solvent such as diethyl ether or benzene. The salt normally precipitates out of solution within about one hour to 10 days and can be isolated by filtration or the solvent can be stripped off by conventional means.
Bases commonly used for formation of salts include ammonium hydroxide and alkali and alkaline earth metal hydroxides, carbonates, as well as aliphatic and primary, secondary and tertiary amines, aliphatic diamines. Bases especially useful in the preparation of addition salts include ammonium hydroxide, potassium carbonate, methylamine, diethylamine, ethylene diamine and cyclohexylamine.
The pharmaceutically acceptable salts generally have enhanced solubility characteristics compared to the compound from which they are derived, and thus are often more amenable to formulation as liquids or emulsions.
Pharmaceutical formulations can be prepared by procedures known in the art. For example, the compounds can be formulated with common excipients, diluents, or carriers, and formed into tablets, capsules, suspensions, powders, and the like. Examples of excipients, diluents, and carriers that are suitable for such formulations include the following: fillers and extenders such as starch, sugars, mannitol, and silicic derivatives; binding agents such as carboxymethyl cellulose and other cellulose derivatives, alginates, gelatin, and polyvinyl pyrrolidone; moisturizing agents such as glycerol; disintegrating agents such as calcium carbonate and sodium bicarbonate; agents for retarding dissolution such as paraffin; resorption accelerators such as quaternary ammonium compounds; surface active agents such as cetyl alcohol, glycerol monostearate; adsorptive carriers such as kaolin and bentonite; and lubricants such as talc, calcium and magnesium stearate, and solid polyethyl glycols.
The compounds can also be formulated as elixirs or solutions for convenient oral administration or as solutions appropriate for parenteral administration, for instance by intramuscular, subcutaneous or intravenous routes. Additionally, the compounds are well suited to formulation as sustained release dosage forms and the like. The formulations can be so constituted that they release the active ingredient only or preferably in a particular part of the intestinal tract, possibly over a period of time. The coatings, envelopes, and protective matrices may be made, for example, from polymeric substances or waxes.
The particular dosage of a compound of formula I required to increase macrophage function or treat an immunocompromised individual, according to this invention, will depend upon the severity of the condition, the route of administration, and related factors that will be decided by the attending physician. Generally, accepted and effective daily doses will be from about 0.1 to about 1000 mg/day, and more typically from about 50 to about 200 mg/day. Such dosages will be administered to a subject in need thereof from once to about three times each day, or more often as needed to effectively treat or prevent the disease(s) or symptom(s).
It is usually preferred to administer a compound of formula I in the form of an acid addition salt, as is customary in the administration of pharmaceuticals bearing a basic group, such as the piperidino ring. It is preferred to administer a compound of the invention to a female, and further to an aging human (e.g. a post-menopausal female). For such purposes the following oral dosage forms are available.
FORMULATIONS
In the formulations which follow, "Active ingredient" means a compound of formula I.
______________________________________Formulation 1: Gelatin CapsulesHard gelatin capsules are prepared using the following:Ingredient Quantity (mg/capsule)______________________________________Active ingredient 0.1-1000Starch, NF 0-650Starch flowable powder 0-650Silicone fluid 350 centistokes 0-15______________________________________
The ingredients are blended, passed through a No. 45 mesh U.S. sieve, and filled into hard gelatin capsules.
Examples of specific capsule formulations of raloxifene that have been made include those shown below:
______________________________________Ingredient Quantity (mg/capsule)______________________________________Formulation 2: Raloxifene capsuleRaloxifene 1Starch, NF 112Starch flowable powder 225.3Silicone fluid 350 centistokes 1.7Formulation 3: Raloxifene capsuleRaloxifene 5Starch, NF 108Starch flowable powder 225.3Silicone fluid 350 centistokes 1.7Formulation 4: Raloxifene capsuleRaloxifene 10Starch, NF 103Starch flowable powder 225.3Silicone fluid 350 centistokes 1.7Formulation 5: Raloxifene capsuleRaloxifene 50Starch, NF 150Starch flowable powder 397Silicone fluid 350 centistokes 3.0______________________________________
The specific formulations above may be changed in compliance with the reasonable variations provided.
A tablet formulation is prepared using the ingredients below:
______________________________________Formulation 6: TabletsIngredient Quantity (mg/tablet)______________________________________Active ingredient 0.1-1000Cellulose, microcrystalline 0-650Silicon dioxide, fumed 0-650Stearate acid 0-15______________________________________
The components are blended and compressed to form tablets.
Alternatively, tablets each containing 0.1-1000 mg of Active ingredient are made up as follows:
______________________________________Formulation 7: TabletsIngredient Quantity (mg/tablet)______________________________________Active ingredient 0.1-1000Starch 45Cellulose, microcrystalline 35Polyvinylpyrrolidone 4(as 10% solution in water)Sodium carboxymethyl cellulose 4.5Magnesium stearate 0.5Talc 1______________________________________
The active ingredient, starch, and cellulose are passed through a No. 45 mesh U.S. sieve and mixed thoroughly. The solution of polyvinylpyrrolidone is mixed with the resultant powders which are then passed through a No. 14 mesh U.S. sieve. The granules so produced are dried at 50°-60° C. and passed through a No. 18 mesh U.S. sieve. The sodium carboxymethyl starch, magnesium stearate, and talc, previously passed through a No. 60 U.S. sieve, are then added to the granules which, after mixing, are compressed on a tablet machine to yield tablets.
Suspensions each containing 0.1-1000 mg of Active ingredient per 5 mL dose are made as follows:
______________________________________Formulation 8: SuspensionsIngredient Quantity (mg/5 ml)______________________________________Active ingredient 0.1-1000 mgSodium carboxymethyl cellulose 50 mgSyrup 1.25 mgBenzoic acid solution 0.10 mLFlavor q.v.Color q.v.Purified water to 5 mL______________________________________
The active ingredient is passed through a No. 45 mesh U.S. sieve and mixed with the sodium carboxymethyl cellulose and syrup to form a smooth paste. The benzoic acid solution, flavor, and color are diluted with some of the water and added, with stirring. Sufficient water is then added to produce the required volume.
Assays
Assay 1
The procedure as set out in Freidman et al., J. Clin, Invest., 75, 162-167 (1985) (herein incorporated by reference) is carried out, with certain modifications. Between five and one hundred mice are administered oral doses in the range of 1-10 mg/kg of a compound of formula 1 on a daily basis. Following the administration, macrophages are harvested and changes in both immune (Fc mediated) and non-immune phagocytosis are quantitated by using fluorescein conjugated yeast particles prepared based on Ragsdale, J Immunol Meth, 123:259, (1989). For immune mediated phagocytosis, fluorescein conjugated yeast is preincubated with mouse sera to promote opsonization. Increase in fluorescence uptake by macrophages is quantitated by an increase in fluorescent emission using excitation and emission wavelengths of 482 and 520 nm, respectively. This procedure is used with ex vivo or in vitro macrophage cultures and changes in fluorescence units quantitated.
An increase in fluorescent units, as compared to control indicates activity of compounds of formula 1.
Assay 2
The procedure as set out in Zuckerman et al., Cell Immunol, 103:207, (1986); J Immunol, 140:978 (1988) (herein incorporated by reference) is carried out. The ability to induce class II antigens and consequently promote antigen presentation is determined on ex vivo primary peritoneal macrophages and in vitro with the murine macrophage cell line P388D1. Between five and one hundred mice are dosed with a compound of formula 1 macrophages are harvested and probed with antibodies against class II antigens of the D haplotype. Increased class II antigen expression is determined by flow cytometry using the appropriate secondary antibodies. In vitro studies evaluate the effects of the compounds in increasing the basal level and gamma interferon inducible expression of class II antigen by flow cytometry. An increase in class II expression reflect an increase in macrophage activation.
Assay 3
The procedure as set out in Seow et al., J. Immunol. Meth., 98, 113 (1987) (herein incorporated by reference) is carried out. The assay is used to evaluate increases in macrophage effector functions which uses measurements of 2-deoxyglucose uptake. Macrophages ex vivo and in vivo are plated in 96 well plates at 10 5 cells per well and incubated in phosphate buffered saline in the presence of 0.78 uCi/ml of 3H-deoxyglucose, and a compound of formula 1 is placed in the wells. Reduction in the amount of extracellular glucose reflects the uptake of this non-metabolizable glucose analog and consequently provides an independent assay for the determination of the state of macrophage activation mediated by the compound of formula 1. Increase in deoxyglucose uptake by the compound demonstrates the ability of the compounds to increase the state of macrophage activation.
Assay 4
The procedure as set out in Zuckerman, Circ Shock 29, 279 (1989) (herein incorporated by reference) is carried out to illustrate the ability of the compounds of formula 1 to protect in murine sepsis and endotoxin lethality models. Between five and one hundred mice are dosed orally with 1-10 mg/kg with a compound of formula 1 for 1 week prior to sepsis challenge. Challenge is performed using a bolus IV endotoxin injection under condition in which an LD100 is achieved (200 μg lipopolysaccharide). Exogenous glucocorticoids such as dexamethasone at 20 mg/kg serve as a positive control in increasing survival. The effects of the compound of formula 1 is also determined using a sepsis model involving cecal ligation and puncture. Sepsis by both Gram positive and Gram negative organisms results in an LD100 by 48 hours despite the use of antibiotics. An increase in the number of surviving animals or in survival time, as compared to control, demonstrates the activity of the compounds.
Assay 5
The ability of the compounds of formula 1 to increase the secretion of cytokines such as TNF is quantitated in vivo by sera measurements using commercially available TNF ELISAs specific for mouse TNF. Between five and one hundred mice are orally dosed with 1-10 mg/kg of a compound of formula 1 for one week prior to injection of a lethal or sublethal dose of lipopolysaccharide (200 and 1 μg, respectively). At one hour post LPS injection the mice are bled and the basal and LPS inducible amounts of serum TNF determined. Routinely, TNF levels below 10 pg/ml are observed prior to LPS injection and achieve levels of 5-20 ng/ml following LPS. The ability of the compounds to modulate the basal or inducible levels of TNF is determined. An increase in basal TNF without triggering massive systemic TNF release in compound treated mice demonstrates the activity of the compounds in promoting cytokyne secretion. Finally, ex vivo and in vitro measurements of TNF release from peritoneal macrophages exposed to 1-5 μM of a compound in vitro is also performed by ELISA to determine the extent of cytokine increase mediated by a compound of formula 1.
Assay 6
Five to fifty women are selected for the clinical study. The women are immunosuppressed. Because of the idiosyncratic and subjective nature of these disorders, the study has a placebo control group, i.e., the women are divided into two groups, one of which receives a compound of formula 1 as the active agent and the other receives a placebo. Women in the test group receive between 50-200 mg of the drug per day. They continue this therapy for 3-12 months. Accurate records are kept as to the number and severity of the symptoms in both groups and at the end of the study these results are compared. The results are compared both between members of each group and also the results for each patient are compared to the symptoms reported by each patient before the study began.
Utility of the compounds of formula I is illustrated by the positive impact they have in at least one of the assays described above. | A method of increasing macrophage function comprising administering to a human in need thereof an effective amount of a compound having the formula ##STR1## wherein R 1 and R 3 are independently hydrogen, --CH 3 , ##STR2## wherein Ar is optionally substituted phenyl; R 2 is selected from the group consisting of pyrrolidine, hexamethyleneamino, and piperidino; or a pharmaceutically acceptable salt of solvate thereof.
Also encompassed by the invention is a method of treating immunocompromissed individuals comprising administering a compound of formula 1. | 0 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method, system, and program for demoting tracks from cache.
2. Description of the Related Art
When data is successfully written to a hard disk drive, the drive returns a write complete message to the host system that initiated the write operation. However, if the read/write head of the hard disk drive is not operating properly, the disk drive may return a write complete without actually writing the data to the disk. In large enterprise storage systems, the disk drive may return a complete to a destage of updated data to the drives. If the read/write head does not write the data even though complete is returned, the data is lost and recovery may not be possible using error correction techniques or Redundant Array of Independent Disk (RAID) algorithms because the data was never written to the disk. This type of error is called a “dropped write” error. Further, once a read/write head starts dropping writes, typically all writes following the failed write will also be dropped.
Dropped write errors may corrupt the parity data because the parity data for the dropped write is inconsistent with the data on the drive, which does not include the dropped write. Subsequently calculated parity based on the block to which the dropped data should have been written would be corrupt because it is not calculated using the dropped data, thereby preventing recovery and reconstruction of the dropped data using the parity data.
SUMMARY
Provided are a method, system, and program for destaging a track from cache to a storage device. The destaged track is retained in the cache. Verification is made of whether the storage device successfully completed writing data. Indication is made of destaged tracks eligible for removal from the cache that were destaged before the storage device is verified in response to verifying that the storage device is successfully completing the writing of data.
BRIEF DESCRIPTION OF THE DRAWINGS
Referring now to the drawings in which like reference numbers represent corresponding parts throughout:
FIG. 1 illustrates a computing environment in which embodiments are implemented;
FIG. 2 illustrates a hard disk drive as known in the prior art;
FIGS. 3 and 4 illustrate track metadata and head verify information; and
FIGS. 5 , 6 , 7 , and 8 illustrate operations to destage and demote data in cache.
DETAILED DESCRIPTION
In the following description, reference is made to the accompanying drawings which form a part hereof and which illustrate several embodiments of the present invention. It is understood that other embodiments may be utilized and structural and operational changes may be made without departing from the scope of the present invention.
FIG. 1 illustrates a computing environment in which aspects of the invention are implemented. A host system 2 communicates Input/Output (I/O) requests to a storage device 4 through a storage controller 6 . The host 2 may communicate with the storage controller 6 via a network, such as a Local Area Network (LAN), Storage Area Network (SAN), Wide Area Network (WAN), wireless network, etc. Alternatively, the host 2 may communicate with the storage controller 6 over a bus interface, such as a Peripheral Component Interconnect (PCI) bus. The host 2 , storage system 8 , and storage controller 6 may be housed in separate housings or be included in the same housings and connect via one or more bus interfaces. The storage controller 6 may comprise any storage management system known in the art, such as a storage controller, server, enterprise storage server, etc. Still further, the storage controller 6 may be implemented in a chip set in the host 2 or in an expansion card in an expansion card slot of the host 2 . Yet further, the host 2 and storage controller 6 may comprise blades in a blade server. The storage device 4 may comprise any storage system known in the art, such as a single storage unit, e.g., hard disk drive, tape drive, optical disk drive, etc., or a Direct Access Storage Device (DASD), Just a Bunch of Disks (JBOD), a Redundant Array of Independent Disks (RAID), virtualization device, tape storage, optical disk storage, or any other storage system known in the art. The host 2 may comprise any computing device known in the art, such as a workstation, desktop computer, server, mainframe, handheld computer, telephony device, etc.
The storage controller 6 may include a processor 8 and a cache 10 . The cache 10 is comprised of one or more volatile memory devices. The storage controller 6 buffers updates to data blocks in the storage device 4 in the cache 10 before writing the updates to the storage device. A “data block” comprises any known accessible unit of data known in the art, such as a byte at a Logical Block Address (LBA), a track, a fraction of a byte, etc. Data stored in the cache 10 may also be backed up in a non-volatile storage unit 12 . The I/O code 9 includes the code to manage the storage of data in the cache 10 and the destaging of data to the storage device 4 .
The storage controller 6 further includes a memory 14 or some type of buffers maintaining the following queues and data structures to manage I/O requests, including:
Active Least Recently Used (LRU) List 16 : includes entries associated with received I/O requests that are actively being processed and the data for such I/O requests remains in cache 10 . Modified LRU List 18 : includes entries associated with a write request whose data to write to the storage device 4 remains in cache 10 and has not yet been destaged from cache 10 . Verify LRU Lists 20 , 22 : includes entries associated with write data remaining in cache 10 after the write data is destaged and completed but before the write to the storage device 4 has been verified. Unmodified Verify LRU List 24 : includes entries associated with a write request previously on one of the verify LRU lists 20 , 22 whose data was verified as being written to the storage device 4 and is eligible for demotion from the cache 10 . Current Verify LRU (VLRU) List 26 : Indicates the current verify LRU list 20 , 22 to which entries are added that are associated with write data written to the storage device 4 that is not yet verified. Device Verify Table 28 : In hard disk drive embodiments, includes information for each read/write head in a hard disk drive indicating whether the read/write head has written data and whether the read/write head was verified.
FIG. 2 illustrates components of a hard disk drive 50 as known in the art, including a plurality of platters 52 a , 52 b , which may include data on both sides of the platters 52 a , 52 b , and read write heads 54 a , 54 b , where there may be heads on both sides of every platter 52 a , 52 b . Disk drive electronics 56 position the read/write heads at different locations on the platters 52 a , 52 b to perform read/write and other disk operations.
FIG. 3 illustrates an example of track metadata 70 maintained for each track in cache 10 , where entries associated with the track may be on one of the LRU lists 16 , 18 , 20 , 22 , 24 . The track metadata 70 includes a track identifier (ID) 72 identifying the track in cache 10 , a demote attempt flag 74 indicating whether an attempt was made to demote the track from cache 10 before the storage device 4 was verified; and a verification required flag 76 indicating whether the track must be verified as having been written to the storage device 4 before being eligible for demotion.
FIG. 4 illustrates an example of an entry 80 in the device verify table 28 maintained for each read/write head in the storage device that needs to be verified. The entries include a head identifier (ID) 82 identifying a particular head in a disk drive unit. If there are multiple disk drives in the storage device 4 , then the head ID 82 would identify the particular disk drive in which the head is included. A used flag 84 indicates whether the head was used and a verify flag 86 indicates whether the head was verified. A write to the storage device 4 is verified if all heads have been have been verified since the write data was in cache 10 pending the verification.
FIGS. 5 , 6 , 7 , and 8 illustrate operations performed by storage controller 6 executing the I/O code 9 to manage updates to tracks in the storage device 4 in the cache 10 . With respect to FIG. 5 , control begins upon receiving (at block 100 ) a track update and adding the update to cache 10 . An entry is added (at block 102 ) to the modified LRU list 18 for the received track. The track in cache 10 is then destaged (at block 104 ) to the storage device 4 and the destaged track is removed from the NVS 12 but left in cache 10 until the heads of the storage device 4 are verified. The destaged track entry is removed (at block 106 ) from the modified LRU list 18 and added to the current verified LRU list 20 , 22 indicated in the current VRLU list 26 . The verification required flag 76 for the track is set (at block 108 ) to “on” indicating that the heads need to be verified before the track may be demoted and the demote attempt flag 74 is set to “off” indicating that an attempt has not been made to demote the track in cache 10 while the track is waiting verification that the data was successfully written, which means in certain embodiments, that all the heads being used were verified.
In certain situations, an update may be received to a track having an entry in one of the VLRU lists 20 and 22 . In such case, the updated track entry may be removed from the VLRU list 20 , 22 and then added to the modified LRU list 18 and processed accordingly.
FIG. 6 illustrates operations to demote tracks in cache 10 , where tracks may be demoted as part of an LRU operation to make room for new tracks being staged into cache 10 . In certain embodiments, tracks are not subject to demotion from cache 10 until they have been destaged to the storage device 4 . For each track entry in the active LRU list 16 (at block 150 ), operations 154 , 156 , and 158 are performed. If (at block 154 ) the verification required flag 76 in the track metadata 70 for the accessed track entry in the active LRU list 16 indicates that verification is needed, then the demote attempt flag 74 is set (at block 156 ) “on”. This indicates that an attempt to demote the track from cache 10 was made, but that the demotion failed because the track had not yet been verified. If the verification required 76 flag is “off, then the track entry from cache 19 is demoted (at block 158 ) and the entry for the demoted track is removed from the active LRU list 16 .
FIG. 7 illustrates operations performed to verify that the data was successfully written, or that the read/write heads are working properly. At block 200 , the storage controller 6 initiates operations to perform write and read back verify for heads in the storage device. For instance, the storage controller 6 may periodically perform a read back verify of an update written to the storage device 4 and when doing the read back verify determine which head was verified. In certain embodiments, only heads that have been used are subject to verification, as indicated in the used 84 field. The verify flag 86 for that head on which the read back verify was performed is then set to “on”. For instance, if the connection between the storage controller 6 and storage device 4 is the Small Computer System Interface (SCSI), then the SCSI SEND DIAGNOSTIC and RECEIVE DIAGNOSTIC may be used to determine the read/write head through which the read back data is verified. The SCSI WRITE AND VERIFY command may be used to perform the write and read back of the data to verify that the data was written correctly to the storage device 4 . These commands are further described in the publication “SCSI Block Commands-2 (SBC-2)”, Rev. 13, Mar. 20, 2004 (Copyright 2003 by Information Technology Industry Council (ITI)), which publication is incorporated herein by reference in its entirety. In alternative embodiments, alternative techniques may be used to determine which head was used for the write and read back verify operation. The storage device 4 is verified once all read/write heads currently being used are verified, as indicated by the verified flag 86 and used flag 84 for each head. If all the heads are not verified within a certain period of time by periodically performing the read back verify of data destaged from cache, then a write and read back verify may be performed with respect to all heads not yet checked after the time period has expired.
If (at block 202 ) the read back verify completed successfully for all heads being used, then the current VLRU list 26 is set (at block 204 ) to the other verify LRU list 20 or 22 not currently being used. After this first verify operation of all used heads, the storage controller 6 initiates operations (at block 206 ) to perform an additional read back verify for each used head in the storage device 4 . If (at block 208 ) this second or any further subsequent read back verify for all heads completes, then the storage controller 6 appends (at block 210 ) the entries in the verify LRU list 20 or 22 not indicated in the current VRLU list 26 to the unmodified verify LRU list 24 . The current VLRU list 26 is set (at block 212 ) to point to the other verify LRU list 20 or 22 . Control then returns to block 206 to perform another verification of all the heads in the storage device. Whenever a new verification operation of all used heads is performed, the verified flag 86 for all the used heads are cleared.
With these operations, entries in the VLRU list 26 are not considered verified until the verification of the heads occurs twice. The reason for using two checks to verify the successful writing of tracks having entries in one VLRU list 20 , 22 is that an entry for a track in cache 10 may be added to one VLRU list 20 , 22 while the head verification is occurring, but before the verification completes, meaning that the data was not written before the head was verified. The second verification is performed so that entries added to a VLRU list 20 or 22 while a check of all the heads is occurring are not verified and demoted from cache 10 until a check of all the storage device 4 heads occurs after an entry is added to one VLRU 20 or 22 list. This ensures that the entry added to a VLRU list 20 , 22 associated with an updated track that is written on a head is not verified until the head on which the data is written is verified in the second verification after the data is written.
If (at block 202 or 208 ) the read back for one head fails, then the storage device 4 is at risk for write dropping errors. In such case, data in the storage device set of storage units, such as hard disk drives, is recovered onto new storage device set not including the device, i.e., hard disk drive, having the head failure. For instance, if the storage device 4 comprises a set of interconnected hard disk drives configured as a RAID array, then the disk having the failed head may be swapped out and the data rebuilt using the RAID algorithm from the surviving disks. Updates in the cache 10 on the verify lists 20 , 22 , 24 , which comprise updates to tracks in the storage device 4 that have not been verified as successfully written, are then written (at block 216 ) from the cache 10 to the storage device 4 to ensure that data not verified to be in the storage device 4 is written back. In this way, data that has been verified as being stored in the disk may be recovered and updates not verified as successfully written to the storage device 4 are recovered from cache 8 as indicated in the verify lists 20 , 22 , 24 .
FIG. 8 illustrates operations for processing the unmodified VLRU list 24 . For each entry in the unmodified VLRU list 24 (at block 250 ), the operations 252 - 258 are performed. If (at block 252 ) the demote attempt flag 74 is on, then the track is immediately demoted (at block 258 ) and the entry from all other lists for the demoted track is removed. This ensures that those tracks where demotion was previously attempted are immediately demoted to avoid further delays to writing the update of that track. If the demote attempt flag 74 is “off”, then the verification required flag 76 is set (at block 254 ) to “off” and the track entry is removed (at block 256 ) from the unmodified verify LRU list 24 and left on the active list 16 eligible for demotion.
Described embodiments provide techniques for ensuring that data destaged to a storage device is removed from cache after the verifying that the storage device successfully completed writing the data to detect and avoid the drop write errors.
Additional Embodiment Details
The described embodiments for copying data between controllers may be implemented as a method, apparatus or article of manufacture using standard programming and/or engineering techniques to produce software, firmware, hardware, or any combination thereof. The term “article of manufacture” as used herein refers to code or logic implemented in hardware logic (e.g., an integrated circuit chip, Programmable Gate Array (PGA), Application Specific Integrated Circuit (ASIC), etc.) or a computer readable medium, such as magnetic storage medium (e.g., hard disk drives, floppy disks, tape, etc.), optical storage (CD-ROMs, optical disks, etc.), volatile and non-volatile memory devices (e.g., EEPROMs, ROMs, PROMs, RAMs, DRAMs, SRAMs, firmware, programmable logic, etc.). Code in the computer readable medium is accessed and executed by a processor. The code in which preferred embodiments are implemented may further be accessible through a transmission media or from a file server over a network. In such cases, the article of manufacture in which the code is implemented may comprise a transmission media, such as a network transmission line, wireless transmission media, signals propagating through space, radio waves, infrared signals, etc. Thus, the “article of manufacture” may comprise the medium in which the code is embodied. Additionally, the “article of manufacture” may comprise a combination of hardware and software components in which the code is embodied, processed, and executed. Of course, those skilled in the art will recognize that many modifications may be made to this configuration without departing from the scope of the present invention, and that the article of manufacture may comprise any information bearing medium known in the art.
The described operations may be performed by circuitry, where “circuitry” refers to either hardware or software or a combination thereof. The circuitry for performing the operations of the described embodiments may comprise a hardware device, such as an integrated circuit chip, Programmable Gate Array (PGA), Application Specific Integrated Circuit (ASIC), etc. The circuitry may also comprise a processor component, such as an integrated circuit, and code in a computer readable medium, such as memory, wherein the code is executed by the processor to perform the operations of the described embodiments.
In described embodiments, the data was verified by checking all read/write heads through which the data is written. In alternative embodiments, different techniques may be used to verify that data was successfully written to the storage device other then verifying the operability of the read/write heads being used.
FIGS. 3 and 4 illustrate information maintained for track metadata and for a head verify information. In alternative embodiments, additional or different information may be maintained.
The illustrated operations of FIGS. 5 , 6 , 7 , and 8 show certain events occurring in a certain order. In alternative embodiments, certain operations may be performed in a different order, modified or removed. Moreover, steps may be added to the above described logic and still conform to the described embodiments. Further, operations described herein may occur sequentially or certain operations may be processed in parallel. Yet further, operations may be performed by a single processing unit or by distributed processing units.
The foregoing description of various embodiments of the invention has been presented for the purposes of illustration and description. It is not intended to be exhaustive or to limit the invention to the precise form disclosed. Many modifications and variations are possible in light of the above teaching. It is intended that the scope of the invention be limited not by this detailed description, but rather by the claims appended hereto. The above specification, examples and data provide a complete description of the manufacture and use of the composition of the invention. Since many embodiments of the invention can be made without departing from the spirit and scope of the invention, the invention resides in the claims hereinafter appended. | Provided are a method, system, and program for destaging a track from cache to a storage device. The destaged track is retained in the cache. Verification is made of whether the storage device successfully completed writing data. Indication is made of destaged tracks eligible for removal from the cache that were destaged before the storage device is verified in response to verifying that the storage device is successfully completing the writing of data. | 6 |
[0001] The present U.S. patent application is a Continuation of U.S. patent application Ser. No. 12/549,205, filed on Aug. 27, 2009, and Claims priority thereto under 35 U.S.C. §120.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention is related to security authentication in computer systems, and more specifically to an authentication system that provides unified user identification across multiple namespaces.
[0004] 2. Description of Related Art
[0005] In networked computer systems, and in particular, in heterogeneous networking environments across multiple operating systems, entity authentication presents a management challenge. Entities, or in the present context, security principals, may be individual users, groups, particular machines, and the like. Entities are typically externally identified by a user ID or name that provides a symbolic tag, but internally, a numeric tag is typically associated with the entity as a practical measure. The numeric tag then provides a uniform identifier in the particular environment, such as security identifier objects (SIDs) used in Microsoft WINDOWS, or group and user identifiers as used in UNIX-type operating systems. (UNIX is a trademark of The Open Group.) Application programming interfaces (APIs) that access secured objects generally require such a numeric tag as an input, either directly or implicitly, as do gateways such as network portals.
[0006] Typically, an external database is used to map an entity identifier from one namespace to all of the various namespaces that the entity might encounter. An entity should be able to access the same set of objects irrespective of the operating system, network, machine, etc. from which an access occurs. Therefore, a large number of mappings may be required to and from various namespaces associated with various operating systems, machines and in some instances particular sub-systems or applications. Such identifier mappings have several drawbacks. First, the database must typically be fully populated before use, which is a labor-intensive process and has a high barrier to entry. Second, the reliance on an external database is a security vulnerability that is continuously exposed. Finally, it is frequently impractical to query a platform-specific database from a different platform, making the interface to the external database awkward for at least some of the access paths.
[0007] Therefore, it would be desirable to provide an identification method and system that provides uniform identification, can provide automatic population of identifiers and that adapts easily to access paths from different platforms.
BRIEF SUMMARY OF THE INVENTION
[0008] The invention is embodied in a computer-performed method, computer program product and computer system that authenticates entities generating accesses in a computer system.
[0009] Accesses to objects or gateways in the computer system, which may be a network of computers executing different operating systems, is made using canonical identifiers from a single namespace. Accesses directly specifying an identifier from the canonical namespace are made directly, while accesses made with identifiers from other namespaces are looked up in a external mapping database to obtain corresponding identifiers in the canonical namespace. If the external mapping database is not available or the identifier is not already present, a new identifier is automatically generated and used for the present access, and generally an entire session. The automatically-generated identifier is stored in an internal database and used for subsequent accesses by the same entity, making it possible to automatically populate the canonical namespace. The external database, if available, can be periodically polled to determine if the entity obtains an identifier in the same namespace mapped to by an automatically generated mapping, indicating a conflict. The external database lookup results are used to resolve the conflict.
[0010] Accesses to objects or gateways requiring an identifier from another particular namespace may be handled by a database lookup that obtains an identifier in the particular namespace that corresponds to the identifier from the canonical namespace. Alternatively, a generic identifier from the particular namespace may be assigned to all accesses from the canonical namespace.
[0011] The foregoing and other objectives, features, and advantages of the invention will be apparent from the following, more particular, description of the preferred embodiment of the invention, as illustrated in the accompanying drawings.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
[0012] The novel features believed characteristic of the invention are set forth in the appended claims. The invention itself, however, as well as a preferred mode of use, further objectives, and advantages thereof, will best be understood by reference to the following detailed description of the invention when read in conjunction with the accompanying Figures, wherein like reference numerals indicate like components, and:
[0013] FIG. 1 is a block diagram illustrating a networked computer system in which techniques according to an embodiment of the present invention are practiced.
[0014] FIG. 2 is a pictorial diagram showing accesses to objects and the relationship of identifier namespaces within the system of FIG. 1 .
[0015] FIG. 3 is a flow chart of a method in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0016] The present invention relates to computer security systems, and specifically identification of entities, including users, groups, and the like between systems and software requiring identifiers from differing namespaces. A canonical namespace is managed such that a fail-free path is provided for accesses made via identifiers from other namespaces. When an identifier from another namespace is used for the access, an external mapping database is consulted to determine if a corresponding identifier from the canonical namespace is present in the external database. If the external database is not available, or the corresponding identifier is not present in the external database, an identifier in the canonical namespace is automatically generated. The generated identifiers are stored in an internal database, making it possible to populate the internal database automatically. Accesses requiring identifiers from another namespace can be made using a canonical identifier to look up corresponding identifiers in the other namespace, or by assigning a generic identifier in the another namespaces to identifiers in the canonical namespace. The external database can be periodically polled to discover any new or changed mappings for identifiers of interest. If a new or changed external mapping is discovered that conflicts with an existing automatically generated mapping stored in the internal database, the external mapping is used.
[0017] Referring now to FIG. 1 , a networked computer system in which an embodiment of the present invention is practiced is depicted in a block diagram. A first workstation computer system 10 A includes a processor CPU coupled to a memory MEM that contains program instructions for execution by CPU, including a virtual file system (VFS) interface 11 A, which provides a native file system interface to the particular operating system executed by workstation computer system 10 A, for example the WINDOWS operating system. Workstation computer 10 A is also depicted as including a graphical display Display and input devices Input Devices, such as mice and keyboards, for interacting with user interfaces including login screens and other user interfaces for interacting with other computers connected to the network, for example, administration screens for administering identification and authorization profiles used by the techniques of the present invention.
[0018] Workstation computer system also includes a hard disc controller HDC 14 that interfaces processor CPU to local storage device 17 A and a network interface that couples workstation computer system 10 A to network 15 , which may be fully wireless, fully wired or any type of hybrid network. VFS interface 11 A provides a uniform set of application programming interfaces (APIs) that provide access to resources, such as local storage 17 A or remote storage such as storage devices 17 B and 17 C, which are coupled to network 15 by network disc controller (NWDC) 18 . An external mapping database DB, external to the VFS, provides storage for traditional administrative mapping information as will be described in further detail below, and which may be a single database, or comprise multiple databases. An internal mapping database IDB provides for storage of automatically-generated identifier mappings and is internal to the VFS, which means that internal database IDB is owned by the VFS and is not generally accessible to other sub-systems. Another workstation computer system 10 B, having an internal organization similar to that depicted in workstation computer system 10 A, is coupled to network 15 and executes a different operating system, e.g., UNIX. A different VFS client 11 B is provided and executed within workstation computer system 10 B to provide suitable native APIs for accessing storage within workstation computer system 10 B, networked storage devices 17 B and 17 C, as well as storage device 17 A within workstation computer system 10 A, if storage device 17 A is shared.
[0019] Network 15 may include wireless local area networks (WLANs), wired local-area networks (LANs), wide-area networks (WANs) or any other suitable interconnection that provides communication between workstation computer systems 10 A and 10 B, storage devices 17 A- 17 C, external database DB and any other systems and devices coupled to network 15 . Internal database IDB is generally a file stored within a storage device, such as one of storage devices 17 A- 17 C, and is thereby accessible by file system interface objects 11 A and 11 B over network 15 . Further, the present invention concerns identification functionality that is not limited to a specific computer system or network configuration. Finally, the specification workstation computer systems 10 A and 10 B and the location of their specific memory MEM and file system interface objects 11 A and 11 B does not imply a specific client-server relationship or hierarchical organization, as the techniques of the present invention may be employed in distributed systems in which no particular machine is identified as a server, but at least one of the machines provides an instance and functionality of an object or interface that performs identification in accordance with an embodiment of the present invention. The objects or interfaces process accesses according to methods and structures of the present invention, as described in further detail below.
[0020] Referring now to FIG. 2 , a pictorial diagram illustrating a relationship between identifiers and interfaces within the system of FIG. 1 is shown. The depicted structure is only one of many possible program structures for implementing the identification methodology described herein, and is provided as an example of an embodiment of a structure in accordance with an embodiment of the present invention, performing an exemplary set of accesses. An input/output request (IORQ) IORQ 1 is received at VFS interface 11 A and has associated with it, an entity identifier ID 1 from system 1 namespace 21 A, e.g., a security identifier (SID) as is used in Windows operating systems. In the example, I/O request IORQ 1 targets storage device 17 , which contains a UNIX-based file system image. In order to access target storage device 17 , a suitable identifier must be provided when VFS interface 11 A passes I/O request IORQ 1 along to the file system driver managing storage device 17 . In order to provide the identifier, VFS interface 11 A (or a remote object or service called by VFS interface 11 A) queries database DB for an entry matching identifier ID 1 . If database DB is available, and the entry is present, the member C(ID 1 ) of canonical namespace 22 corresponding to identifier ID 1 is obtained from database DB 1 . Otherwise, a new identifier is automatically generated CVD 1 ) in a reserved portion 24 of canonical namespace 22 . In practice, identifiers such as identifier CVD 1 ) are not generated for each access, rather internal database IDB stores all such automatically generated identifiers, so that subsequent accesses by the same entity will be mapped by internal database IDB directly to canonical namespace 22 . A reserved portion 24 of canonical namespace 22 is used to ensure that no overlap of automatically-generated identifiers occurs with another identifier already being used, e.g., by a mapping in external database DB. In the exemplary embodiment, the automatically-generated identifiers are constructed by incrementing a counter, as other than the uniqueness of each identifier, no special significance nor information is contained in the identifier itself, only the mapping to the corresponding identifiers e.g. identifier ID 1 in the other namespace(s) is important in general. However, alternative techniques such as hashing or other computation may be used to generate the automatically-generated identifiers. Once identifier C′(ID 1 ) is generated, it is stored in internal database IDB for future use, since any files that become owned or are created by the entity identified by identifier C′(ID 1 ) will require the owner.
[0021] In the depicted example, for generality, the file system driver managing storage device 17 is depicted as requiring identifiers from canonical namespace 22 . However, under certain circumstances, an identifier from canonical namespace 22 or another namespace may be needed as a return value to the originating platform. For example, when a query from a WINDOWS operating system is made to obtain the owner of a file which in WINDOWS is a security identifier sd.SID. In order to provide a security identifier for a file having an owner identified only in canonical namespace 22 , a conversion algorithm 26 may be used to generate an artificial, but compatible, security identifier sd.SID from canonical ID C′(ID 1 ). Alternatively, a dummy or generic identifier compatible with namespace 21 A may be provided from VFS interface 11 A in response to a request for an owner identifier of a file whose owner is not identified in namespace 21 A.
[0022] It is understood that the techniques illustrated above apply to object accesses in general, and storage devices/files are only an illustrative example of an object type for which access may be mapped according to embodiments of the present invention. Further, it is understood that the mapping provided by the above-described technique is not a 1:1 security mapping, but for automatically-generated identifiers, can provide some level of access, e.g., that level of access available to non-owner non-group members in UNIX. However, once the identifiers are populated in database DB in traditional administrative fashion, or automatically generated and stored in internal database IDB, permissions can be subsequently tailored to the entity's needs. For example, a user may access a UNIX storage device from a WINDOWS operating system temporarily, receiving access to directories such as /tmp via identifier ID 1 mapped to automatically-generated canonical namespace identifier C′(ID 1 ). Subsequently the entity can arrange for an administrator to set permissions for accessing /usr/entity1, providing the same permissions as entity1 has under their normal UNIX account, for example.
[0023] Referring now to FIG. 3 , a method in accordance with an embodiment of the present invention is illustrated in a flowchart. In the depicted method, an access attempt including an identifier ID is received by a subsystem (step 40 ). If the ID is from the canonical namespace (decision 41 ), then the access is made using the ID from the canonical namespace (step 48 ). (The illustrative embodiment of FIG. 3 presumes that the ultimate access is made from the canonical namespace, so no second lookup is required.) If the ID is not from the canonical namespace (decision 41 ), a check is performed to determine if external database DB is present (decision 42 ). If external database DB is present (decision 42 ), then a lookup is performed in database DB to obtain the corresponding identifier to identifier ID in the canonical namespace (step 43 ). If the ID maps to the canonical namespace (decision 44 ), then the access is made with the ID retrieved from database DB in the canonical namespace (step 48 ). If external database DB is not present (decision 42 ) or the ID is not mapped to the canonical namespace in external database DB (decision 44 ), then a lookup is performed in internal database to determine if a previously auto-generated mapping to the canonical namespace is already present for the entity (decision 46 ). If a previous auto-generated mapping exists (decision 46 ), the access is then made using the ID from the canonical namespace retrieved from internal database IDB (step 48 ). If a previous auto-generated mapping does not exist (decision 46 ), an ID in the canonical namespace is automatically generated for the entity and stored in internal database IDB (step 47 ), then the access is made using the new ID from the canonical namespace (step 48 ).
[0024] While the invention has been particularly shown and described with reference to the preferred embodiments thereof, it will be understood by those skilled in the art that the foregoing and other changes in form, and details may be made therein without departing from the spirit and scope of the invention. | An identification system that may be used in heterogeneous computing environments provides a fail-free path to providing identifiers from a single canonical namespace. Objects or gateways requiring an identifier for access are accessed using an identifier for the canonical namespace. If an entity requests access using an identifier from another namespace, an external database is consulted to determine if a mapping exists for the identifier to another identifier the canonical namespace. If no mapping exists, or the external database is unavailable, then an identifier is automatically generated in the canonical namespace and is used for the access. An internal database is updated with the automatically generated identifier, providing a mechanism to add mappings without administrative intervention. To access resources requiring an identifier from another particular namespace, a canonical namespace identifier may be mapped to another identifier in the particular namespace, or a generic identifier may be used. | 6 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application is a continuation-in-part of pending U.S. patent application Ser. No. 11/951,083, filed Dec. 5, 2007 which claims the benefit of the earlier filing date of co-pending U.S. Provisional Patent Application No. 60/882,122, filed Dec. 27, 2006, and incorporated herein by reference.
FIELD
[0002] Neonatal electrocardiogram screening.
BACKGROUND
[0003] Long QT syndrome (LQTS) is a genetic disease characterized by an abnormally prolonged QT interval in the electrocardiogram (ECG) waveform. LQTS is a leading cause of sudden cardiac death in the young. When infants with undiagnosed LQTS die, their sudden deaths are often labeled as sudden infant death syndrome (SIDS) because no apparent cause of death could be found by autopsy. Using post-mortem genetic analysis, researchers have found that more than 10% of SIDS cases are actually due to undiagnosed LQTS. LQTS can be diagnosed by a routine 12-lead ECG. Once diagnosed, the treatments for LQTS, including beta-blocker therapy and implantable cardioverter defibrillator (ICD), are very effective in preventing cardiac arrhythmia and sudden death. Therefore, some European countries are considering the possibility of introducing neonatal (days 15-25) ECG screening as part of their National Health Services. Among the European countries, Italian Ministry of Health funded an electrocardiogram (ECG) screening program on over 50,000 babies to assess the feasibility and outcomes of a nationwide neonatal ECG screening. The program has been tremendously successful, and such success has generated enthusiasm toward implementation of a nationwide screening program from many European nations and the United States.
[0004] Since the proposed screening ECGs are targeted at two to four weeks of life, the screenings for LQTS proposed will likely have to be done at a pediatrician's office or at home. Most nurses or nurse's assistants are not trained to perform newborn ECGs. A regular ECG machine has 10 long cables which often tangle among themselves. When conducting an ECG test, the operator needs to place 10 electrodes (stickers) on the patient and match the cables with each respective electrode on the patient. This process of untangling the cables, placing electrodes, and matching the cables and electrodes takes skill and time.
[0005] Performing an ECG on a newborn is challenging and often takes up to 20 minutes or more. Placing the leads on a newborn is difficult because of limited space on the torso and the babies are not cooperative. Furthermore, performing an ECG on a newborn using the current complicated leads system by inexperienced nurses is prone to error, such as wrong leads placement, artifacts, and inadequate ECG signal acquisition.
[0006] To solve the issues with improper leads placement and tangling of cables, prior inventions have used pre-positioned leads or one-piece design. U.S. Pat. Nos. 4,608,987 and 5,224,479 describe a vest containing pre-positioned leads, which is cumbersome to use in babies and requires a large area of skin contact when worn. Chest strip designs have been proposed by U.S. Pat. Nos. 4,233,987, 5,184,620, and 5,868,671. The limitations of these designs are that they are not designed for use in newborns and infants; and only three to six chest leads are typically provided (e.g., the strips lack limb leads) and therefore cannot be used for QT analysis. U.S. Pat. No. 6,847,836 proposes a one-piece chest pad design for use of ECG monitoring in the emergency room. The chest pad design is not specific for newborns and infants, and has a large skin contact area, which is an important limitation for use in babies because of their sensitive skin. Furthermore, the limb lead positions in the chest pad design of U.S. Pat. No. 6,847,836 are not generally proper for accurate measurement of QT intervals on a 12-lead ECG. As a result, QT analysis using such a design and system is not generally accurate.
[0007] ECG is mostly performed in adults, especially elderly people. ECG on newborns used to be a rare practice. None of the current ECG machine or leads system is designed for use in newborns or infants. As many nations are considering implementing a nationwide newborn ECG screening program, there is an urgent need for a simple, quick and error-proof ECG leads system for newborns. The current design is an ECG leads system specifically designed for newborns to be used in pediatrician's office, hospital or even at home by parents for newborn screening.
SUMMARY
[0008] An ECG system designed for performing newborn ECG is disclosed. In one embodiment, the leads system includes a chest strip which contains precordial leads; retractable limb leads, wireless connector or cable and a leads adaptor. This system with simple, pre-positioned leads allows quick and accurate leads placement for conducting newborn ECG.
[0009] A method of performing an ECG using an ECG leads system is also disclosed. In one embodiment, the method may be used on a newborn infant to detect LQTS and minimize the risk for SIDS.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 illustrates a schematic view of an embodiment of an ECG leads system including a cross-sectional top view of a chest strip, and side views of a receiver and an adapter.
[0011] FIG. 2 shows a side view of the chest strip of FIG. 1 .
[0012] FIG. 3 shows a schematic side view of two portions of the chest strip of the ECG leads system of FIG. 1 and shows retractable limb leads partially retracted.
[0013] FIG. 4 shows a schematic top view of a disposable electrode strip suitable for use with the chest strip of the ECG leads system of FIG. 1 .
[0014] FIG. 5 shows a schematic top view of a disposable electrode lead suitable for use with limb leads of the ECG leads system of FIG. 1 .
[0015] FIG. 6 shows a schematic view of the ECG leads system recording an ECG of a newborn.
[0016] FIG. 7 shows a schematic side view of another embodiment of an ECG leads system including a chest strip, a cable, and an adapter.
[0017] FIG. 8 shows a schematic top view of another embodiment of an ECG system including a chest strip and a data recorder.
[0018] FIG. 9 shows a block diagram of components of a recorder module suitable for use with a chest strip.
[0019] FIG. 10 shows two modes of operation of an ECG system.
DETAILED DESCRIPTION
[0020] An ECG leads system for conduction of newborn ECG is described. In one embodiment, this ECG leads system connects directly with an ECG machine. In another embodiment, this ECG leads system includes an adapter that can connect to the cables of an ECG machine to allow the use with existing ECG machines already in hospitals or physician's offices.
[0021] FIG. 1 illustrates an embodiment of an ECG system. In the illustrated embodiment, ECG system 100 includes the following components: chest strip 110 including a plurality of precordial leads 120 and transceiver 125 ; retractable limb leads 130 ; receiver 160 ; and adapter 170 to connect to an ECG machine. A cross-sectional top view of chest strip 110 is shown to illustrate precordial leads 120 and transceiver 125 .
[0022] In one embodiment, chest strip 110 is designed to embed six precordial leads 120 (V 1 , V 2 , V 3 , V 4 , V 5 , and V 6 ). The chest strip is shaped in a way shown in FIG. 1 so that when placed on a newborn's chest, precordial leads 120 (V 1 to V 6 ) will be in proper positions for routine ECG leads placements. As shown in FIG. 1 , the chest strip will be placed so that V 1 will be in the 4 th intercostal space (ICS) on the right sternal border, and V 2 will be in the 4 th ICS on the left sternal border. The 4 th ICS is at approximately the nipple line which is a convenient landmark for chest strip placement. Indicators for sternum position are shown on the chest strip to assist the operator to position V 1 and V 2 at opposite sides of the sternum. The positions of V 3 to V 6 will also be placed properly and chest strip 110 will be shaped accordingly. V 4 will be at 5 th ICS in the left mid-clavicular line; V 3 will be half way between V 2 and V 4 ; V 5 will be at the level of V 4 in the left anterior auxiliary line, and V 6 will be at the level of V 4 in the left mid-auxiliary line. Because the chest sizes of newborns at three to five kilograms (kg) body weight do not vary widely, chest strip 110 may be one size that will fit all. In one embodiment, the width of the chest strip is 2 cm and length is 12 cm. In another embodiment, the dimensions are reduced to fit premature infants or infants with smaller chest sizes. FIG. 6 shows chest strip 110 applied to the chest of a newborn.
[0023] In one embodiment, chest strip 110 is made of nonconductive, flexible material such as plastic, or natural or synthetic fabric. FIG. 2 shows a side view of an embodiment of chest strip 110 . In this embodiment, chest strip 110 is made of two layers of material (material layer 1105 and material layer 110 ). Chest strip 110 has surface 140 intended to face away from a newborn's skin when chest strip 110 is applied and surface 150 opposite surface 140 and having leads 150 exposed therethrough. Surface 140 of chest strip 110 is generally smooth with no exposed components. On opposite surface 150 of chest strip 110 , six round shape precordial leads 120 , each representatively 10 millimeters (mm) in diameter, are positioned in V 1 , V 2 , V 3 , V 4 , V 5 , and V 6 locations. Precordial leads 120 are made of a conductive material such as silver. Each of the leads V 1 to V 6 connects to its own wire that connects to transceiver 125 or a cable (see FIG. 5 and the accompanying text). The wires are electrically insulated from one another so that there will be no interference among the leads. In the embodiment shown in FIG. 2 , precordial leads 120 may be placed through layer 1110 with wires connected between the leads and transceiver 125 . Layer 1105 lies on the wires and hides the wires in chest strip 110 (e.g., the wires are disposed between layer 1110 and layer 1105 ).
[0024] In one embodiment, ECG system 100 shown in FIG. 1 and FIG. 2 includes limb leads 130 connected to chest strip 110 . Right limb leads 130 , RA and RL, are located on the right end of chest strip 110 when the chest strip is applied to a newborn's chest ( FIG. 1 ). Left limb leads 130 , LA and LL, are located on the left end of chest strip 110 ( FIG. 1 ). FIG. 6 shows limb leads 130 applied to a newborn
[0025] In one embodiment, a wire extends between each limb lead 130 and transceiver 125 , with a portion of each wire extending through chest strip 110 similar to the wires that connect the precordial leads 130 to transceiver 125 . The wires are electrically insulated from one another and from the wires of precordial leads 120 . As shown in FIG. 2 , in one embodiment, the wires that connect limb leads 130 to transceiver 125 extend at each end from chest strip 110 into a respective hub 145 (shown illustratively on surface 140 of chest strip 110 ). Each hub 145 includes drum 175 on which, in this example, wire 1300 is wound. Drum 175 is rotatable on axis 180 defined by axle bolt or rivet 185 and bearing 190 . Spring biased roller 195 is connected to wire 1300 interiorly of drum 175 and having a center axis co-axially aligned with axis 180 , the roller functioning to exert a retract force continuously on wire 1300 even when the wire is uncoiled from drum 175 and hub 145 . Wire 1300 is continuously biased toward a storage position in hub 145 .
[0026] The wires connecting to limb leads 130 are self-retractable or are biased toward coiling the wires in respective hubs 145 . A pulling force on a limb lead is required to uncoil a wire for a limb lead. Release of the pulling force returns the wire to a coiled configuration. In this manner, when not placed on a limb of a newborn, the leads are conveniently housed in respective hubs 145 to minimize wires tangling. When in use, after chest strip 110 is properly placed on the newborn, each of limb leads 130 can be pulled out to position in the proper places for the regular limb leads placement ( FIG. 3 and FIG. 6 ). In one embodiment, the wires for upper limb leads (RA and LA) are five inches when fully uncoiled, and the wires for lower limb leads (RL and LL) are eight inches when fully uncoiled. The lengths of the limb leads wires will allow proper placement of limb leads 130 . In one embodiment, a stop may be included on each wire when a lead is uncoiled and positioned. Such a stop may be as simple as a clip on the wire directly outside hub 145 or more elaborate such as an actuator connected to hub 145 to lock roller 195 . When an ECG recording is finished, the operator will push the actuator to unlock roller 195 and allow a wire to retract back to hub 145 and return the lead into a stored position ( FIG. 2 ).
[0027] Referring to precordial leads 120 and limb leads 130 , in one embodiment, the leads are not placed directly on a newborn's skin. Instead, disposable electrodes are representatively used to ensure good skin contact and connection with the ECG leads. FIG. 4 shows a side view of disposable electrode 300 that is in a similar shape of chest strip 110 with six round-shaped ionically conductive hypoallergenic hydrogel adhesives 320 placed in similar positions of the V 1 , V 2 , V 3 , V 4 , V 5 and V 6 leads 120 on chest strip 110 (see FIG. 1 ). In one embodiment, each adhesive 320 is 16 millimeters (mm) in diameter, with electrically conductive button 325 (e.g., a stainless steel button) in the center on a first surface. A second surface of electrode 300 is covered by a removable plastic cover. Prior to applying chest strip 110 to a newborn's chest, an operator will place the disposable electrode 300 on the underside of chest strip 110 such that each button 325 in the center of each adhesive 320 is in proper contact with the electrically conductive (e.g., silver) center of leads 120 on the chest strip. Then the operator will remove the thin plastic cover of electrode 300 to expose an adhesive side of each adhesive 320 and apply electrode 300 and chest strip 110 on the newborn's chest. In one embodiment, the adhesive between electrode 300 and chest strip 110 is hypoallergenic hydrogel. In an embodiment where the adhesive is associated only with adhesive 320 rather than the entire chest strip, the contact with a newborn's skin is minimized.
[0028] FIG. 5 shows disposable electrode 305 that may be used with the limb leads 130 . Electrode 305 includes round ionically conductive hypoallergenic hydrogel adhesive 330 , 20 mm in diameter, with a conductive (e.g., stainless steel) button 335 in the center on one surface to contact a conductive portion of limb lead 130 . A removable plastic cover may be placed over a second adhesive surface of adhesive 330 . The cover will be removed prior to attaching the electrode on the newborn. In one embodiment, a hypoallergenic hydrogel is provided on the adhesive surface of each electrode 305 that will ensure good skin contact. After chest strip is placed properly on the chest, the operator will pull each individual limb leads out and clip or snap on a respective electrode 330 .
[0029] As noted above, in one embodiment the wires from limb leads 130 (RA, RL, LA, LL) and precordial leads 120 (V 1 , V 2 , V 3 , V 4 , V 5 , V 6 ) run through chest strip 110 individually and connect to transceiver 125 . Transceiver 125 is, for example, a Bluetooth chip located at the left end of chest strip 110 . In one embodiment, transceiver 125 is programmed to receive and transmit ECG signals from limb leads 130 and precordial leads 120 . In the embodiment of ECG system 100 shown in FIG. 1 , transceiver 125 wirelessly sends ECG signals received from the various leads to receiver 160 , such as a Bluetooth chip. Receiver 160 then distributes the received signals to contact points of adaptor 170 (contact points corresponding to signals for six precordial leads V 1 , V 2 , V 3 , V 4 , V 5 , V 6 , and four limb leads RA, RL, LA, LL). Such signals may be transmitted from adaptor 170 by hard wiring a connection between the contact points and an ECG machine (see FIG. 6 ).
[0030] In one embodiment, adaptor 170 is designed to make ECG leads system 100 compatible with existing, commercially available ECG machines. In one embodiment, the contact points on adaptor 170 are the same as used on regular ECG electrodes, which allows the leads from commercial ECG machine to clip on or clamp on. FIG. 6 shows ECG system 100 connected to ECG machine 195 and illustrates an ECG signal displayed on ECG machine 195 .
[0031] FIG. 7 shows another embodiment of an ECG system where the connection between a chest strip and a leads adaptor uses wired cable instead of wireless technology. FIG. 7 shows chest strip 410 including precordial leads 420 (V 1 , V 2 , V 3 , V 4 , V 5 , V 6 ). FIG. 7 also shows limb leads 430 (RA, RL, LA, LL) connected by individual wires to chest strip 410 . The wires for precordial leads 420 and limb leads 430 extend into harness 450 which connects to adaptor 470 . The signals at adaptor 470 may then be transferred (e.g., via wires) to an ECG machine. Alternatively, harness 450 may connect limb leads 430 and precordial leads 420 on chest strip 410 directly to an ECG machine without the use of adaptor 470 . The wires inside harness 450 are electrically insulated from one another. A representative length of harness 450 is from one foot up to 12 feet depending on the needs.
[0032] FIG. 8 shows an embodiment of an ECG system shaped for proper positioning of leads on a newborn. FIG. 8 shows chest strip 510 with leads individually wired into flexible printed circuit board 515 disposed in or on chest strip 510 .
[0033] Chest strip 510 is shaped to conform to the anatomic positions of a newborn for the placement of the six precordial electrodes connected to leads (electrodes) (V 1 , V 2 , V 3 , V 4 , V 5 , and V 6 ). RL electrode is positioned at the left lower corner of the strip (as viewed) to serve as the reference (ground) electrode. In this embodiment, three limb electrodes (RA, LA, LL) are connected to the chest strip by individual wires which run through chest strip 510 with six inches of extra wires outside the strip to connect to electrodes. The electrodes may be similar to electrodes described above (see FIG. 5 ). When the electrodes are detached from the chest strip, the RA, LA and LL electrodes can each be pulled to its respective anatomic position and still maintain a respective wire connection to the chest strip.
[0034] In this embodiment, chest strip 510 has three anatomic landmarks to assist proper electrode positioning; sternum mark 550 to place V 1 and V 2 electrodes on either side of the sternum, nipple line mark 555 for positioning V 1 and V 2 at the level of the 4 th intercostal space, and left nipple mark 558 above the V 4 electrode to ensure that the chest strip is of appropriate size for the infant. The weight of 2-4 week old infants can vary, with the majority weighing 3 kg to 5 kg. To make the chest strip appropriate for newborns of various body sizes, the chest strip may be made in different sizes, e.g., one for newborns weighing approximately 2.5 kg to 4 kg and another for newborns weighing over 4 kg.
[0035] An upper or top surface of chest strip 510 , in one embodiment, is covered by smooth fabric material with no exposed components. On the opposite or undersurface of chest strip 510 (intended to be in contact with the skin of a newborn), seven round shape electrodes, each 10 mm in diameter, are positioned in RL, V 1 , V 2 , V 3 , V 4 , V 5 , and V 6 locations. The 10 mm electrodes contact surface is made of hydrogel adhesives. All chest and limb electrodes are connected to leads that are individually wired through chest strip 510 and connect to recorder module 525 on the right end (as viewed). In one embodiment, recorder module 525 is detachable from chest strip 510 . Representatively, the leads in chest strip 510 terminate in a pin connection that mate or otherwise connect with terminals of recorder module 525 . A snap on connector is designed to enable the connection of the wires from the chest strip to the recorder module. In one embodiment, the male connector of the snap on connector is at the chest strip and the female connector is at the recorder module. In one embodiment, the female connector at the recorder module is connected to an analog front end in the recorder module so that the analog signals from the chest strip are directed to the analog front end to be processed and converted to digital signals.
[0036] Referring to FIG. 9 in one embodiment, recorder module 525 contains two components, analog front end 5210 and digital data recorder 5220 . Representatively, analog front end 5210 includes: preamplifier 5212 , low pass filter 5214 , amplifier 5215 , and high pass amplifier 5216 . The analog front end receives the electrical signals collected from the leads/electrodes in chest strip 510 (e.g., signals from 10 leads/electrodes) and amplifies the signals to a suitable level (in mV) for signal processing. The bandpass filters are used to filter out the noise and select the frequency of interest at, for example, 0.04 Hz˜150 Hz. After ECG signals are amplified and noise-filtered, the analog signals are converted to digital signals by the analog-to-digital converter (ADC) 5218 .
[0037] In one embodiment, analog front end or receiver 5210 utilizes an ADS1298, a fully integrated analog front end chip for 12-lead ECG by Texas Instrument (TI). The ADS1298 has an integrated design on a single chip that is 12 millimeters (mm) by 12 mm by 0.8 mm, suitable to be accommodated on chest strip 510 . ADS1298 is equipped with eight high-resolution, simultaneous sampling ADCs and integrated amplifier. The chip is also capable of digital pace detection and continuous lead-off detection.
[0038] Digital data recorder 5220 of recorder module 525 receives digital signals from analog front end 5210 (e.g., from ADC 5218 ) and, in one embodiment, writes the data on to a flash memory or sends the data to a wireless transmitter. The main components of digital data recorder 5220 include a microcontroller (MCU) 5222 , flash memory 5224 , wireless transmitter 5226 , and a battery (not shown). MCU 5222 will regulate the data flow as well as manage the power. In one embodiment, the battery is a rechargeable Li-Polymer battery that will supply power for the entire detachable ECG Recorder Module. The default data flow function by MCU 5222 is to write the data to the flash memory. A mini-USB port may be placed for accessing the flash memory recording via a USB cable connecting to a processor (e.g., a computer). A user can switch the data to be directed to wireless transmitter 5226 , which will send the data instantly. The transmitted data will be received by a wireless receiver connected to the processor.
[0039] Once chest strip 510 is placed on the infant, the analog front end 5210 will detect and ensure all electrodes have proper skin contact and signals. If there are leads off detected by ADS1298, a red signal light will be on. 12-Lead ECG data can be recorded continuously for many hours, until the flash memory is full, or until the battery power runs out. For the purpose of long QT syndrome screening, continuous ECG recording of 30 minutes typically results in adequate ECG data for reliable analysis. When the user finishes ECG data acquisition, in one embodiment, recorder module 525 , may be detached (removed) from chest strip 510 . In one embodiment, chest strip 510 is designed to be one-time use and will be disposed. The recorder module 525 can be transmitted (e.g., carried, mailed, etc.) by the user to a data center for ECG interpretation and data storage. Once any data on recorder module 525 is delivered to a data center by, for example, connecting recorder module 525 to the processor. Following any transmission, the data is transmitted to a processor at the data center, recorder module 525 may be sterilized, its battery recharged if necessary, and then the module can be attached to a new chest strip to be ready for use on the same or another infant.
[0040] FIG. 10 presents two modes of operation of the ECG systems described with reference to FIG. 8 and FIG. 9 . In the first mode (identified by identifier 600 ), upon a baby's discharge after birth, the parents of the baby receive an ECG system from the hospital. When the baby is two to four weeks of age, the parents perform an ECG according to instructions. Once acquisition of ECG data is complete, the recorder module is detached and transported (e.g., mailed) to a central lab. At the central lab, the ECG data is retrieved and interpreted, and the recorder module is sanitized and recharged for reuse.
[0041] In the second mode of operation (identified by identifier 700 ), the ECG system is available at a pediatrician's office or other examination room. Representatively, at a baby's 2-week-old well childcare visit, a nurse places the device on the baby while taking vital signs. ECG data is continuously transmitted to a wireless receiver in the office for 30-60 minutes, until the baby is ready to go home. The wireless receiver can connect to a PC via a USB port, or to a router via an Ethernet port to forward the ECG data via the Internet to a secure server at a central lab. The recorder module will be sanitized at pediatrician's MD office for reuse on the next baby.
[0042] The ECG system described herein has many advantages over traditional ECG leads and cables. In particular, the ECG system described herein has a simple design that is easy to use, relatively error-proof, and compatible with current ECG machines. The ECG system described herein also minimizes skin contact on newborn thereby decreasing the risk for infection and/or skin reaction.
[0043] In the preceding detailed description, the invention is described with reference to specific exemplary embodiments thereof. It will, however, be evident that various modifications and changes may be made thereto without departing from the broader spirit and scope of the invention as set forth in the claims. The specification and drawings are, accordingly, to be regarded in an illustrative rather than a restrictive sense. | An apparatus including a chest strip comprising a plurality of precordial and limb leads for an electrocardiogram (ECG) and an ECG data recorder coupled to the chest strip, wherein the ECG data recorder configured to receive signals from the leads. An apparatus including a chest strip comprising a plurality of precordial leads positioned to correspond with desired lead placement for an electrocardiogram (ECG) and an ECG data recorder; a plurality of limb leads coupled to the chest strip, wherein the ECG data recorder is coupled to plurality of precordial leads and the plurality of limb leads and configured to receive electrocardiogram data generated by the plurality of precordial leads and the plurality of limb leads. A method including coupling a chest strip including precordial leads and a data recorder to a newborn, the data recorder configured to receive electrocardiogram data from the precordial leads; and transmitting electrocardiogram data from the data recorder. | 0 |
BACKGROUND OF THE INVENTION
The present invention relates in general to dispensing and container devices and more particularly to an improved container-dispensing apparatus for effectively storing and dispensing disposable diapers of various sizes.
Only within the last ten years has the utilization of individually packaged disposable diapers for infants come into widespread use. Prior to that time, and to a substantial degree today, parents relied upon diaper service for conventional cloth diapers or went through the inconvenience and labor of washing and maintaining a stock of equivalent cloth diapers.
With the widespread use, availability, and relative low cost of disposable diapers, users of these substantially paper products, though greatly convenienced, have been confronted with problems inherent to the storage and dispensing of such products. Parents for example, have often stored such disposable diaper products in large bulky cartons in closets only to find that, at the most inconvenient time, it was necessary for them to lay the infant down while they ran to get a new sanitary disposable diaper.
Another problem that has arisen with regard to the utilization of such paper products is the availability of the diapers in several sizes to accommodate different purposes. Different sizes of disposable diapers have been manufactured for infants and toddler body sizes, as well as daytime and nighttime thicknesses. With all these and other various sizes and shapes of the diapers, parents have experienced confusion in keeping the diapers properly organized as to type of diaper, have lost diapers in conventional storage areas, such as closets and the like, and have often run into situations where the protective packaging has been torn or ruined, exposing the paper diapers to dirt and germs.
It is thus an object of the present invention to provide a container and dispensing apparatus which may be unobtrusively integrated into an infant's room to appear to be a toy.
It is further an object of the present invention to reduce inadvertent loss or tearing of the disposable diapers and the protective packaging in order to reduce the cost involved with regularly maintaining a stock of disposable diapers.
It is additionally an object of the present invention to provide an apparatus which dispenses the disposable diapers in a facilitated manner and which is yet capable of accommodating any one of a number of various size diapers equally as well.
These and other objects of the invention will become apparent in light of the present specification.
SUMMARY OF THE INVENTION
The present invention is an improved container and dispensing apparatus for effectively storing and dispensing disposable diapers of various sizes. The apparatus comprises: container means, having a top and bottom portion, a front and back portion, and at least two sides respectively adjacent to the front and back, and top and bottom portions to describe a cavity into which the disposable diapers may be stacked and constrained. Slot release means are interposed between the bottom portion and either the sides, or the front or back portions, in order to enable removal of the disposable diapers one at a time from the cavity portion. Means are provided for adjusting the interior dimension of the cavity portion within the container for effectively accommodating and maintaining the disposable diapers of varying size in place in a neatly stacked position for facilitated dispensation from within the cavity portion. Means are also provided for ascertaining the number of non-dispensed disposable diapers remaining within the cavity portion of the container.
As discussed earlier, disposable diapers come in any one of a variety of sizes depending upon the size and age of the infant, or for that matter, depending upon whether the diaper will be used at night while the infant is sleeping, or during the day when more changes of diapers are necessary.
The preferred embodiment of the invention includes apparatus attachment means for securely fastening the disposable diaper-dispensing apparatus to a wall, to a chest of drawers, to a table top, and the like in order to effectively restrain the apparatus as the disposable diapers are dispensed by the user. Such attachment means could comprise a series of wall clamps affixed to the apparatus proximate to the back portion of the container in order to juxtapose the back portion of the apparatus to the wall, chest of drawers, or the table.
The preferred embodiment of the invention further includes the incorporation of release means for facilitating the release and dispensation of the diaper from the apparatus. This release means, preferably, comprises a plurality of rollers proximate to the bottom portion of the container in which the rollers are arranged substantially along a single plane to assist the conveyance of the diaper atop the plane and proximate to the bottom portion, towards and through the slot release means. In this embodiment, one or more of the roller means utilizes a plurality of scored indentations about its respective circumference to accommodate the adjustable attachment of means for adjusting the interior dimension of the cavity portion within the container. The adjustment means are operably attached to the roller means through a plurality of V-shaped adjustment clamps, wherein each of these adjustment clamps comprises a springedly formed strap having a roller aperture therethrough and a pair of free ends.
Each of these V-shaped adjustment straps is capable of alternatively sliding along the roller means when the free ends of the strap are pinched inwardly towards one another and of crimping the roller means at one of the scored identations, so as to be restrained at a desired location along the roller means while allowing rotation of the roller means.
In one embodiment of the invention the means for adjusting the interior dimension of the cavity portions within the container comprises a spacing object which is insertable into the cavity portion between the stack of disposable diapers and one or more of the sides or the back portion to abut the disposable diapers. This spacing object in turn, maintains the diapers in a constrained position proximate to the other side and proximate to the slot release means for facilitated dispensing from the cavity portion. Preferably, the spacing object would take the more appealing shape of a toy so as to be unobtrusive in the apparatus and in turn within an infant's room.
In another embodiment of the invention, the means for adjusting the interior dimension of the cavity portion comprises an adjustable side member interposed between the sides in a plane substantially parallel to the two or more sides. This adjustable side member is adjustable to alternatively increase or reduce the interior cavity portion between the sides and to describe a dimension into which the sides of the disposable diapers will be constrained in place for dispensation, and to in turn maintain the diapers neatly in a stacked configuration proximate to the slot release means. The adjustable side member has means for facilitated adjustment which are capable of maintaining the side member rigidly at a desired position between the sides after the position of the adjustable side member is adjusted.
And yet another embodiment of the invention, the means for adjusting the interior dimension of the cavity portion comprises adjustable back member means in a position between the front and back portions and in a plane substantially parallel to the front and back portions. The adjustable back member is adjustable to alternatively increase or reduce the interior cavity portion between the front and back portion to describe a dimension into which the front and back of the disposable diapers will be constrained in place for dispensation and to maintain the diapers neatly in place in a stacked configuration. As with the adjustable side members, the adjustable back members have means for facilitated adjustment which are capable of maintaining the back member rigidly at a desired position between the front and back portions after the position of the back member is adjusted.
The preferred embodiment of the invention further includes fabrication of the apparatus with the front, back, and sides comprising a plurality of bar members in parallel arrangement respectively. One or more of the sides utilize rail means for adjustable attachment of the adjustment means for adjusting the interior dimension of the cavity portion. The plurality of bar members forming the front, back, and side members are capable of exposing the interior cavity portion of the apparatus as well as the disposable diapers contained therein to a user thereby enabling the user to ascertain the number of non-dispensed disposable diapers remaining within the cavity portion of the container.
Further, the plurality of bar members provides the ability to the apparatus of being easily decorated or disguised as a toy, such as a circus wagon as shown in the drawings for unobtrusive utilization in an infants room.
The means for adjusting the interior dimension of the cavity portion are attached to, and cooperate with, the rail means through a plurality of V-shaped adjustment clamps similar to those described for utilization with the roller means proximate the bottom portion of the apparatus container. Each of the adjustment clamps comprises a springedly formed V-shaped strap having a rail aperture therethrough, and a pair of free ends. Each of the V-shaped adjustment straps is capable of sliding about the rail means when the free ends of the strap are pinched inwardly or is capable of rigidly crimping the rail means when the free ends are released, to exert spring tension about the rail means to thereby alternatively enable movement of the back portion or securely restrained positioning of the back portion as desired. In a like manner, it should be realized that the dimensions of the slot release means may be made adjustable to accommodate various thicknesses of the diapers depending upon the various type of disposable diaper contained within the apparatus, while limiting the number of diapers capable of withdrawal from the cavity portion during a single dispensation.
In yet another embodiment of the invention also, the means for ascertaining the number of non-dispensed disposable diapers comprises the utilization of a slotted opening in one or more of the front and back portion and/or side portions through which an amount of the contained diapers may be viewed by a user. Through such a slot type opening, the top portion of the apparatus may be enclosed to reduce contamination of the diapers contained within the apparatus. Alternatively, the top portion of the apparatus may be opened to provide facilitated access to the interior cavity portion and to similarly provide means for ascertaining the number of non-dispensed disposable diapers remaining within the apparatus.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 of the drawings is a side perspective view of one embodiment of the disposable diaper dispensing apparatus, showing placement and positioning of the stacked diapers within the cavity portion of same;
FIG. 2 is a side perspective view of a preferred embodiment of the invention, particularly illustrating the various means for adjusting the dimensions of the cavity portion;
FIG. 3 is a top plan view of the dispensing apparatus and disposable diapers contained therein, as one such diaper is dispensed from the device;
FIG. 4 is a partial cross sectional view taken along lines 4--4 of FIG. 3 and looking in the direction of the arrows, illustrating, in detail, the construction of the apparatus including the adjustable side member;
FIG. 5 is an enlarged view of the adjustable clamp means utilized with rails or rollers in order to adjust the dimensions of the interior cavity portion;
FIG. 6 is an enlarged side perspective view of the rollers utilized on the bottom portion of the apparatus; and
FIG. 7 is an enlarged side perspective view of the attachment means utilized in combination with the apparatus for attaching the dispenser to a wall and the like.
DETAILED DESCRIPTION
While this invention is susceptible of embodiment in many different forms, there is shown in the drawings and will herein be described in detail, several specific embodiments, with the understanding that the present disclosure is to be considered as an exemplification of the principles of the invention and is not intended to limit the invention to the embodiments illustrated.
Disposable-diaper dispensing apparatus 10, is shown in FIG. 1, in its simplest embodiment wherein front portion 15 meets side 17 and bottom portion 14. Between front portion 15 and bottom portion 14 are slot entry means 25 through which disposable diapers such as diaper 11 may be dispensed one at a time with front portion 15 maintaining the remaining stack of diapers in place within the dispenser for future dispensation. In this particular embodiment, top portion 18 is open and the front and rear portions, bottom portion, and sides are constructed in a configuration of bars to permit viewing of the interior so as to ascertain the number of remaining disposable diapers for refilling.
When the stack of remaining diapers 12 is depleted to a certain extent, additional disposable diapers may be placed into the container for subsequent use. Through such a fabrication in which bars are utilized, it should be readily apparent that the device may be camouflaged and its design enhanced through the addition of members which convert the dispenser into a toy for unobtrusive installation and utilization in an infants room. Spacing object 16 is utilized to maintain stacked diapers 12 in a neatly stacked configuration within the cavity portion of the container and may be placed, as shown, between one of the sides and the sides of the stacked diapers, and/or may be placed between the back portion and the back side of the diapers to further exert a force against the diapers so as to maintain them in close proximity to the slot release means 25.
In the preferred embodiment spacing object 16 is shaped into a toylike object or plaything so as to be as unobtrusive as the container apparatus itself.
Another preferred embodiment of the invention is shown in FIG. 2 in which dispensing apparatus 20 is formed by sides 53 and 54, front portion 98, bottom portion 50, back portion 21 and a top portion which, in this case has been left substantially opened. Slot release means 25 is formed between the position of front portion 98 and bottom portion 50. The slot release means are further interposed between the front portion and the sides of the apparatus. Further, bottom portion 50, in this embodiment, utilizes a plurality of rollers such as rollers 27, 28, 29, and 55 for the purposes of facilitating the dispensing of disposable diapers from within the cavity portion of the apparatus.
Apparatus brackets 31 through 34 are utilized for securely fastening the dispensing apparatus 20 to a wall or other equivalent plane. Placement of the attachment means could be made on the bottom of bottom side 50 for equivalent attachment to a horizontal planer surface. Rails 22, 46, 30 and 47 are affixed to sides 53 and 54 to provide adjustable attachment of back member 21 forming the back portion of the device to snuggly constrain the edges of the disposable diapers maintained within the container for facilitated dispensing thereof.
Members 36 and 43, and 35 and 44 on side 53 provide for the attachment of rails 22 and 46 respectively, and members 40 and 48, and 45 and 51 on side 54 provide means for the attachment of rails 47 and 30 on side 54. Through such an arrangement, back member 21 can slide towards and away from front portion 98 through the utilization of the V-shaped clamping apparatus 23, 37, 41, and 42. Means are also provided, in this preferred embodiment, for adjusting the dimension of the container cavity between sides 53 and 54. Adjustable side member 39 is connected by member 38 to enable sliding to any one of a number of positions along rollers 28, 29, and 99. Each of these rollers for example, utilizes a series of notches such as notch 94 in roller 28 and notch 93 in roller 99, into which a V-shaped adjustment clamp rides to restrain the longitudinal position of adjustable side member 39 while allowing the rotation of the rollers for facilitated dispensing of the disposable diaper. These V-shaped clamps for utilization with the adjustable side member are shown in FIG. 3 by reference numerals 62 and 63 proximate to notches such as notch 90. Optional cover member 100 is also shown.
A top plan view of the dispensing apparatus 20 is shown in FIG. 3 as having V-shaped clamps 23 and 41 sliding on rails 22 and 47 respectively. The edge views of sides 53 and 54 are shown as is the edge view of backside 21 which, in this embodiment comprises the adjustable back member.
Facilitated release means comprising rollers 27, 28, 29, and 55 facilitate the dispensing of diaper 61 as it is dispensed in the direction of the arrow. Depending upon the size of the slot release means and thus the dimension of front portion 49, a remaining stack of diapers 60 is maintained within the cavity portion of the container for subsequent dispensing. It should be noted that the stack of diapers themselves or the box containing the diapers as packaged by the manufacturer may alternatively be maintained within the cavity position for dispensing of the diapers. As is readily apparent, adjustable side member 39 together with adjustable back member 21 closely constrains the plurality of stacked diapers 60 into a desired area of the container 20 and maintains them proximate to the slot release means for neat and facilitate dispensing.
Member 38 of adjustable side member 39 is shown in greater detail in FIG. 4 saddling several of the rollers such as roller 28, to enable adjustable side member 39 to closely and securely maintain diapers 60 in a stacked configuration together with adjustable back member 21. As also shown in FIG 4, while V-shaped members 23 and 37 can be attached directly to adjustable rear member 21 to maintain it in place, portions of adjustable member 21 can be interposed between the two extending sides of clamps 23 and 37 to maintain adjustable member 21 between the confines of the interior portion of the V-shaped clamps with virtually identical results. Through such an arrangement, pinching of the clamps would permit movement of the back member 21 along rails 22 and 46.
An enlarged view of the adjustable V-shaped clamp 23 is shown in FIG. 5 in which clamp 23 is in position about rail 22. Pinching the ends of clamp 23 together enables sliding to occur with respect to rail 22, to in turn provide the adjustment feature discussed regarding, for example, the adjustable back member. An equivalent manner of operation is involved with the utilization of similar V-shaped clamps about rollers. In such an operation, wherein the adjustable side member would be adjusted, the V-shaped clamp would settle into one of several provided notches such as notches 91 or 95 shown in dashed lines on rail 22, for the express purpose of maintaining the longitudinal position of V-shaped clamp 23 while permitting rotation of the roller within the aperatures of the clamp itself.
Notch 92 in roller 29 of FIG. 6, more clearly shows utilization of the notches in combination with the roller means for the aforementioned co-operation with the V-shaped clamp. Bar member 74 communicates with rollers 27 through 29 through the utilization of axle members 73, 72, and 71 respectively.
In FIG. 7, a portion of side 47 is shown having attached thereto brackets 31-34 for subsequent and facilitated attachment of the dispensing apparatus to a wall or equivalent structure.
The foregoing description and drawings merely explain and illustrate the invention and the invention is not limited thereto, except insofar as the appended claims are so limited, as those skilled in the art who have the disclosure before them will be able to make modifications and variations therein without departing from the scope of the invention. | An improved container and dispensing apparatus for effectively storing and dispensing disposable diapers. The apparatus is formed by a container having a slot release portion as well as adjustment devices for altering its interior dimension to accommodate various sizes of disposable diapers. The apparatus is constructed to enable the user to quickly and easily ascertain the level of diapers within it and may be easily decorated as a toy for unobtrusive incorporation into and utilization in an infant's room. | 0 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This patent application is a continuation patent application, pursuant to 35 U.S.C. sec. 120, of U.S. patent application Ser. No. 10/941,144 filed Sep. 14, 2004, which claims benefit of U.S. provisional patent application 60/503,513, filed Sep. 15, 2003, entitled A Method and Apparatus to Immobilize an Internal Combustion Engine Motor Vehicle, all of which are incorporated by reference herein in their entirety.
FIELD
[0002] The invention relates generally to stopping a motor vehicle, and more particularly to choking off and stopping an internal combustion engine.
BACKGROUND
[0003] Law enforcement officials must routinely stop motor vehicles by a roadway. As part of a routine procedure and for safety precautions, the motor vehicle operator is often requested to turn off the motor vehicle engine. The law enforcement officer may make such a request for additional reasons including suspicion that the vehicle operator may flee. In some cases, the vehicle operator does flee.
[0004] Additionally, law enforcement officials are often called on to forcibly stop a fleeing vehicle. High speed pursuit by law enforcement frequently results in personal injury and property damage. Often, law enforcement officers will pursue motor vehicle suspects for a considerable amount of time while subjecting the suspects, officers and bystanders to potential risk of injury and property damage during high speed pursuits. It is of interest that occupants of a fleeing vehicle, which may include hostages, not be injured by immobilization of the vehicle.
[0005] Known vehicle immobilization systems exhibit shortcomings and dangers to those involved in a vehicle chase and to innocent bystanders. One known method is to force the fleeing vehicle to stop by driving the pursuing vehicle to the side or in front of the fleeing vehicle, or to push the fleeing vehicle from a back corner so that the fleeing driver looses control of the vehicle. Other known methods of stopping fleeing vehicles include tire spikes and eventual fuel depletion. Tire spikes may lead to additional property damage by an uncontrollable vehicle. Fuel depletion often requires a lengthy hot pursuit during which persons and property are subject to possible injury and damage. Another known technique includes engaging a metal structure on the fleeing vehicle and force stopping the fleeing vehicle, which presents a difficult maneuver given a moving and evasive vehicle. Further, road blocks are not easily deployed or positioned and a fleeing vehicle may simply reroute to an alternate path around a road block.
[0006] A need for detaining or immobilizing motor vehicles also applies to other settings including border settings, military settings and water settings with boating vehicles. A need exists for a transportable, rapidly deployed, vehicle immobilization device that does not encompass the shortcomings and dangers of the prior art.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] The foregoing aspects and many of the attendant advantages of this invention will become more readily appreciated by reference to the following detailed description, when taken in conjunction with the accompanying drawings, wherein:
[0008] FIG. 1 is a side view of a conical plug having a handle, in an embodiment of the present invention;
[0009] FIG. 2 is a side view of a rectangular plug having an extension and handle, in an embodiment of the present invention;
[0010] FIG. 3 is a side view of a conical plug having an extension and handle, in an embodiment of the present invention;
[0011] FIG. 4 is a side view illustration of insertion of a plug by a human into an exhaust pipe of a motor vehicle, in an embodiment of the present invention;
[0012] FIG. 5 is a side view illustration of a plug having been inserted into an exhaust pipe of a motor vehicle, in an embodiment of the present invention;
[0013] FIG. 6 is a side view illustration of a plug block mounted to the front end of a law enforcement vehicle, in an embodiment of the present invention;
[0014] FIG. 7 is a front view illustration of a plug block mounted to the front end of a law enforcement vehicle, in an embodiment of the present invention; and
[0015] FIG. 8 is a side view illustration of a law enforcement vehicle having a plug block mounted to the front end forcing plug material into an exhaust pipe of a fleeing vehicle, in an embodiment of the present invention.
DETAILED DESCRIPTION
[0016] Exemplary embodiments are described with reference to specific configurations. Those of ordinary skill in the art will appreciate that various changes and modifications can be made while remaining within the scope of the appended claims. Additionally, well-known elements, devices, components, methods and the like may not be set forth in detail in order to avoid obscuring the invention.
[0017] A method and apparatus of choking off and stopping an internal combustion engine is described herein. It will be apparent that features of the discussion and claims may be utilized with a motor vehicles including, a car, a truck, a boat, military vehicles, as well as other motor vehicles. In an embodiment, the present invention may be used to detain a stationary vehicle so that the engine shuts down and cannot be restarted until the device is removed. In another embodiment, the present invention may be used to stop a fleeing vehicle. In an embodiment, the present invention may be employed by law enforcement and at geographical borders of countries, or vehicle inspection checkpoints.
[0018] Referring to the drawings wherein identical reference numerals denote the same elements throughout the various views, FIG. 1 illustrates stationary detainment device 100 in an embodiment of the present invention. Stationary detainment device 100 includes conical plug 102 having a handle 104 . Conical plug 102 is shaped such that a first end is smaller in diameter than a second end, to fit with a variety of sizes or diameters of internal combustion engine exhaust pipes. As the plug enters an exhaust pipe, it reaches a position wherein it fits tight with and seals the exhaust pipe. Handle 104 is provided for a human hand to have a solid grasping place for facilitating insertion (and extraction) of the plug 102 , and can be twisted to further obtain a tight fit within an exhaust pipe. Additionally, in an embodiment, plug 102 is comprised of a material (as discussed below) that expands upon heating, to further obtain a tight fit with the inside surface of an exhaust pipe. In an embodiment, plug 102 is formed of an adhesive material that adheres to a metal exhaust pipe.
[0019] The material selected for plug 102 is nonflammable when exposed to temperatures of hot exhaust fumes that are expelled from exhaust pipes. For better sealing results, plug 102 is comprised of a material that remains intact or does not substantially melt when being subjected to exhaust temperatures. It is to be appreciated that only a partial seal by plug 102 with an exhaust pipe can choke off and stop an internal combustion engine due to partial blockage. Therefore, while plug 102 might partially seal an exhaust pipe, the engine can in some cases nevertheless be stopped. Additionally, in an embodiment, plug 102 is comprised of a material that can be inserted into and exhaust pipe and pulled from or completely retracted from an exhaust pipe without leaving any remaining material in the exhaust pipe. Further, the plug 102 is to be of a material that is not easily blown or expelled from an exhaust pipe by exiting exhaust fumes.
[0020] Various materials can be used for plug 102 . In an embodiment, the material is a sticky, tacky, gluey and metal adhesive substance. Alternatively, a sticky foam may be used. Further alternative materials that can be used for plug 102 include a caulk, putty, paste, plaster, bond, epoxy, adhesive, binder, sealant, glue, cement, gum, plaster, resin, motor, wax and tar.
[0021] In an embodiment, plug 102 is comprised of a metal adhesive. Metal adhesives include acrylic, polyurethane, PU, Polysufide, PSR, Anaerobic, Epoxy, EP, and cyanoacrylate. The bonding of an adhesive to an exhaust pipe is a result of mechanical, physical and chemical forces. One force, mechanical interlocking, is caused by mechanical anchoring of adhesive in the pores, holes, crevices and other irregularities of the exhaust pipe surface. Another force, electrostatic forces, is caused by differences in electronegatives of adhering materials, and other adhesion mechanisms dealing with intermolecular and chemical bonding forces that occur at interfaces. For example, when an organic polymer contacts metal, electrons are transferred from the metal into the polymer, creating an attracting electrical double layer. The electrostatic forces at the interface account for resistance to separation of the adhesive and the substrate.
[0022] An internal combustion engine may be stopped by sealing an exhaust pipe since the engine is choked off. In order for the engine to run, a fresh mixture of gasoline (fuel vapor) and air must be introduced into the combustion chamber. However, the fresh mixture cannot be injected or be effective unless the spent, burned-up fumes and exhaust is expelled. Further, back pressure in the engine prevents the engine from restarting.
[0023] It is to be appreciated that conical plug 102 having handle 104 provides an easily transportable and rapidly deployed device for emergency use. The conical plug 102 and handle 104 may further be carried by law enforcement officers on foot, attached to a person's belt.
[0024] FIG. 2 is a side view of a rectangular plug 202 having an extension 206 and handle 204 , in an embodiment of the present invention. Rectangular plug 202 is an alternative shape to conical plug 102 . Extension 206 is provided for additional reach by a human to an exhaust pipe and can be used to seat plug 202 further into an exhaust pipe.
[0025] FIG. 3 shows is a side view of conical plug 102 having an extension 306 and handle 104 in a further embodiment of the present invention. Extension 306 can be sized as a desired length.
[0026] FIG. 4 is a side view illustration of insertion of plug 306 by a human 420 into an exhaust pipe 408 of a motor vehicle 402 . This method may be utilized by a law enforcement officer to detain a stationary vehicle by stopping the internal combustion engine. As may be observed, extension 306 provides additional reach for insertion of plug 102 into exhaust pipe 408 . Muffler 406 is shown connected to exhaust pipe 408 , positioned at the back end 404 of detained vehicle 402 .
[0027] Further, to the advantage of the law enforcement officer, the operator/driver of vehicle 402 would not have a clear view (or any view) of the actions by a law enforcement officer inserting plug 102 into exhaust pipe 408 , and the engine may quit before the vehicle operator realizes what has occurred.
[0028] FIG. 5 shows a side view illustration of a plug having been inserted into an exhaust pipe of a motor vehicle. It is to be observed that plug 502 extends into exhaust pipe 408 and, in an embodiment, is compressed and also expands in any internal exhaust pipe surface irregularities forming a tight seal, while plug end 504 expands around an outer edge of exhaust pipe 408 . Extension 506 and handle 508 provide additional reach to exhaust pipe 408 , and a twisting/tightening means for a human. Plug 502 could be extracted from exhaust pipe 408 when desired by pulling on handle 508 .
[0029] FIG. 6 shows a side view illustration of a plug block 602 mounted to the front end 606 of a law enforcement vehicle 604 , in an embodiment of the present invention. Attachment 610 provides an attachment means for attaching plug block 602 to front end 606 . Plug block 602 is positioned clear and safely away from air intake/radiator or tires 620 of law enforcement vehicle 604 . In an embodiment, plug block 602 is shaped having an angled and extended end 616 for directed impact and insertion into an exhaust pipe of a fleeing vehicle.
[0030] FIG. 7 shows a front view illustration of plug block 602 mounted to the front end 606 of a law enforcement vehicle 604 , in an embodiment of the present invention. It will be observed that, in an embodiment, plug block 602 extends across the entire width of law enforcement vehicle 604 . The height and width of plug block 602 can be designed as desired, but should not obstruct the law enforcement vehicle 604 driver/operator view. It is to be appreciated that plug block 602 can take on other shapes, dimensions and position orientations other than that as shown in FIG. 7 .
[0031] FIG. 8 shows a side view illustration of a law enforcement vehicle 820 having a plug block 602 mounted to the front end 606 , forcing material 816 into an exhaust pipe 812 of a fleeing vehicle 810 . The front end 606 of law enforcement vehicle 820 is driven into the back end 818 of the fleeing vehicle 810 , wherein a portion of the plug block 602 is forced into exhaust pipe 812 of fleeing vehicle 810 . In some cases, the back end 818 of fleeing vehicle 810 will be squared up with law enforcement vehicle 820 , and in other cases the back end 818 of fleeing vehicle 810 will not be squared up with law enforcement vehicle 820 . However, plug block 602 can in many cases nevertheless be forced into exhaust pipe 812 . Once the plug block 602 is forced into exhaust pipe 812 of the fleeing vehicle 810 , a portion of the plug block 602 can break off or separate from the portion attached to law enforcement vehicle 820 . It is to be appreciated that the material utilized for plug block 602 can be similar or the same as that utilized for plug 102 ( FIG. 1 ). However, the material utilized for plug block 602 (and inserted in an exhaust pipe) should readily break or separate from the portion attached to law enforcement vehicle 820 . This way, it is unnecessary for law enforcement vehicle 820 to maintain contact or a close proximity to fleeing vehicle 810 . Once some portion of plug block 602 is forced into and sufficiently seals exhaust pipe 812 , the fleeing vehicle will either slow or stop, since the exhaust of the internal combustion engine will be obstructed. Loss of control of fleeing vehicle 810 is therefore avoided since forcing the vehicle into an out-of-control spin is avoided. Should the fleeing driver attempt to restart the vehicle, attempts would be futile in virtually all or all cases. A non-lethal method and device is therefore provided by the present invention to stop a fleeing vehicle and driver. Further, it is to be appreciated that plug block 602 provides an easily transportable and rapidly attachable and deployed device for emergency use.
[0032] Other features and advantages of this invention will be apparent to a person of skill in the art who studies this disclosure. For example, the plug 102 ( FIG. 1 ) may be further employed in a situation wherein vehicle door and ignition keys are locked within a vehicle and it is desired that the vehicle be shut down. Thus, exemplary embodiments, modifications and variations may be made to the disclosed embodiments while remaining within the spirit and scope of the invention as defined by the appended claims. | A readily transportable and rapidly deployable vehicle immobilization device is provided. The exhaust of an internal combustion engine is obstructed, resulting in choking off and stopping of the engine. In an aspect, a plug is provided having an extension fixed to the plug for human grasping, and facilitating insertion into an end of a vehicle exhaust pipe. In an aspect the plug expands upon being heated and is adhesive to the exhaust pipe for at least partially sealing the exhaust pipe. In another aspect, a length of adhesive material is attached to the front of a pursuing vehicle and engages an end of an exhaust pipe of a fleeing vehicle. | 8 |
BACKGROUND OF THE INVENTION
[0001] 1. The Field of the Invention
[0002] The invention relates to the field of personal computer manufacturing, and more particularly to the ability to securely modify system attributes of a pre-configured computing device that has already completed the manufacturing process.
[0003] 2. Background of the Art
[0004] Nearly every modern personal computer system is sold with Basic Input Output System (BIOS) code, but only recently have manufacturers of BIOS code provided mechanisms for enabling users of personal computers and manufacturers of personal computers to access BIOS code. BIOS is an embedded code storage application of the personal computer, and more particularly is a low level code interfacing the operating system to the specific hardware implementation. BIOS is typically stored in a flash Electrically-Erasable-Programmable-Read-Only-Memory (EEPROM) that in turn is mounted on the main system board of the personal computer. The BIOS of a main system board is often software stored on an EEPROM chip which helps the main system board to function correctly and communicate with devices on the board surfaces and also secondary devices and software protocols that are attached to or running on the main system board respectively.
[0005] Typical functions of the BIOS code include the initialization of disk drives (including floppy, hard, and compact), setting control registers settings and the initialization of the video and graphical interfaces. The BIOS is specifically configured for each PC based on the presence of specific hardware and the current version or manufacturer of the hardware to take advantage of all or select BIOS functions. Often, when the hardware of the personal computer is updated or modified, the BIOS code may need to be upgraded to properly recognize and initialize the new hardware. Typically, an updated BIOS can be flashed to the Flash Read-Only Memory (ROM), after additional components of the PC have been replaced or upgraded.
[0006] Additionally, it is known that the Flash ROM memory array may be divided into two distinct sections, the boot block and the main block. The main block of the Flash ROM contains applications, such as those presented above, which are hereinafter referred to as the“main data applications.” The boot block of the Flash ROM is however protected from an ordinary flash, such that the data remaining in the boot block portion is present even after a corrupted Flash ROM image is flashed.
[0007] During the manufacturing process of personal computers, particularly of large volume orders, it is often typical for each ordered personal computer within a large order to be required to contain certain hardware capability, specific select software programs, and to be configured in a particular manner, per the order. In essence, a system is manufactured based upon a suite of features and capabilities (i.e., system attributes) for a specific customer or user. It is also quite common in these types of orders to include as a result of manufacture standardized or stock feature cards and/or chips that have functional capabilities beyond those functions or features initially ordered. Though the inclusion of such additional capabilities and functionality may appear to be more expensive, due to the quantity of stock product, the economics often favorably support such a manufacturing decision. This economic trade is becoming better understood in the industry, and is becoming a decision point that is resulting in manufacturers including a common set of features and equipment in most assembled products; this common set of equipment/functionality offering is also known as the manufacturer's “common building block.”
[0008] However, for a variety of reasons, including specific customer requirements, it is often necessary to de-function or limit the capabilities of the additionally included functionality that is present on these cards and chips. Ensuring that this de-functioning result is maintained (such that the scope of system attributes as defined as of the time manufacture versus the broad capability available as a result of that present), and that such de-functioning survives post-manufacture is also an important issue as otherwise it may be possible for a user to order a “reduced-function” system at a reduced cost and perform unauthorized post-manufacturing modifications to illegally upgrade and sell a “full-function” system that does not meet the standards of the labeled manufacturer of the system. Similarly, there also may exist a situation where one or more manufactured system needs to be modified or upgraded (e.g., a customer has cancelled orders or there exists an oversupply of stock of a manufactured line in-house) such that further functionality of system attributes of those systems need to be either increased or decreased in functioning scope. Since manufacturing of systems often occurs at locations separate from order facilities and by vendors who are contracted to manufacture, ensuring that end products produced are commensurate with the prescribed system attributes assigned at the time of manufacture is important but is clearly difficult to track.
[0009] Fixing a set of system attributes for a system at a particular time or stage of manufacture is however possible using the boot block. For instance, when a system has completed the manufacturing stage (i.e., the system has not yet been shipped to the customer but has been built to a prescribed level of manufacture), it is possible to concurrently set a bit (e.g., MFG_DONE) within the boot block of the system in the manufacturing environment to indicate that the system is complete (or at a particular stage) and that no further system attribute changes or modifications are to take place. In other words, the system has a fixed set of system attributes. Although the MFG_DONE bit is identified herein by example, other one-way bits located in the boot block are also envisioned by the present invention, and the invention is not so limited to the examples set forth.
[0010] The MFG_DONE bit is a bit that may be set by the manufacturer at the time of completion of the system (or at a predetermined stage of manufacture), and the setting of the bit prevents further modification to the set of system attributes of that particular system outside of the manufacturing environment. This bit setting approach in the manufacturing environment is an approach that is well-aligned with requirements set forth by the Trusted Computer Platform Alliance (TCPA) requiring that a manufacturer establish a Core Root of Trust for Measurement (CRTM) that is to be controlled by manufacturing. One of the goals of the TCPA is to maintain the privacy of the platform owner while providing a ubiquitous interoperable mechanism to validate the identity and integrity of a computing platform. However, since the MFG_DONE bit is set in the manufacturing environment, in the event the finished system is recalled, withdrawn, identified as overstock to be modified, selected for re-introduction, or the like, or when there is an express order to alter its functionality, the system attributes of that system cannot be easily changed since the MFG_DONE bit is set to indicate that the system is“outside of the manufacturing environment.” Similarly, there may exist the situation where a large volume system user orders an upgrade of the functions and features of numerous systems that were originally ordered as“low-function” to“full-function” and are presently in operation at the client site, which is physically remote from the manufacturing environment.
[0011] As used herein the terms“BIOS”,“BIOS code”,“BIOS image files” and“system BIOS” are used interchangeably and are intended to have similar meanings and uses in relation to functions and characteristics associated with BIOS. As used herein the terms“personal computer,” “computer,” “PC,” “system,” “computing device,” and“server,” are used interchangeably and are intended to have similar meanings and uses in relation to functions and characteristics associated with electronic information handling systems.
SUMMARY OF THE INVENTION
[0012] Therefore, what is needed is a method that allows for secure and limited access to a completed system so as to modify the system attributes of the completed system as though the system were in the manufacturing environment by accessing the identifying bit of the boot block to allow system attributes to be modified, even when the system is physically outside of or has already left the manufacturing environment.
[0013] One embodiment of the present invention is directed to a method for securably updating one or more system attributes of a client computer having a BIOS, comprising the steps of signing a public key of a secure server with a private key of the BIOS of the client computer prior to manufacturing completion of the client computer. Once signed, an encrypted public key and an embedded private key is created and stored at said server. When the system attributes of a completed system are to be modified, the client computer transmits a transmitted request packet requesting system attribute modification to the server, and the server upon receipt of the packet, encrypts the received request packet at with the server's private key to create an encrypted packet. The server then may transmit a return packet to the requesting client computer wherein the return packet comprises the encrypted packet, the server's public key, and the server instructions regarding a command sequence to update the system attributes. The client computer receives the return packet and decrypts the server's public key and compares the return packet with the request packet originally transmitted for equivalency. If the two packets are equivalent, the client computer executes the transmitted server instructions at the client computer so as to modify the client computer's boot block and thereby update the client computer's system attributes.
[0014] In another embodiment, the present invention is directed to a secure method for remotely updating one or more system attributes of one or more client computers from a client computer site, comprising the steps of signing a public key of a secure server with a private key of the BIOS of the one or more client computers prior to manufacturing completion of the one or more client computers. Once at the client site, a single client computer of the one or more client computers is identified to facilitate initial and terminal communication between the manufacturing server and the one or more client computers. The identified single client computer initiates a secure communication session between the manufacturing server and the single client computer. The manufacturing server receives the transmitted request packet from the one or more client computers requesting a specific system attribute modification for each of the one or more client computers, respectively. Each received request packet at the secure server is encrypted with a server private key to create an encrypted packet for each of the one or more client computers, respectively. A unique return packet is then transmitted to each of the one or more client computers, respectively, such that the unique return packet comprises the encrypted packet, the server public key, and the server instructions. Preferably, the server instructions include commands related to system attribute modifications for the specific client computer. At each of the one or more client computers, respectively, the server public key is decrypted and the unique return packet and the transmitted request packet are compared for equivalency. If equivalent, the server instructions are executed so as to modify each of the one or more client computers' boot block to update each of the one or more client computers' system attributes. Once all client computers to be modified have communicated with the manufacturing server, the session is terminated between the manufacturing server and the single client computer.
[0015] In a further embodiment, the present invention is directed to a method for a retail environment having one or more client computers to securably update the one or more client computers to reflect current customer system configuration interests.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Other aspects, features, and advantages of the present invention will become more fully apparent from the following detailed description, the appended claims, and the accompanying drawings in which:
[0017] [0017]FIG. 1 is a diagram of a secure manufacturing server and a secure client in a preferred embodiment of the present invention.
[0018] [0018]FIG. 2 is a diagram of a secure client operation in a preferred embodiment of the present invention.
[0019] [0019]FIG. 3 is a block diagram of a secure manufacturing server operation in a preferred embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0020] The use of figure reference labels in the claims is intended to identify one or more possible embodiments of the claimed subject matter in order to facilitate the interpretation of the claims. Such labeling is not to be construed as necessarily limiting the scope of those claims to the embodiments shown in the corresponding figures. The preferred embodiments of the present invention and its advantages are best understood by referring to the drawings, like numerals being used for like and corresponding parts of the various drawings.
[0021] [0021]FIG. 1 is a diagram of a secure manufacturing server and a secure client in a preferred embodiment of the present invention. From FIG. 1, the secure manufacturing server ( 100 ) is shown in communication via a communication link ( 105 ) with a client computer ( 110 ). For exemplary purposes, as will be evident in the discussion following, FIG. 1 is demonstrative in depicting the presence of the embedded server private key ( 120 ), the server public key encrypted with BIOS private key ( 125 ) and the client's embedded BIOS public key ( 130 ). From FIG. 1 it is possible to better understand the communications between a manufacturing server ( 100 ) and one or more client computers ( 110 ) according to preferred embodiments of the present invention.
[0022] In a preferred embodiment of the present invention, the manufacture's public key of the manufacturer's server (Manufacture Sever Public Key) is encrypted with the manufactured computer's BIOS private key (Client BIOS Private Key). The secure manufacturing server will store the resulting encryption ( 125 ). Upon the event when one or more client computers ( 110 ) requests a modification to their respective system attributes, the client computer issues a request packet ( 140 ) to the secure manufacturing server. By example, the request packet issued may be a secure random number generated or the like, and is preferably a NONCE. As used herein, the term NONCE, is a parameter that varies with time, such as a time stamp, a special marker, or a unique random number specific to the message generated, for instance.
[0023] Once received at the secure manufacturing server ( 100 ), the request packet is encrypted at the secure manufacturing server ( 100 ) using the embedded server private key ( 120 ). The secure manufacturing server ( 100 ) then transmits the encrypted request packet ( 150 ) along with the resulting encryption (Server Public Key Encrypted with BIOS Private Key ( 125 )) at 126 to the client computer initiating the request ( 110 ). Preferably the encrypted request packet also comprises server instructions for execution upon decryption related to system attribute modifications of the client computer ( 110 ).
[0024] Upon receipt of 150 and 126 , the client computer ( 110 ) decrypts the Server Public Key Encrypted with BIOS Private Key portion with the embedded BIOS Public Key ( 130 ), and stores the decrypted Server Public Key portion of 126 locally at the client computer ( 110 ). The client computer ( 110 ) then uses the stored and decrypted Server Public Key portion to decrypt the encrypted request packet ( 150 ) received from the secure manufacturing server ( 100 ). Once decrypted, the client computer ( 110 ) compares the NONCE, or similar, to determine if the received encrypted request packet ( 150 ) is an authentic request packet.
[0025] Upon favorable comparison, such that the client computer ( 110 ) determines that the received encrypted request packet ( 150 ) is an authentic request packet, the server instructions, if any, are executed and a sequence to initiate system attribute modification for the client computer ( 110 ) is initiated.
[0026] [0026]FIG. 2 is a diagram of a secure client operation in a preferred embodiment of the present invention. From FIG. 2 it is possible to better understand the communications from and activities of the client computer according to a preferred embodiment of the present invention.
[0027] In a preferred embodiment of the present invention, a client computer ( 205 ) is identified as being in the manufacturing process. An assessment is performed at the client computer ( 205 ) to determine the status of a predetermined boot block bit, such as MFG_DONE, at 210 . If the predetermined boot block bit is set to indicate that the manufacturing is complete ( 215 ), the system attributes are then evaluated to determine if the attributes are locked or unlocked, at 220 . If the predetermined boot block bit is set to indicate that the manufacturing is not complete ( 225 ), such that the system remains in the manufacturing environment, the system attributes are then evaluated to determine if the attributes are locked or unlocked, at 230 .
[0028] For either event, if the system attributes are determined to be unlocked, at 235 and 240 , respectively, modifications to the system attributes may continue as the client computer ( 205 ) remains in the manufacturing environment ( 245 ). However, once the client computer ( 205 ) is deemed to be completed, the system is identified as being“ready” for release and the system attributes are locked (i.e., fixed), at a predetermined point in the manufacturing process, by setting the boot bit indicator ( 250 ).
[0029] In the event that the system attributes are determined to be locked, at 255 and 260 , respectively, modifications to the system attributes may not be performed as the client computer ( 205 ) is deemed to be out of the manufacturing environment and is completed. A further event may occur where the identified client computer ( 205 ) is assessed as to its present system attributes ( 265 ). If it is determined that system attributes require modification ( 270 ), the client computer issues request packet ( 275 ) preferably comprising a generated NONCE to be sent to the secure manufacturing server (not pictured). If it is determined that no further modification is needed, the client computer is deemed to be complete.
[0030] Upon the issuance of the request packet by the client computer at 275 , the client waits for a response from the secure manufacturing server at 280 , which is described in detail with regard to FIG. 3. If a response is not received from the secure manufacturing server, the client computer may continue to wait until a system administrator overrides the request or the request is timed out ( 285 ). During the wait, a wait for a response is assessed ( 290 ), and once a response is received from the secure manufacturing server ( 295 ), a decryption event is initiated. Upon receipt of an encrypted response, the client computer assesses whether it is able to decrypt the public key of the secure manufacturing server at 296 . Typically, the response received is a packet from the secure manufacturing server that includes the NONCE, supplements of command information from the server, if any, along with a secure manufacturing server private key. The response received is also preferably encrypted with the secure manufacturing server public key.
[0031] If the client computer is able to successfully decrypt the public key of the secure manufacturing server, the client computer then compares the NONCE of the encrypted request packet with the NONCE issued by the client, at 297 . If the comparison of the NONCEs by the client computer is successful, the client computer executes the commands contained in the received encrypted request file from the secure manufacturing server, at 298 and updates the system attributes. Once updated, if the update is deemed complete at 299 , the client computer is deemed complete at 201 and the system attributes are locked at 250 .
[0032] For the above event, if the client computer is not able to decrypt the public key of the secure manufacturing server or identifies that the NONCEs are not equivalent, the client computer may wait at 276 for another encrypted return packet from the server or the session may be timed out or cancelled. If it is determined at 299 that system attribute modifications are not complete, the client computer may generate a further request at 271 . FIG. 3 is a block diagram of a secure manufacturing server operation in a preferred embodiment of the present invention. From FIG. 3 it is possible to better understand the communications from and activities of the secure manufacturing server according to a preferred embodiment of the present invention.
[0033] In a preferred embodiment of the present invention, a secure manufacturing server ( 300 ) having a server public key of the manufacturer is identified. Using a secure process at 305 , an encrypted signing occurs between the server public key of the manufacturer at the server and the BIOS private key of the client computer at 310 . The secure manufacturing server stores the resulting encrypted public key at 315 . At the secure manufacturing server, the encrypted public key and the embedded private key are identified at 320 . Upon the receipt of a request by a client computer (identified as Client A at 330 ) to modify system attributes, at 325 , the secure manufacturing server verifies that the request packet is authentic at 335 . If the request packet received is not authentic, the server may continue to wait or may send a notice that the packet is void. If the request packet is authenticated, the secure manufacturing server encrypts the NONCE therein and supplements with command information, if any, along with secure manufacturing server public key. The secure manufacturing server then encrypts the return request with secure manufacturing server private key for a return packet sent to client computer at 340 .
[0034] The present invention also has other possibilities such as using the methods for secure access in military applications, manufacturing environments and retail space sectors, without limitation. It is evident that the invention is suitable for use under these and other circumstances, as system attributes may often require updating or modification in a variety of locations and markets, wherever computers exist. It is also evident that the present invention could be implemented in other manners and by other methods.
[0035] It will be further understood that various changes in the details, materials, and arrangements of the parts which have been described and illustrated in order to explain the nature of this invention may be made by those skilled in the art without departing from the principle and scope of the invention as expressed in the following claims. | The disclosed methods enable users to securably modify system attributes of completed computer systems, without requiring that the system be returned to their manufacturer or that the system be “overhauled.” The methods of the present invention permit manufacturing cost savings and efficiencies, while allowing existing built inventory to be modified to meet current market demands without the need to recall built systems back to the origin of manufacture. | 6 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application No. 61/556,732, filed on Nov. 7, 2011, the disclosure of which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
The present invention relates generally to processing timestamps in communication packets and, more particularly, to processing timestamps in communication networks that include media access control security.
It may be advantageous in a networked system for devices in the network to include timestamp information in some communication packets. The timestamp information may be indicative of when a packet is transmitted or received by one of the devices. The timestamp information may be used, for example, to synchronize clocks between devices in the network. The timestamp information may also be used for operation, administration, and maintenance functions in the network. The electronics industry has developed several standard protocols that use timestamped packets, for example, the Precision Time Protocol (PTP) of IEEE Std. 1588 and ITU-T Recommendation Y.1731 on Internet protocol aspects—Operation, administration and maintenance.
It may also be advantageous to secure at least some communication in a network to avoid interception of information or disruption of network operations. Some information may be protected by encrypting the information at its source and decrypting it at its destination. Other information may be protected by inclusion of a check value or digital signature that allows a receiving device to confirm that the information has not been altered since it was sent from a transmitting device. One protocol for increasing network security is Media Access Control (MAC) Security of IEEE Std. 802.1AE.
It may be further advantageous for a network to provide both timestamp information and increased security. However, security measures may interfere with timestamp information by, for example, increasing uncertainty with respect to the timing information, which in many cases should also be subject to the security measures. Reducing effects of security measures on timing information may be difficult, however, particularly without unduly reducing bandwidth of a communication system.
BRIEF SUMMARY OF THE INVENTION
Some aspects of the present invention provide a method performed by a physical layer communication device implemented using electronic circuitry, the method comprising: receiving a packet for transmission; determining whether the packet is a packet that is to receive timestamp processing; if the packet is to receive timestamp processing, determining a value indicative of a time of transmission of the packet to a communication network; if the packet is to receive timestamp processing, delaying the packet for a time interval determined to avoid having the packet incur a variable delay during subsequent processing due to MACsec processing of a prior packet; and transmitting the packet over the communication network.
Another aspect of the invention provides a method performed by a physical layer device (PHY) comprising a transmit chain including a transmitter, a MACsec processing block, a timestamp processing block, and a flow control block, the method comprising: buffering packets for transmission by the flow control block; determining, by the timestamp processing block, whether packets for transmission are packets subject to timestamp processing; providing, by the timestamp processing block, for the packets subject to timestamp processing, an indication of predicted time of transmission of the packet from the PHY; delaying, by the timestamp processing block, provision to the MACsec processing block of packets subject to timestamp processing so as to reduce in accuracy of the predicted time of transmission; performing, by the MACsec processing block, MACsec operations on at least some of the packets; and transmitting, by the transmitter, the packets.
Another aspect of the invention provides a physical layer device, comprising: a transmit chain including a transmit flow control block, a transmit timestamp processing block, a transmit MACsec processing block, and a transmitter; a receive chain including a receiver, a receive MACsec processing block, a receive timestamp processing block, and a receive flow control block; and wherein the transmit timestamp processing block is configured to determine whether a packet is subject to timestamp processing, and delay provision of the packet to the transmit processing block if and only if the packet is determined to be subject to timestamp processing.
Another aspect of the invention provides a physical layer device, comprising: means for receiving a packet for transmission; means for determining whether the packet is a packet that is to receive timestamp processing; means for, if the packet is to receive timestamp processing, determining a value indicative of a time of transmission of the packet to a communication network; means for, if the packet is to receive timestamp processing, delaying the packet for a time interval determined to avoid having the packet incur a variable delay during subsequent processing due to MACsec processing of a prior packet; and means for transmitting the packet over the communication network.
Another aspect of the invention provides a communication network device including a physical layer device (PHY), a media access controller (MAC), and a packet processing module, the PHY comprising: means for receiving a packet for transmission; means for determining whether the packet is a packet that is to receive timestamp processing; means for inserting a value into the packet indicative of a time of transmission of the packet to a communication network if the packet is to receive timestamp processing; means for delaying the packet for a time interval determined to avoid having the packet incur a variable delay during subsequent processing due to MACsec processing of a prior packet if the packet is to receive timestamp processing; and means for transmitting the packet over the communication network.
These and other aspects of the invention are more fully comprehended upon review of this disclosure.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 is a block diagram of physical layer communication device in accordance with aspects of the invention;
FIG. 2 is a block diagram of a transmit path for a physical layer communication device in accordance with aspects of the invention;
FIG. 3 is a flowchart of a process for handling timing information in accordance with aspects of the invention; and
FIG. 4 is a block diagram of a communication network device in accordance with aspects of the invention.
DETAILED DESCRIPTION
FIG. 1 is a block diagram of a physical layer communication device (PHY) in accordance with aspects of the invention. The PHY includes a receive block 100 to receive an input signal from a communication network and a transmit block 110 to transmit an output signal to the communication network. A local clock 121 may be included in the PHY to provide a timebase for the PHY and supply time values to the receive block and the transmit block. The receive and transmit blocks provide both timestamp processing and MAC security (MACsec) processing. The PHY also includes an interface block 131 for coupling to a higher-level device, such as a media access control device. In some embodiments, other processing blocks may also be included in the signal paths between the receive block and the interface block and between the transmit block and the interface block. The blocks of the PHY are generally implemented with electronic circuitry. As one of skill in the art would understand, the PHY may be implemented as a stand-alone device or as part of a higher layer device that contains the PHY or parts thereof. For example, in one embodiment the PHY is provided in an integrated circuit. Software programming may be used to control operation of some circuitry in the PHY. A programmable processor may be used to configure the circuitry of the PHY and to handle exception conditions.
The transmit block 110 generally receives packets for transmission, buffers the packets, performs timestamp processing for appropriate packets, performs MACsec processing for appropriate packets, and transmits the packets. In various embodiments the transmit block may also perform other functions commonly performed in a transmit chain of a PHY. In addition, in some embodiments the transmit block also pauses packets for flow control purposes in response to receipt of a valid PAUSE frame requesting a pause in transmission in packets by the receive block 100 . In the embodiment shown in FIG. 1 , a transmit flow control block 113 performs the buffering of packets, a transmit timestamp processing block 115 performs the timestamp processing for appropriate packets, a transmit MACsec processing block 119 performs MACsec processing for appropriate packets, and a transmitter 111 transmits the packets.
The transmit flow control block 113 receives packets to be transmitted from the PHY and buffers the packets. As shown in FIG. 1 the transmit flow control block 113 receives packets from the interface block 131 . The transmit flow control block buffers the packets, for example to account for differences in rates between a rate of a higher-level device and a rate of transmission from the transmit block 110 . For example, the reception and transmission may occur at the same nominal bit rate, but the transmit MACsec processing block 119 may add additional bits to packets that slow packet transmission. Additionally, the transmit timestamp processing block 115 may delay transmission of packets. The transmit flow control block 113 may receive indications from the transmit MACsec processing block 119 and the transmit timestamp processing block 115 that data transmission is extended. Alternatively, the transmit flow control block 113 may receive an indication that transmission may proceed. The transmit flow control block 113 may signal the higher-level device to pause or slow supplying packets to the PHY. In some embodiments, the signaling occurs by way of the receive block 100 , with for example the transmit flow control block 113 providing signals to a receive flow control block 107 of the receive chain. In addition, in some embodiments the transmit flow control block delays transmission of packets in response to an indication that a PAUSE frame requesting a pause in transmission of packets has been received. In some of these embodiments control packets, however, are not so delayed. In various embodiments the transmit flow control block receives the indication from the receive block and/or from a higher level by way of the interface block 131 . Pausing packets for flow control purposes in the transmit chain prior to calculating and writing timestamp values may be beneficial in assisting in maintaining accuracy of timestamp information.
The buffered packets are received by the transmit timestamp processing block 115 . The transmit timestamp processing block 115 adds, in some of the packets, an indication of the time the packet is transmitted from the PHY.
The transmit timestamp processing block 115 , for each packet received from the transmit flow control block 113 , determines, for example, using addresses and tags in the packet, whether the packet is one for which timestamp processing will be performed. The timestamp processing generally utilizes the time, as indicated by the local clock 121 , that the packet will be transmitted. For various packets, the time of transmission may be inserted in the packet, added or subtracted to a value in the packet, or supplied to the higher-layer device.
The transmit timestamp processing block 115 may predict the time of transmission by adjusting a time value from the local clock based on expected delays related to or in the transmit MACsec processing block 119 and the transmitter 111 . In some embodiments the transmit timestamp processing block may adjust the time value by a fixed amount for packets subject to MACsec processing. The delay incurred by a timestamped packet in the transmit MACsec processing block 119 may depend on what processing the transmit MACsec processing block 119 performs on a preceding packet. For example, the transmit MACsec processing block 119 may add bits to the preceding packet, and in some embodiments perform operations on information of the packet, for example encryption processing, that otherwise delays the packet, and possibly delays processing of the subsequent packet. Accordingly, the transmit timestamp processing block 115 may delay supplying an already timestamped packet to the transmit MACsec processing block 119 , and account for that delay in determining a timestamp value, so that the added bits, and/or other delays, do not cause a delay in transmission that would reduce accuracy of the predicted time of transmission. In some embodiments all timestamped packets, but not non-timestamped packets, are so delayed, without regard to whether the preceding packet in the transmit chain is modified or to be modified by MACsec processing. In some embodiments the delay of packets subject to timestamping may be performed after determination that a packet is to be timestamped, but prior to timestamping of the packet, such that delay of a packet by the timestamp processing block need not be accounted for in determining timestamp values. The transmit timestamp processing block 115 may also signal the transmit flow control block 113 when a packet is delayed.
The transmit MACsec processing block 119 receives the packets from the timestamp processing block 115 . The transmit MACsec processing block 119 performs, for some of the packets, security related processing, such as encryption. The transmit MACsec processing block 119 , for each packet received from the transmit timestamp processing block 115 , determines, for example, based on addresses and tags in the packet, whether the packet is one for which MACsec processing will be performed. For packets subject to MACsec processing, the MACsec processing generally adds a security tag to a packet and utilizes a cipher to generate and add an integrity check value (ICV) to the packet for use at a receiver to verify that the packet has not been modified. The MACsec processing may also encrypt payload data in the packet. The addition of the security tag and ICV increases the size of the MACsec processed packet so that a following packet may be delayed by the time used to transmit the additional bits, and possibly also delayed due to time required for, for example, encryption processing. The delay incurred may vary with the gap between packets provided to the MACsec processing block, with the delay decreasing as the gap between the packets increases. For example, if the following packet were separated from the MACsec processed packet by a minimum allowed gap, the delay would be large, and if the following packet were separated from the MACsec processed packet by at least the minimum allowed gap plus the number of bits added by the MACsec processing, no additional delay would be incurred.
The transmitter 111 is coupled to the communication link, for example, a fiber optic cable or other communication medium in the communication network, to transmit the output signal. The transmitter 111 processes the packets from the transmit MACsec processing block 119 to produce the output signal. In many embodiments, the output signal is transmitted according to a standard format, for example, a standard for Ethernet.
The receive block 100 generally include blocks that correspond to the blocks of the transmit block 110 . A receiver 101 is coupled to a communication link, for example, another fiber optic cable in the communication network, and thereby receives the input signal. In many embodiments, the input signal is received according to the same standard format as used for the output signal from the transmitter 111 . The receiver 101 processes the input signal to recover data from the input signal and produces data packets. In various embodiments, the receiver 101 also determines starts of the packets, for example, by determining that frame delimiter signals or frame synchronization signals have been received.
A receive MACsec processing block 103 receives packets from the receiver 101 . For each packet, the receive MACsec processing block 103 may determine if a packet is subject to MACsec processing and, if so, perform MACsec processing for the packet. The MACsec processing uses a security tag and ICV in the packet to verify integrity of the packet. The packet may also be decrypted. In some embodiments the receive MACsec processing block performs additional MAC related processing. For example, in some embodiments the receive MACsec processing block also determines if a valid PAUSE frame has been received by the receive block 100 . If so, the receive MACsec processing block provides a signal indicative of receipt of a valid PAUSE frame and in most embodiments information of a length of a requested pause time indicated by the PAUSE frame. The signal is provided to the transmit block 110 , in some embodiments directly and in some embodiments by way of being passed to the receive flow control block 107 . Performing PAUSE frame reception related processing in the PHY, particularly soon after reception, may be beneficial in reducing numbers of packets transmitted after receipt of a PAUSE frame requesting a pause in transmission, or in earlier recommencing of transmission of packets if the PAUSE frame indicates, usually by way of a zero value, that transmission of packet should no longer be paused.
A receive timestamp processing block 105 , for each packet received from the receive MACsec processing block 103 , determines, for example, using addresses and tags in the packet, whether the packet is one for which timestamp processing will be performed. The timestamp processing generally utilizes the time, as indicated by the local clock 121 , that the packet was received. For various packets, the time of reception may be inserted in the packet, added or subtracted to a value in the packet, or supplied to the higher-layer device. The receive timestamp processing block 105 may adjust time values from the local clock based on delays in the receiver 101 and receive MACsec processing block 103 for use as the time of reception. In some embodiments the receive timestamp processing block adjusts time values based on delays in the receive MACsec processing block by a fixed amount for packets subject to MACsec processing.
The receive flow control block 107 receives packets from the receive timestamp processing block 105 and transmits the packets to the interface block 131 . The flow control block 107 buffers the packets to match rates that may differ between reception and transmission. For example, in some embodiments, the reception and transmission may occur at the same nominal bit rate, but with specific bit rates that vary from the nominal rate by different amounts. Additionally, the receive flow control block 107 may supply signals to the higher-layer device to indicate flow control in the transmit path 110 . In addition, in some embodiments the receive flow control block receives a signal from the receive MACsec processing block regarding receipt of a valid PAUSE frame, and the receive flow control block provides information of the PAUSE frame to the transmit flow control block 113 and/or to the interface block 131 for use by higher level processes.
The local clock 121 generally provides time values that are synchronized or syntonized to another clock in the communication network. In some embodiments, the PHY may receive time from a clock external to the PHY.
FIG. 2 is a block diagram of a transmit path for a physical layer communication device in accordance with aspects of the invention. The transmit path may, in some embodiments, be the transmit path in the PHY of FIG. 1 . Accordingly, the transmit path of FIG. 2 receives packet from a higher-layer for transmission and transmits the packets, after processing, to a communication link. Processing that may be performed includes timestamp processing and MACsec processing.
The transmit path includes a flow control block 213 that receives the packets to be transmitted. The flow control block 213 rate buffers the packets and supplies them to a timestamp classifier 215 . The timestamp classifier 215 determines whether the packets are to receive timestamp processing and what type of processing. A timestamp calculator 216 calculates timestamp values related to transmission times of the packets, and a timestamp writer 217 may write the calculated timestamp values into the packets. A MACsec classifier 219 determines whether the packets are to receive security processing and what type of processing. A MACsec cipher block 220 performs the security processing and supplies the packets to a transmitter 211 that outputs a physical signal to the communication link.
The flow control block 213 is similar to or in some embodiments that same as the transmit flow control block of FIG. 1 . Accordingly, the flow control block 213 buffers the packets it receives to match rates that may differ between reception from the higher-level device and transmission from the transmitter 211 . The rates may differ, for example, due to different tolerances between rates that are nominally equal, bits added to packet for security processing, or delays added for timestamp processing. The flow control block 213 may signal the higher-level device to pause or slow supplying packets for transmission.
The timestamp packet classifier 215 classifies the packets according to what type, if any, timestamp action is to be performed. In one embodiment, the packets are classified to be one of five types. A first type includes packets that are not to receive timestamp processing in the transmit path. A second type includes packets that are to have a transmission time value written into the packet. A third type includes packets that are to have a timestamp in the packet modified by subtracting the transmission time value and adding an offset value. A fourth type includes packets that are to have a timestamp in the packet modified by adding the transmission time value and adding an offset value. A fifth type includes packets for which the transmission time value is to be supplied to the higher-layer device. In some embodiments, a timestamp FIFO is used to supply the transmission time values to the higher-layer device. Packets may be classified using values of source and destination addresses in the packets. In some embodiments, the timestamp packet classifier 215 classifies packets according to values of addresses and/or tags in the packets. For example, some of the packets may contain tags for virtual local area networking (VLAN) and/or for multiprotocol label switching (MPLS). Additionally, packets, in some embodiments, may be classified using messages contained in the packets, such as precision time protocol or operations, administration, and maintenance messages. Furthermore, packet classification may use combinations of packet characteristics.
The timestamp packet classifier 215 may delay supplying packets that are classified to receive processing to the timestamp calculator 216 . In some embodiments, however, the delay may be provided subsequent to writing of the timestamp, with for example the timestamp writer 217 instead providing the delay, and with the timestamp calculator 216 taking account of such a delay. The delay is to avoid variation in transmission time, with respect to a timestamp value, that may occur due to MACsec processing. In one embodiment, the timestamp packet classifier 215 delays packets that will receive timestamp processing to allow transmission of a maximum number of bits that may be added to packets by MACsec processing of a preceding packet, and, in some embodiments, an amount of additional time that may be required by MACsec processing of the preceding packet, for example additional time due to encryption processing. In another embodiment, packets are delayed by an amount that provides a gap between a timestamped packet and the preceding packet of at least a minimum gap between packets plus the maximum number of bits that may be added to the preceding packet for MACsec processing. The timestamp packet classifier 215 , in many embodiments, signals the flow control block 213 when packets are delayed for timestamp processing.
The timestamp calculator 216 produces a new timestamp value depending on the classification of the packet. For many packet classifications, the timestamp calculator 216 uses time values supplied to the timestamp calculator 216 . The time values may be supplied by a clock such as the local clock of the PHY of FIG. 1 . Since transmission time may be defined by when a specific part of the packet (for example, the end of an Ethernet start of frame delimiter) enters the communication link from the transmitter 211 , the timestamp calculator 216 adjusts the time values for delays expected in subsequent blocks of the transmit path. In some embodiments the timestamp calculator adjusts the time values by a fixed amount to account for MACsec processing. However, due to delays provided by the timestamp packet classifier 215 , the timestamp calculator 216 may provide accurate timestamp information without adjusting for variable delays caused by MACsec processing, if the packet to be time stamped is delayed by the timestamp packet classifier. In embodiments in which a timestamped packet is delayed to allow for MACsec processing of a preceding packet after timestamp writing, the timestamp calculator also accounts for that delay.
The timestamp writer 217 may write the new timestamp value from the timestamp calculator 216 to a location in the packet. The location written may vary depending on the format of the packet and the classification of timestamp processing. For example, the location of a PTP packet's correction field. In one embodiment, the receive packet writer 107 additionally updates checksum fields in packets that have timestamp values written.
The MACsec packet classifier 219 classifies the packets according to what type, if any, security processing is to be performed. For example, some packets may be classified to have an ICV added to allow integrity checking of the packet, other packets may be classified to be encrypted, and other packets may be classified to receive no MACsec processing. Packets may be classified using values of source and destination addresses in the packets. In some embodiments, the MACsec packet classifier 219 classifies packets according to values of tags in the packets, such as VLAN or MPLS tags. Packet classification may use combinations of packet features. Packets that receive MACsec processing have additional bits added to the packets, accordingly the MACsec packet classifier 219 may signal the flow control block 213 so that it may adequately buffer the packets it receives from the higher-layer device including, in some cases, signaling the higher-layer device to defer supplying packets to the transmit path.
The MACsec cipher block 220 performs security processing according to the classifications provided by the MACsec packet classifier 219 . A security tag is added to the packets that receive security processing. The security tag may be formatted according to IEEE Std. 802.1AE. Various packets have integrity check values added for use at a receiver to verify that the packet has not been modified. The MACsec processing may also encrypt payload data in the packet. Additionally, the MACsec cipher block 220 may recalculate checksum fields for packets that receive security processing. In some embodiments, the MACsec cipher block 220 recalculates checksum fields for packets that had timestamp values written by the timestamp writer 217 .
The transmitter 211 receives packets from the MACsec cipher block 220 and supplies the output signal to the communication link coupled to the transmit path. The transmitter 211 is similar to or in some embodiments that same as the transmitter of FIG. 1 . The blocks of the transmit path may operate on a packet concurrently with one part of the packet in one of the blocks while another part of the packet is in another one of the blocks.
FIG. 3 is a flowchart of a process for handling timing information in accordance with aspects of the invention. The process may be implemented by a PHY device, for example, the device of FIG. 1 .
In block 302 , the process receives a packet for transmission. The packet may be received from a higher-layer device, for example, a media access controller.
In block 312 , the process determines whether the packet is a packet that will receive timestamp processing. Whether a packet will receive timestamp processing may be determined utilizing values of source and destination addresses in the packet. In some embodiments, the process may utilize the values of tags, such as VLAN or MPLS tags, in the packets. Additionally, in some embodiments, the process may utilize a message contained in the packets, such as a precision time protocol or operations, administration, and maintenance message. Furthermore, the process may determine whether the packet is a packet that will receive timestamp processing utilizing a combination of packet features. If the packet is a packet that will receive timestamp processing, the process continues to block 322 ; otherwise, the process continues to block 332 .
In block 322 , the process processes the packet according to a timestamp protocol. For example, the process may insert a value into the packet indicative of when the packet is transmitted to a communication network. The transmission time may be determined by adjusting a time value from a clock to compensate for delays incurred by the packet subsequent to timestamp processing. For example, the packet may be delayed by a MACsec processing block and a transmitter in a PHY as shown in FIG. 1 , and a delay as discussed with respect to block 324 .
In block 324 , the process delays for a time interval. The delay is of a length determined so as to avoid having the packet incur a variable delay in subsequent processing that would impair accuracy of the timestamp processing performed in block 322 . For example, when the packet is transmitted via a block that performs MACsec processing, the packet may be delayed by an amount that depends on the MACsec processing performed on a preceding packet. In one embodiment, the delay length corresponds to a time for transmission of a maximum number of bits that may be added to the preceding packet for MACsec processing. In another embodiment, the delay length corresponds to a time that provides a minimum gap from the preceding packet after the maximum number of bits that may be added to the preceding packet for MACsec processing. In some embodiments the process performs operations of block 324 prior to performing operations of block 322 , in which case the operations of block 322 would not account for the delay provided by the operations of block 324 .
In block 332 , the process transmits the packet on a communication link. The packet may be transmitted by way of a block that performs MACsec processing. The process thereafter returns.
FIG. 4 is a block diagram of a communication network device in accordance with aspects of the invention. The device includes a first line card 401 and a second line card 403 . The first line card includes a PHY 403 that provides timestamp processing and MACsec processing. The PHY may be a PHY as described with reference to FIG. 1 . The PHY is coupled to a MAC 405 which is coupled to a packet processing module 407 . Operation of the first line card is controlled and monitored by a line card control processor 409 . The second line card 411 includes corresponding blocks and in some embodiments is the same as the first line card. FIG. 4 shows two line cards but a system may include many more line cards.
The PHYs 403 , 413 of the first and second line cards 401 , 411 may include a transmit path as described with reference to FIG. 2 . The PHYs provide timestamp processing that includes delaying timestamped packets so that variable delays that the packets may incur due to the MACsec processing do not impair accuracy of timestamp information.
A system card 441 is coupled to the first and second line cards. A switch fabric 445 couples the line cards and switches packets between line cards. A system control processor 443 controls and monitors operation of the system card.
Although the invention has been discussed with respect to various embodiments, it should be recognized that the invention comprises the novel and non-obvious claims supported by this disclosure. | A physical layer device provides both timestamp processing and security processing. The timestamp processing may be PTP processing according to IEEE Std. 1588 and/or OAM processing according to ITU-T Recommendation Y.1731. The security processing may be MACsec processing according to IEEE Std. 802.1AE. The timestamp processing may delay some packets to avoid impairing accuracy of timing information. For example, the accuracy of timing information could be impaired when a packet containing the timing information is delay due to additional bits added to a preceding packet to include a security tag and integrity check value. | 7 |
[0001] This application claims the benefit of U.S. Provisional Application No. 61/030,346, entitled “Simultaneous Generation of Centralized Lightwaves and Double/Single Sideband Optical Millimeter-Wave Requiring Only Low frequency Local Oscillator Signals for radio-Over-Fiber Systems”, filed on Feb. 21, 2008, the contents of which is incorporated by reference herein.
BACKGROUND OF THE INVENTION
[0002] Optical networks designed for Ethernet traffic are becoming more important as the dominance of data over voice services increases. Work in both standards committees and research communities have targeted the transport of 100-Gbit/s Ethernet (100 GE) over wide area networks. Orthogonal frequency division multiplexing (OFDM) is a good transmission format for realizing 100 Gbit/s signal transmission. In recent years, a number of different alternatives have OFDM as a promising method to eliminate the need for optical dispersion compensation in long-haul transmission links. Fiber-optic OFDM systems can be realized either with direct detection optical (DDO) or with coherent optical (CO) detection. Recently, several high data rate OFDM transmission experiments have been reported. Up to 52.5 Gbit/s OFDM signal has been generated and transmitted over 4160 km. But due to the limited bandwidth of the analog to digital converter (A/D) and digital to analog converter (D/A), no 100 Gbit/s OFDM signal has been generated.
[0003] The diagrams of FIGS. 1 and 2 show the architecture to generate over 50 Gbit/s OFDM signal in a publication, Sander Jansen et al., 16×52.5-Gb/s, 50-GHz spaced, POLMUX-CO-OFDM transmission over 4,160 km of SSMF enabled by MIMO processing, ECOC 2007: PD. 1. 3. The diagram of FIG. 1 is directly from the Sander Jansen et al. publication and can be reviewed for further details beyond what are necessary here.
[0004] In the Sander Jansen et al. technique, each modulator structure consists of two single-ended MZM modulators 202 or MZ to modulate each polarization independently. Subsequently the two POLMUX signals are combined using a polarization beam splitter 208 and the even and odd WDM channels are combined with a 50-GHz inter-leaver. The electrical OFDM channel allocation is illustrated in FIG. 1 . Two different frequency RF signals 205 , 206 are mixed with data 1 and data 2 . After the intensity modulator 202 , the electrum spectrum is shown in FIG. 1 , while the optical spectrum is shown in FIG. 2 . Due to the optical carrier suppression, the carrier is suppressed. Then optical filter or inter-leaver ( 207 ) is aligned such that the image band of the OFDM signal is rejected. As you can see in FIG. 2 , only one sideband is employed. Because both sidebands have the same information, one sideband has to be rejected. In this way, only 50 Gbit/s OFDM can be generated due to the limited bandwidth of an A/D converter.
[0005] Accordingly, there is need for a method to generate over 100 Gbit/s OFDM signals with the limited bandwidth for A/D and D/A converter tolerance.
SUMMARY OF THE INVENTION
[0006] In accordance with the invention, a method includes modulating lightwaves to provide first and second OFDM signal sidebands at a first polarization direction and first and second OFDM signal sidebands at a second polarization direction, and combining sidebands that are oppositely positioned and joined from the first and second OFDM signal sidebands at each polarization direction to provide a polarization multiplexing OFDM signal.
[0007] In another aspect of the invention, an apparatus includes a modulator for varying lightwaves to provide first and second OFDM signal sidebands at a first polarization direction and first and second OFDM signal sidebands at a second polarization direction; and a polarization beam combiner for combining sidebands that are oppositely positioned and joined from the first and second OFDM signal sidebands at each polarization direction to provide a polarization multiplexing OFDM signal.
BRIEF DESCRIPTION OF DRAWINGS
[0008] These and other advantages of the invention will be apparent to those of ordinary skill in the art by reference to the following detailed description and the accompanying figures.
[0009] FIGS. 1 and 2 are diagrams illustrating a known technique for generating over 50 Gbit/s in an OFDM signal.
[0010] FIG. 3 is a diagram of an exemplary 100 Gbit/s OFDM optical signal generation for transmission in accordance with the invention.
[0011] FIG. 4 is a diagram of an exemplary reception of 100 Gbit/s OFDM optical signal generated for transmission in accordance with the invention.
[0012] FIG. 5 a diagram of an exemplary 100 Gbit/s OFDM optical signal generation with two RF frequencies for transmission, in accordance with the invention
DETAILED DESCRIPTION
[0013] The invention is directed to a method for generating an over 100 Gbit/s OFDM signal due to both sidebands being employed.
[0014] FIG. 3 is a diagram of an exemplary 100 Gbit/s OFDM optical signal generation for transmission, in accordance with the invention, with only one RF frequency. FIG. 4 is a diagram of an exemplary reception of 100 Gbit/s OFDM optical signal generated for transmission in accordance with the invention. FIG. 5 a diagram of a modification to the configuration of FIG. 3 to show 100 Gbit/s OFDM optical signal generation with two RF frequencies for transmission, in accordance with the invention.
[0015] The diagrams of FIGS. 3 , 4 and 5 are exemplary configurations using the following optical and electrical components: lightwave source 301 , 501 , RF frequency 304 , 505 , 506 ; electrical mixer 303 , 304 , 504 ; optical coupler 306 , 507 ; intensity modulator 302 , 502 ; optical filter 305 , 508 ; and optical polarization beam combiner 307 , 509 .
[0016] The lightwave 301 , 501 can be a narrow linewidth laser less than 2 MHz and the intensity modulator generates optical carrier suppression signals. The electrical mixer 303 , 304 , 504 up-converts the baseband signal to an RF band. The RF signal 304 , 505 , 506 is provided to the electrical mixer so that the base-band can be up-converted. The optical filter 305 , 508 is realized by an optical interleaver so that only a high or low frequency signal can be passed for each port if the interleaver has two ports. Preferably, the interleaver has two input ports and one output port with sharp edge characteristics. The optical coupler 306 , 403 , 507 are preferably 50% to 50% ratio optical couplers that divide the signal into two equal parts. The optical beam combiner or splitter 307 , 404 , 509 combines or splits the orthogonal signal. The electrical combiner 503 combines two different frequency RF signals.
[0017] Referring to the diagram of FIG. 3 , each intensity modulator 302 is driven by the mixed OFDM signal at RF frequency of f 304 by an electrical mixer 303 . The lightwave 301 is split into two parts by an optical coupler 306 . Then the two parts will be split again by the same optical coupler 306 . There are two polarization directions. We assume that the up-subchannel is X polarization direction and the bottom-one is Y polarization direction. Each modulator 302 is operated at carrier suppression OCS mode. After the modulator, the carrier is suppressed. Then for each polarization direction, we use an optical filter 305 , such as an optical inter-leaver to combine the two subchannels. When the interleaver 305 is matched to the wavelength of the input lightwave, we can generate an optical spectrum 308 and 309 as shown in FIG. 3 . Each one just passes through half of spectrum (right or left). The optical filter 305 plays a key role tin generating the optical spectrum 308 or 309 and this is the main difference from that technique of FIG. 1 or 2 . For example, in this figure with the invention, only right (black) and blue (left) can pass the interleaver. Then both sidebands can be used to carry the optical signals. After combing the X and Y polarization direction subchannels by an optical polarization beam combiner 307 , we can generate polarization multiplexing OFDM optical signals.
[0018] The diagram of FIG. 4 shows an exemplary receiver configuration for receiving the 100 Gbit/s OFDM signal generated according to FIG. 3 . The incoming lightwave is separated into two parts by an optical filter 401 , interleaver or other optical filter. Then the right and left side will be detected by a regular 90 degree polarization-diversity coherent detector which includes a local oscillator LO 402 fed through optical couplers 403 , 404 to separate coherent detectors 403 .
[0019] The OFDM signal is generated from the D/A converter. Due to the D/A converter bandwidth limitation, the OFDM signal may not be high enough to carry a signal for over 100 Gbit/s signal (the total capacity with all sub-channels). So we need to change FIG. 3 to FIG. 5 to add one more RF frequency. Here, two RF frequencies, f 1 505 and f 2 506 are used. They are used to carry the OFDM signal and drive the modulator. The overall architecture is similar to FIG. 3 , only one more RF frequency is used. From FIG. 5 we can see that more spectrum components are generated.
[0020] The present invention has been shown and described in what are considered to be the most practical and preferred embodiments. It is anticipated, however, that departures may be made therefrom and that obvious modifications will be implemented by those skilled in the art. It will be appreciated that those skilled in the art will be able to devise numerous arrangements and variations which, not explicitly shown or described herein, embody the principles of the invention and are within their spirit and scope. | A method includes modulating lightwaves to provide first and second OFDM signal sidebands at a first polarization direction and first and second OFDM signal sidebands at a second polarization direction, and combining sidebands that are oppositely positioned and joined from the first and second OFDM signal sidebands at each polarization direction to provide a polarization multiplexing OFDM signal. | 7 |
FIELD OF THE INVENTION
The present invention relates to a process for the conversion of 1, 4 butynediol to 1, 4 butanediol, or a mixture of 1, 4 butenediol and 1,4 butanediol. More particularly, the present invention relates to a process for the preparation of 1, 4 butanediol, or a mixture of 1, 4 butenediol and 1,4 butanediol (in different compositions) in a fixed bed reactor using a platinum supported calcium carbonate catalyst.
BACKGROUND OF THE INVENTION
1, 4 butenediol is a useful intermediate in the production of pesticide, insecticide and vitamin B6. Being an unsaturated diol it can be used in the synthesis of many organic products such as tetrahydrofuran, n-methyl pyrrolidione, γ-butyrolactone, etc. It is also used as an additive in the paper industry, as a stabiliser in resin manufacture, as a lubricant for bearing systems and in the synthesis of allyl phosphates. 1, 4 butanediol also has a variety of applications such as in the preparation of polyurethane foams and other polyesters as well as in the preparation of tetrahydrofuran.
Prior art discloses the use of a number of catalysts for the manufacture of 1, 4 butenediol by the hydrogenation of 1, 4 butynediol. Most of the prior art patents are based on a combination of palladium with one or more mixed compounds of copper, all zinc, calcium, cadmium, lead, alumna, mercury, tellurium, gallium, etc. GB A 871804 describes the selective hydrogenation of acetylinic compound in a suspension method using a Pd catalyst which has been treated with the salt solutions of Zn, Cd, Hg, Ga, Th, In, or Ga. The process is carried out at milder conditions with 97% selectivity for cis 1,2-butenediol and 3% to the trans form. Moreover, additional amines are used in this process.
U.S. Pat. No. 2,681,938 discloses the use of a Lindlar catalyst (lead doped Pd catalyst), for the selective hydrogenation of acetylinic compounds. The drawback of this process is the use of additional amines such as pyridine to obtain good selectivity for 1, 4 butenediol.
German patent DE 1, 213, 839 describes a Pd catalyst doped with Zn salts and ammonia for the partial hydrogenation of acetylinic compounds. However, this catalyst suffers from the drawback of short lifetime due to poisoning.
German patent application DE-A 2, 619, 660 describes the use of Pd/Al 2 O 3 catalyst that has been treated with carbon monoxide for the hydrogenation of butynediol in an inert solvent. The disadvantage of this catalyst is that the catalyst is treated with carbon monoxide gas which is highly toxic and difficult to handle.
U.S. Pat. No. 2,961,471 discloses a Raney nickel catalyst useful for the partial hydrogenation of 1, 4 butynediol. The catalyst of this process gives a low selectivity for 1, 4 butenediol.
U.S. Pat. No. 2,953,604 describes a Pd containing charcoal and copper catalyst for the reduction of 1,4 butynediol to 1,4 butenediol with 81% selectivity for 1,4 butenediol. However, this process results in the formation of a large number of side products and is therefore undesirable.
U.S. Pat. No. 4,001,344 discloses the use of palladium mixed with γ- Al 2 O 3 along with both zinc and cadmium or either zinc or cadmium together with bismuth or tellurium for the preparation of 1,4 butenediol by the selective hydrogenation of 1, 4 butynediol. However, a large number of residues are formed (7.5-12%) which lowers the selectivity of 1,4 butenediol to 88%.
U.S. Pat. Nos. 5,521,139 and 5,278,900 describes the use of a Pd containing catalyst for the hydrogenation of 1,4 butynediol to prepare 1,4 butenediol. The catalyst used is a fixed bed catalyst prepared by applying Pd and Pb or Pd and Cd successively by vapor deposition or sputtering to a metal gauze or a metal foil acting as a support. In this process also the selectivity obtained for cis 1,4 butenediol is 98%. The disadvantage of this process is that a trans butenediol with residues are also obtained.
Prior art also discloses a number of catalysts for the preparation of 1,4 butanediol by the hydrogenation of 1,4 butynediol.
Most prior art patents are based on a combination of palladium or nickel with one or more of mixed compounds of copper, manganese, molybdenum, zirconium, etc.
U.S. Pat. No. 3,449,445 discloses a process for the hydrogenation of 1,4 butynediol to 1,4 butanediol with good yield using a catalyst containing Ni, Cu, and Mn on silicon dioxide. The disadvantage of this process is that when 1,4 butanediol is prepared by this process on an industrial scale, silicon dioxide is deposited in the heat exchangers and pipelines, the removal of which is a highly laborious procedure.
De OS 2,536, 276 describes the preparation of 1,4 butanediol by the hydrogenation of 1,4 butynediol using the oxides of Ni, Cu, Mo, and Mn.
U.S. Pat. No. 5,015,788 describes a process for the hydrogenation of acetylinic compounds using a catalyst containing oxides of Ni, Cu, Mo and Zr. While the process shows promising results at high temperature of upto 250° C. and pressure of 150 bar, side products such as butanol, 2-methyl 1,4 butanol, γ-hydroxylactone, 4-hydroxybutaraldehyde, etc. are formed.
EP 337572 discloses a process for the preparation of alkanediols using H in the presence of cationic Pd, a corresponding anion and bidentate ligands with high selectivity for 1,4 butanediol. However, this process suffers from a major drawback in that side products such as γ-hydroxy butyraldehyde are formed and expensive bidentate ligands need to be used.
EP 295435 describes a process for the preparation of 1,4 butanediol with high selectivity using a nickel acetate catalyst with the addition of C ≧2 organic acids at high temperatures (185-195° C.) and hydrogen pressure (250 bar). While the selectivity for 1,4 butanediol is good, unwanted side products such as n-butanol, hydroxybutaraldehyde, 2-methyl 1,4 butanediol, acetal and the like are formed. Moreover, the process is carried out at a very high temperature and H 2 pressure.
All the above processes for the hydrogenation of butynediol to butenediol or butanediol suffer from disadvantages such as high temperatures, pressures, formation of side products. The formation of side products and residues affect the efficiency of the process and the recovery of pure 1,4 butenediol and butanediol is difficult. An additional drawback is that the catalysts used for these processes contain more than two metals along with other promoters such as organic amines. Their preparation is cumbersome. All the reported processes also do not give complete selectivity for the desired products either 1,4 butenediol or 1,4 butanediol. The catalysts also suffer from fast deactivation due to poisoning.
The prior art literature shows that the catalysts used for the hydrogenation of 1,4 butynediol are mainly palladium or nickel based catalysts. There is no disclosure or report on the use of platinum based catalysts for the hydrogenation of 1,4 butynediol to prepare 1,4 butanediol or a mixture of 1,4 butenediol and 1,4 butanediol (in various compositions).
It is therefore important to obtain and/or develop catalysts that overcome the disadvantages of prior art catalysts used in the hydrogenation of 1,4 butynediol to 1,4 butanediol or a mixture of 1,4 butenediol and 1,4 butanediol (in various compositions) enumerated above.
OBJECTS OF THE INVENTION
The main object of the invention is to provide a process for the preparation of diols, particularly 1, 4 butanediol or mixtures of 1,4 butenediol and 1,4 butanediol (in varying proportions) by the hydrogenation of 1,4 btuynediol that is cheap and efficient.
It is another object of the invention to provide a process for the preparation of 1,4 butanediol with 100% selectivity.
It is another object of the invention to provide a process for the preparation of mixtures of 1,4 butenediol and 1,4 butanediol in vrying proportions under mild reaction conditions.
SUMMARY OF THE INVENTION
Accordingly the present invention provides a process for the conversion of 1, 4 butynediol to 1, 4 butanediol, or a mixture of 1, 4 butenediol and 1,4 butanediol comprising hydrogenating aqueous solution of 1,4 butynediol using platinum supported CaCO 3 catalyst at a temperature in the range of 20-190° C. under a hydrogen pressure in the range between 5-100 bar and collecting the product by any conventional method.
In one embodiment of the invention, the concentration of 1,4 butynediol in aqueous medium is in the range of 10-70%, preferably 15-50%.
In another embodiment of the invention, the gas hourly space velocity (GHSV) is in the range of 500-12000 h −1 , preferably 1000-10000 h −1 .
In another embodiment of the invention, the liquid hourly space velocity (LHSV) is in the range of 0.05-15 h −1 , preferably 0.1-10 h −1 .
In another embodiment of the invention, the process is carried out under hydrogen pressure of 10-80 bar.
In a further embodiment of the invention, the process is carried out at a temperature in the range of 40-160° C.
In another embodiment of the invention, the catalyst is run for 200 hours and the turn over number (TON) is 7.24×10 4 .
In another embodiment of the invention, the catalyst is of the of the general formula AB(y) wherein A is a support comprising of carbonate of calcium, B is platinum and y=0.2 to 10%.
DETAILED DESCRIPTION OF THE INVENTION
In the present invention the catalyst is prepared by impregnating platinum supported CaCO 3 in a basic medium (pH=7-12), stirred in water and heated in the temperature range of 60-120° C., preferably 70-90° C. The mixture is then reduced by adding a conventional reducing agent such as formaldehyde. The solution is stirred, filtered, washed and dried at a temperature in the range of 100-250° C., preferably 140-200° C. in static air for a period in the range of 5-12 hours.
The hydrogenation catalyst used is of the general formula AB(y) wherein A is a support comprising of a salt of a Group II A metal, B is platinum and y=0.2 to 10%.
The catalyst used in the invention is prepared by:
i. dissolving a platinum precursor in a mineral acid by stirring at a temperature in the range between 60° C. to 120° C.;
ii. diluting the above solution by adding water;
iii. adjusting the pH of the solution to the range of 8-12 by the addition of a base,
iv. adding a support to the above solution;
v. heating the mixture to a temperature in the range of 60° C. to 120° C.;
vi. reducing the above mixture using a conventional reducing agent;
vii. separating the catalyst formed by any conventional method;
viii. washing and drying the product to obtain the desired catalyst.
The platinum precursor is a salt of platinum selected from the group comprising of acetate, bromide, and chloride of platinum. The support is a salt of a Group II A metal selected from the group comprising of acetate, nitrate, chloride, carbonates of magnesium, calcium, and barium. The base used may be selected from the group comprising of sodium carbonate, potassium carbonate, potassium hydroxide, and sodium hydroxide.
The reducing agent used is selected from the group comprising of hydrazine hydrate, hydrogen containing gas, and formaldehyde.
Hydrogenation was carried out in a single tube reactor of 19 mm diameter. In a typical experiment the catalyst was charged approximately in the middle portion of the reactor tube. The space above and below the catalyst was packed with inert carborundum beads. The reactor was heated by an electric furnace. The liquid feed 1,4 butynediol and hydrogen were introduced near the top of the reactor. The inert zone over the top of the catalyst served as a preheater for the reactants. The product stream leaving the reactor is cooled to condense the liquid products. The products are analysed using a gas chromatograph after the reaction. It is noted that the selectivity of the process at milder process conditions is 100%.
The present invention is described below by way of examples. However, the following examples are illustrative and should not be construed as limiting the scope of the invention.
EXAMPLE 1
Preparation of 1% Pt/CaCO 3 Catalyst
0.17 gms of platinum chloride was dissolved in 4 ml of hydrochloric acid and stirred at 80° C. till the platinum chloride was completely dissolved. The resultant solution was diluted by adding 50 ml of water and stirring for 2 hours, the pH being maintained between 9-10 by the addition of sodium hydroxide. To the diluted solution, 10.03 gins of calcium carbonate was added and the mixture heated at 80° C. for 1 hour. The mixture was then reduced by the addition of formaldehyde (3 ml), stirred for 45 minutes, filtered and washed with water till the solution is alkaline free. The catalyst was then dried at 150° C. for 10 hours.
EXAMPLE 2
Performance of 1% Pt/CaCO 3 Catalyst (10 gms)in the Hydrogenation of 1,4 Butynediol to 1,4 Butenediol and 1,4 Butanediol
This example illustrates the performance of 1% Pt/CaCO 3 catalyst (10 gms) in the hydrogenation of 1,4 butynediol to 1,4 butenediol and 1,4 butanediol
The reaction was carried out in a fixed bed reactor in the presence of the catalyst according to the procedure described hereinabove.
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
10.0 gms
Temperature
50°, 75° and 100° C.
H 2 pressure
25 bar
H 2 flow
10 NL/hour
Liquid flow
10 cm 3 /hour
The following results are obtained:
Temperature (° C.)
50
75
100
1,4 butynediol conversion (%)
35.0
53.7
50.2
Selectivity for 1,4 butanediol (%)
51.0
54.1
55.0
Selectivity for 1,4 butenediol (%)
49.0
45.9
45.0
EXAMPLE 3
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
10.0 gms
Temperature
100° C.
H 2 pressure
25 bar
H 2 flow
10, 20, 30 and 60 NL/hour
Liquid flow
10 cm 3 /hour
The following results are obtained:
H 2 flow (NL/hr)
10
20
30
60
1,4 butynediol conversion (%)
50.2
59.1
56.5
54.4
Selectivity for 1,4 butanediol (%)
55.0
60.6
30.0
30.2
Selectivity for 1,4 butenediol (%)
45.0
39.4
70.0
69.8
EXAMPLE 4
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
10.0 gms
Temperature
75° C.
H 2 pressure
25 bar
H 2 flow
10, 20, 30 and 60 NL/hour
Liquid flow
10 cm 3 /hour
The following results are obtained:
H 2 flow (NL/hr)
10
20
30
60
1,4 butynediol conversion (%)
53.7
21.7
20.1
20.1
Selectivity for 1,4 butanediol (%)
54.0
29.8
30.9
30.0
Selectivity for 1,4 butenediol (%)
46.0
70.2
69.1
70.0
EXAMPLE 5
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
10.0 gms
Temperature
50° C.
H 2 pressure
25 bar
H 2 flow
10, 20, 30 and 60 NL/hour
Liquid flow
10 cm 3 /hour
The following results are obtained:
H 2 flow (NL/hr)
10
20
30
60
1,4 butynediol conversion (%)
35.0
21.4
19.2
18.2
Selectivity for 1,4 butanediol (%)
51.0
65.0
64.3
62
Selectivity for 1,4 butenediol (%)
49.0
35.0
35.7
38
EXAMPLE 6
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
10.0 gms
Temperature
100° C.
H 2 pressure
25 bar
H 2 flow
10 NL/hour
Liquid flow
10, 20 and 40 cm 3 /hour
The following results are obtained:
Liquid flow (cm 3 /hour)
10
20
40
1,4 butynediol conversion (%)
50.2
39.6
16.0
Selectivity for 1,4 butanediol (%)
55.0
69.0
27.9
Selectivity for 1,4 butenediol (%)
45.0
31.0
72.1
EXAMPLE 7
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
10.0 gms
Temperature
75° C.
H 2 pressure
25 bar
H 2 flow
10 NL/hour
Liquid flow
10, 20 and 40 cm 3 /hour
The following results are obtained:
Liquid flow (cm 3 /hour)
10
20
40
1,4 butynediol conversion (%)
53.7
28.3
23.5
Selectivity for 1,4 butanediol (%)
54.1
24.0
24.6
Selectivity for 1,4 butenediol (%)
46.0
76.0
75.6
EXAMPLE 8
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
20.0 gms
Temperature
50° C.
H 2 pressure
15, 25, 40 and 60 bar
H 2 flow
10 NL/hour
Liquid flow
10 cm 3 /hour
The following results are obtained:
H 2 pressure (bar)
15
25
40
60
1,4 butynediol conversion (%)
32.1
50.9
62.6
90.0
Selectivity for 1,4 butanediol (%)
60.1
60.7
57.8
62.0
Selectivity for 1,4 butenediol (%)
39.9
39.3
42.2
38.0
EXAMPLE 9
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
20.0 gms
Temperature
75° C.
H 2 pressure
15, 25, 40 and 60 bar
H 2 flow
10 NL/hour
Liquid flow
10 cm 3 /hour
The following results are obtained:
H 2 pressure (bar)
15
25
40
60
1,4 butynediol conversion (%)
49.6
70.9
62.6
100
Selectivity for 1,4 butanediol (%)
52.4
52.8
57.8
66.6
Selectivity for 1,4 butenediol (%)
47.6
47.2
42.2
33.5
EXAMPLE 10
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
20.0 gms
Temperature
100° C.
H 2 pressure
15, 25 and 40 bar
H 2 flow
10 NL/hour
Liquid flow
10 cm 3 /hour
The following results are obtained:
H 2 pressure (bar)
15
25
40
1,4 butynediol conversion (%)
74.7
92.8
100
Selectivity for 1,4 butanediol (%)
52.5
55.2
55.5
Selectivity for 1,4 butenediol (%)
47.5
45.1
44.5
EXAMPLE 11
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
20.0 gms
Temperature
50°, 75° and 100° C.
H 2 pressure
25 bar
H 2 flow
10 NL/hour
Liquid flow
20 cm 3 /hour
The following results are obtained:
Temperature (° C.)
50
75
100
1,4 butynediol conversion (%)
16.8
18.3
53.4
Selectivity for 1,4 butanediol (%)
48.2
50.0
39.5
Selectivity for 1,4 butenediol (%)
51.8
50.0
60.5
EXAMPLE 12
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
20.0 gms
Temperature
100° C.
H 2 pressure
25 bar
H 2 flow
20, 40 and 60 NL/hour
Liquid flow
10 cm 3 /hour
The following results are obtained:
H 2 flow (NL/hr)
20
40
60
1,4 butynediol conversion (%)
80.5
78.6
86.5
Selectivity for 1,4 butanediol (%)
44.2
49.4
43.3
Selectivity for 1,4 butenediol (%)
55.9
50.4
57.1
EXAMPLE 13
This example illustrates the performance or the use of the 1% Pt/CaCO 3 catalyst (5 gms) in the hydrogenation of 1,4 butynediol to 1,4butenediol and 1,4 butanediol.
The reaction was carried out in a fixed bed reactor in the presence of the catalyst according to the procedure described hereinabove.
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
5.0 gms
Temperature
75° C.
H 2 pressure
25 bar
H 2 flow
10 NL/hour
Liquid flow
10 and 20 cm 3 /hour
The following results are obtained:
Liquid flow (cm 3 /hour)
10
20
1,4 butynediol conversion (%)
13.0
8.3
Selectivity for 1,4 butanediol (%)
40.2
55.0
Selectivity for 1,4 butenediol (%)
59.8
45.0
EXAMPLE 14
This example illustrates the performance or the use of the 1% Pt/CaCO 3 catalyst (30 gms) in the hydrogenation of 1,4 butynediol to 1,4butenediol and 1,4 butanediol.
The reaction was carried out in a fixed bed reactor in the presence of the catalyst according to the procedure described hereinabove.
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
30.0 gms
Temperature
125° C.
H 2 pressure
25 and 40 bar
H 2 flow
10 NL/hour
Liquid flow
10 cm 3 /hour
The following results are obtained:
H 2 pressure (bar)
25
40
1,4 butynediol conversion (%)
100
100
Selectivity for 1,4 butanediol (%)
95.8
96.2
Selectivity for 1,4 butenediol (%)
4.2
3.8
EXAMPLE 15
The reaction was carried out at the following reaction conditions:
Concentration of 1,4 butynediol in water
20%
Weight of catalyst
30.0 gms
Temperature
140° C.
H 2 pressure
25 bar
H 2 flow
10 NL/hour
Liquid flow
10 cm 3 /hour
The following results are obtained:
1,4 butynediol conversion (%)
100
Selectivity for 1,4 butanediol (%)
100
Advantages of the Invention
1. The catalyst of the invention is useful for the selective hydrogenation of 1, 4 butynediol to 1, 4 butanediol or 1, 4 butenediol and 1,4 butanediol (in various compositions) without poisoning.
2. Selective hydrogenation of 1, 4 butynediol to 1, 4 butanediol is achieved in a continuous operation using 1% Pt/CaCO 3 catalyst without addition of any promoter or ammonia in the reaction mixture.
3. Substantially complete conversion of 1, 4 butynediol to 1, 4 butenediol with almost 100% selectivity to cis 1, 4 butenediol is obtained at milder process conditions.
4. The separation of the product 1, 4 butanediol in pure form is achieved easily by the removal of the catalyst from the reaction mixture.
5. The product mixture of 1,4 butenediol and 1,4 butanediol is obtained without any side product formation. Also, the composition of the product mixture can be varied by changing the reaction conditions. | The present invention relates to a process for the conversion of 1,4 butynediol to 1,4 butanediol or a mixture of 1,4 butanediol and 1,4 butenediol comprising hydrogenating an aqueous solution of 1,4 butynediol using platinum supported CaCO 3 catalyst at a temperature in the range of 20-190° C. under a hydrogen pressure in the range between 5-100 bar and collecting the product by any known method. | 2 |
[0001] This is a continuation of application Ser. No. 11/703,827 filed Feb. 8, 2007 which is a continuation of application Ser. No. 10/375,458 filed Feb. 27, 2003, which claims the benefit of Provisional Application No. 60/362,475 filed Mar. 7, 2002. The entire disclosures of the prior applications, application Ser. Nos. 11/703,827 and 10/375,458 are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
[0002] During the early to mid-1980s, car manufacturers, under pressure to increase fuel economy and simultaneously reduce emissions, switched to electronic fuel injection to obtain more precise control of engine fuel under all operating conditions. When the automotive aftermarket saw the trend, it entered the field, first with PROM chips that allowed the buyer to modify the constants programmed into the electronic controller unit at the factory by simply switching chips. This allowed one to increase performance somewhat, generally at the expense of gas mileage, and to make engine modifications for which changes in program parameters were needed. Gradually, conversion kits were developed to allow hobbyists and racers to upgrade carbureted engines to Electronic Fuel Injection (EFI) or to replace OEM Electronic Control Units (ECUs) to obtain much more control over the system than the re-programmed PROM chips allowed. One of the first of these was U.S. Pat. No. 4,494,509 (1985) to Long. Although now plentiful, these kits are quite costly and difficult to install and configure. Numerous drivability problems whose solutions are beyond the capabilities of the users are also often reported after the installation. Furthermore, the price of these systems places them well beyond the reach of most hobbyists and enthusiasts.
[0003] The present invention provides an engine controller that is: more cost effective because of its low parts count due to integrated technology; simpler to install because of its generic design and flexible software, allowing it to be used with all models and makes of
[0000] engines from motorcycles to trucks, even or odd number of cylinders, and regardless of the experience of the end user. The design is also more reliable because of several software algorithms that will be described.
OBJECTS AND SUMMARY OF THE INVENTION
[0004] A general object of an embodiment of the present invention is to provide a simple, reliable, user configurable system (electronic circuit and software) for electronic fuel injection control.
[0005] An object of an embodiment of the present invention is to provide an aftermarket EFI system that can be manufactured at low cost.
[0006] Another object of an embodiment of the present invention is to provide a generic EFI system that can be used with a large variety of engines of different sizes, numbers of cylinders, types and sizes of fuel injectors, and types of ignition systems.
[0007] A further object of an embodiment of the present invention is to provide an EFI system that can be easily installed by hobbyists and non-professional users with only a limited knowledge of electronics, computers, and the principles of electronic fuel control.
[0008] Another object of an embodiment of the present invention is to provide an EFI system with reduced susceptibility to electronic noise.
[0009] Briefly, and in accordance with at least one of the foregoing objects, an embodiment of the invention provides an integrated microprocessor based electronic circuit and software that uses an external tachometer signal and various sensor inputs to calculate combustion engine fuel requirements, and provides corresponding electronic control signals to open and close the engine mounted fuel injectors. Parameters for the calculation of these signals are user configurable.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The present invention may best be described with reference to the accompanying drawings in which:
[0011] FIG. 1 is a block diagram providing an overview of the system.
[0012] FIG. 2 shows specifics of the integrated microprocessor and its regulated power supply.
[0013] FIG. 3 provides circuit diagrams of the conditioning and filtering of the sensor inputs.
[0014] FIG. 4 provides circuit diagrams for the fuel injector drivers, auxiliary outputs, and status LED lights.
[0015] FIG. 5 provides a block diagram of the software logic.
[0016] FIGS. 6A to 6 G provide a software assembler listing for the ECU in the form of s-records that can be downloaded to a suitable micro controller.
DETAILED DESCRIPTION OF THE INVENTION
[0017] While the invention may be susceptible to embodiment in different forms, there is shown in the drawings, and herein will be described in detail, a specific embodiment with the understanding that the present disclosure is to be considered an exemplification of the principles of the invention, and is not intended to limit the invention to that as described herein.
[0000] 1. Circuit Description
[0018] The overall hardware system is shown in FIG. 1 and is detailed in the following figures. We start the circuit description with the power supply (U 5 in FIG. 2 ). This is an automotive grade linear 5-volt regulator that can, by itself, handle reverse and over-voltages. To this has been added the combination of diodes D 14 and D 16 , which clamp reverse voltage spikes to −12 volts. D 13 only permits positive polarity voltage to pass to D 15 , which clamps this voltage to 22 volts eliminating the over-voltage effects of switched loads. The total combination provides an extremely robust power supply. Also, there are two power supply filter circuits—one consists of capacitor C 18 and inductor L 1 , providing power to the internal Phase Lock Loop (PLL) clock, and L 2 , C 21 , and C 22 , which filter the analog power supply for the analog-to-digital converter.
[0019] The CPU of choice for this application is the Motorola MC68HC908GP32 (U 1 ). This CPU is a member of Motorola's HCO8 family of micro controllers, providing a rich integration of features, and hence allows a low system parts count. The CPU core runs at an internal bus speed of 8 MHz, which is derived from an internal phase-locked loop clocked from a 32.768 KHz crystal (Y 1 ). The GP32 version has 32 Kbytes of on-chip flash ROM memory with direct in-circuit programming, which allows for the storage and runtime re-programming of constants that is extremely desirable in this application. There are 512 bytes of on-chip RAM memory—more than adequate for this application. Other features include two 16-bit, 2-channel timers, serial communication channels, and an 8-channel, 8-bit Analog to Digital Converter (ADC) for measuring sensor inputs.
[0020] The CPU oscillator circuit is comprised of a 32.768 watch crystal (Y 1 ), two capacitors (C 23 and C 24 ), and two resistors (R 21 and R 22 ). The on-chip PLL clock circuit requires the external loop filter network C 19 , C 20 , and R 20 . The microprocessor has an internal power-on reset circuit, so no external circuitry is required.
[0021] Tuning of system configuration parameters while the engine is running is key to a successful injector control unit. This system uses a standard RS-232 communication interface chip (U 6 ) to talk to a host PC, which is running a custom application that allows the download and tuning of the relevant parameters.
[0022] The sensor inputs to the system are shown in FIG. 3 . The driving input for the system is the tachometer or timing signal, which is generally taken from the ignition circuit (ignition coil primary circuit or tachometer drive). This signal is clipped to +5V by Zener diode D 8 , and applied to a 4N25 opto isolator (U 4 ) providing immunity to damage from over-voltage. The phototransistor in the opto isolator is biased by R 11 and fed into the interrupt pin IRQ 1 of the micro controller. By timing the interrupts and knowing that each one represents a cylinder firing, the RPM can be calculated by the micro controller. Furthermore, to significantly reduce the probability of a false tach trigger, a software time-adaptive filter is used on the interrupt such that it is only re-enabled for future triggers after some point in the RPM period is reached, for example the V 2 way point.
[0023] The other critical input to the system comes from the manifold absolute pressure (MAP) sensor (U 3 ) that monitors intake manifold vacuum. The sensor used here is the Motorola MPX4250 which is an integrated pressure sensor containing the sensing element, coupled to the engine manifold by a flexible tube, and an amplifier and temperature compensation circuitry all in one package, yielding an analog output which is proportional to applied pressure (absolute, not gauge). The output of the MAP sensor is filtered by R 2 and C 4 , clamped by diode D 1 , and is supplied to channel 0 of the ADC in the micro controller. Using this sensor allows the system to handle normally aspirated and turbo engines to 2.5 Bar. Also, the MAP sensor ADC is sampled in the CPU at a fixed time after receipt of the tach signal; doing this eliminates fluctuation of the pressure due to piston motion during the engine cycle, and hence provides a consistent fuel mixture and a smoother running engine.
[0024] This fuel injection system is of the “speed-density” variety, meaning that the amount of air consumed (and required fuel) is deduced from the manifold absolute pressure and the RPM at which the engine is operating. Hence, with just these inputs, the engine can be run; the other inputs that follow provide more optimal control under different load and environmental conditions.
[0025] Engine temperature measurements are sensed by negative-coefficient thermistors mounted in the intake air stream (MAT) and engine coolant liquid (CLT). In order to sense the resistance of the sensors, they are configured as part of a voltage divider circuit—R 4 for the MAT sensor and R 7 for the CLT sensor. One side of each sensor is tied to ground. The resultant divider voltage is filtered by R 5 and C 5 , C 6 for the MAT sensor and R 8 and C 8 , C 7 for the CLT sensor, and protected from over-voltage by D 2 and D 3 .
[0026] Real-time sensing of throttle position is required by the CPU in order to provide more fuel during periods of rapid throttle opening. The standard throttle position sensor (TPS) is a simple 10K potentiometer attached to the engine throttle shaft with a constant voltage (5 volts in this case) across the potentiometer. The wiper terminal of the pot will therefore provide a variable voltage between 0 to 5 volts. This voltage is filtered by C 10 and R 9 and clamped by diode D 4 , and then applied to ADC channel 3 .
[0027] Other input sensors include battery voltage (needed to adjust the injector opening time), derived by the resistor divider consisting of R 3 and R 6 , and the exhaust gas oxygen content sensor (02). The 02 sensor is a special device that generates a small voltage (approx. 0.6 volts) when the ratio of gas to air is less than 14.7. Once again, the common theme of filtering (R 1 and C 2 ) and limiting (D 11 ) is utilized.
[0028] The boot loader header (H 1 ) allows a user to pull the battery voltage terminal (AD 4 ) on the CPU down to ground. This is sensed in the CPU software and is recognized as the signal to cease normal operation and load new software in the CPU ROM memory using the RS232 port.
[0029] FIG. 4 is the schematic for the various output drivers for fuel injectors and relays. Starting with the fuel injectors, there are two separate but identical fuel injector drivers (only the first of them will be described). A timer output compare/PWM channel in the CPU is fed into one of the two input channels of the transistor driver chip (U 7 ), which provides fast gate drive (via R 12 ) to the Field Effect Transistor (FET) Q 2 . This is important because the injector needs to be opened as rapidly as possible if fuel metering is to be precise. The fuel injectors are pulled low by Q 2 , and over-voltage and inductive kickback from them are handled by the combination of Zener diode D 21 and the Darlington transistor (Q 1 ). The two FET injector drivers may be connected to two banks of as many injectors as the drivers can handle. This must be determined by the injector current requirements, but 4 injectors per bank is easily achievable. The user can specify through the configuration software how often to fire each bank of injectors relative to the tach input, and whether to fire them sequentially, so that each injector fires once every engine cylinder cycle of two crank revolutions, or simultaneously, such that each injector fires every crank revolution. This allows the system to be used with throttle body injectors (one or two central injectors) or multiport (one injector per cylinder).
[0030] To be truly generic it is required that the system handle the two common electrical impedances for fuel injectors: high impedance (roughly 12-16 ohms) and low impedance (1.2 to 2.5 ohms). The high impedance type (also known as saturated) provides its own current limiting, due to its comparably high resistance, and can be driven directly by Q 2 . The low-impedance types, known as peak-and-hold injectors, require a different drive strategy. These injectors like to have higher “peak” current applied, say 4 amps, while they are opening, and a lower “hold” current (like 1 amp or so) to keep them open. To provide this relative current control, Q 2 is driven fully on during the time the injector is opening. When a predetermined time has elapsed which is sufficient to ensure that the injector is open (based on injector impedance and supply voltage), the drive to Q 2 is switched to a pulse-width modulation mode (using the PWM mode of the timer channel), with a frequency of 15 KHz and a duty cycle which keeps the average current through the injector at the desired “hold” value. Both the duration of the “peak” current and the amount of reduction in amplitude during the “hold” portion are configurable by the user in the software.
[0031] Direct control of a fast-idle solenoid is provided by Q 5 (spikes limited by D 9 ), which is opened when the engine is first started and not at a fully warmed temperature. The fast idle solenoid provides an air bypass around the throttle plates to provide additional air in the intake manifold. The operation of the electric fuel pump is also controlled in the micro controller (via a relay) using Q 3 .
[0032] Finally, three LED lights are switched by transistors Q 9 -Q 11 . The first tells the user that the injectors are being driven, the other two tell the user when extra fuel enrichment is being supplied to compensate for cold engine warm up, and for acceleration, as indicated by a large throttle opening rate.
[0000] 2. Software Description
[0033] A summary of the software flow is provided in FIG. 5 , and a complete listing of the embedded code is provided in FIG. 6 in the form of s-records which can be downloaded into Motorola HC08 series micro controllers through a serial port with commercially available software for this purpose installed on a host computer. As can be seen from the flowchart, the main loop of the program performs calculations on a continuing basis, as long as there are no interrupts. The latter, shown in the right column of FIG. 5 , are used for time critical operations and for a 100 microsecond clock.
[0034] The primary control algorithm, performed in the main loop of the embedded program, is the calculation of injector on time or pulse width. For this simple fuel injection system, the equations used for this have been optimized as follows:
air_density=0.3916*MAP/(MAT+459.7)
mass_air=air_density cylinder_volume
mass fuel=mass air/ AFR
Inj — PW =mass_fuel/ Inj _Flow_Rate
[0035] The injector flow rate is a constant measured at the factory by flowing the injector at the line pressure specified for the car. The fuel required in the above equation depends on the amount (in mass) of air entering the engine and the desired air/fuel ratio (AFR). In the above, air density is in pounds per cubic foot, MAP in kilopascals, MAT is the intake manifold air temperature in degrees Fahrenheit, and the 459.7 converts to degrees Kelvin. The volume of the cylinder is in cubic feet.
[0036] To simplify the calculations required by the microprocessor, one can define a quantity at a specific set of input values. In this system, we define the variable Req_fuel which is the amount of injector open time required for a MAP value of 100 Kpa (essentially wide-open throttle), MAT value of 70 degrees F., and assign values for AFR and cylinder volume which relate to the application. Req_fuel is a constant inside of the program. With this definition, the code is simplified by the use of direct units for the calculations, for example, MAP readings in Kpa/100 can be directly multiplied by Req_fuel to yield the change in pulse width time. Also, quantities, like volumetric efficiency (VE), which is the efficiency of the engine in pumping air at a specific RPM and load, can also be directly multiplied to the Req_fuel value. Likewise, acceleration and warm up enrichment values are directly multiplied in normalized percentages, as well as feedback settings for closed loop operation (02). Lookup tables for percent changes from the defined baseline value for Req_fuel is also used for temperature correction and barometric pressure correction, and are multiplied in a similar manner. This approach is very intuitive for users and yields:
Inj — PW=Req — fuer (MAP/100)*( VE/ 100)*(02/100)*(Warm/100)*( Acce 1/100)*( Baro/ 100)*(Air/100).
[0037] The preceding description covers the basic requirements, but there are several other corrections that need to be made. The first of these is enrichment for a cold start. During the cranking period and for at least a minute or more thereafter, an extremely rich fuel mixture is required for the engine to fire and run properly. How rich depends on the coolant temperature as measured by the coolant sensor. Hence, a user-configurable table is provided in flash memory for fuel enrichment vs temperature, and this is factored into the injector pulse width equation. As the engine warms up, the enrichment tapers off.
[0038] During the cranking phase, more sophisticated strategies employ asynchronous injection, in which the injector is made to pulse several short bursts of fuel rather than a single long shot. This produces better mixing of the fuel and air. This is needed during cranking, because there is very little engine vacuum generated at the slow cranking speeds. Hence, the air moves very slowly through the intake tract and does not mix well with the fuel, thereby producing a weaker and rougher combustion event.
[0039] A second area requiring special enrichment is acceleration. When the throttle is depressed rapidly for acceleration, a very rich mixture is required for a short period to keep the engine, from stumbling. To do this the ECU must first sense that acceleration is occurring. It does this by polling for a TPS and/or MAP sensor rate of change that is above a fixed threshold. When this occurs, the mixture is enriched by an amount, and for a time period, which is a function of the rate of change.
[0040] Another fuel correction commonly used is for barometric pressure. This affects the airflow and air density, and hence the fuel must be corrected to maintain a desired AFR. In the present system the intake MAP reading just before starting the engine is used as the barometric pressure, and a correction table is applied.
[0041] A stoichiometric air/fuel ratio of 14.7 is generally considered optimal for all around driving, economy and emissions, and this is what is strived for in closed loop mode using oxygen sensor feedback. This sensor, as the name implies, sends back to the ECU a voltage proportional to the amount of free oxygen in the exhaust. Too much means a lean mixture requiring more fuel be added; too little, just the opposite. Thus, in closed loop mode a PID loop is used to modify the basic fuel equation so as to maintain a just right fuel mix regardless of the type of gas used or the amount of wear in the engine. This
[0000] mode is used off idle during cruise conditions when such a stoichiometric mixture is desired.
[0042] The fuel injector is a solenoid tied to battery voltage on one end, and is grounded by the ECU at the other end when it is desired to turn on the injector. Now the specification injector flow rate is for steady state conditions, but the injector in the engine is not run at steady state, it is constantly pulsed on and off, and requires about 1-2 ms to fully open, and 1 ms to fully close. (During opening it is fighting spring pressure, while the spring assists in closing.) This fact requires two more corrections for fuel regulation. One is for the fact that the flow rate is not constant during the open/close ramps, and the other is a compensation for battery voltage, which has an effect on the open time. If the battery is weak, the injector will take longer to open. Hence, battery voltage is measured as shown in FIG. 3 , and the injector open time is modified either linearly or from a table according to the deviation of battery voltage from 12 volts.
[0043] A practical feature of the software not directly related to engine control is the provision for a bootloader program. This feature allows corrections and upgrades to the software to be easily downloaded by the users when they are developed. | An electronic engine fuel controller that is simple, low cost, easily installed, and configurable for any internal combustion engine. The system is intended for upgrading older carbureted vehicles or vehicles that have been modified beyond the limits of the OEM controller. It takes advantage of modern microcontroller technology with integrated memory, digital input/output, sensor and timer channels to produce a low parts count, as well as reliable operation in a large variety of vehicles, even when installed by people with little experience or knowledge in this area. Operation is by sensing a tachometer signal from the existing distributor, ignition coil, toothed wheel or similar device that produces one electronic pulse for each cylinder cycle. When a pulse is received, software in the micro measures engine operating parameters, calculates fuel parameters, and fires one or more injectors depending on how the system is configured. Configuration software operating on an external computer or laptop and communicating with the micro allows the user to modify any of the controller parameters or tables used for the fuel calculations. | 5 |
FIELD OF THE INVENTION
This invention is in the field of retrievable attachment of guidelines to undersea oil and gas well equipment.
BACKGROUND
When a subsea well has been drilled, the wellhead is typically terminated in a base or guide template which rests on the ocean floor. It is necessary from time to time to lower equipment from the surface of the ocean to the ocean floor and to attach or mate that equipment to other equipment or fixtures on the base. This requires a means for guiding the equipment being lowered to the vicinity of the base and for accurately aligning that equipment with its mating fixture on the base once it has arrived.
These guidance and alignment functions are served by guidelines which descend from the ocean surface to the tops of guideposts which rise from the base, preferably by being inserted in a guidepost-receptacle on the base designed for the purpose. Typically, the guidepost-receptacle will have an annular depression or groove on its inner surface and the guidepost will have retractable dogs or other locking features protruding from its outer surface. As the guidepost is inserted into the guidepost-receptacle, the retractable dogs snap outward into the groove when the guidepost reaches full insertion. The dogs then act as locking devices to retain the guidepost in the guidepost-receptacle until removal of the guidepost is required.
There are various methods for removal of a guidepost from a guidepost-receptacle for retrieval. The dogs can be retracted by downward force on a component of the guidepost, by frangible devices or by manipulation of the guidepost by a remotely operated vehicle on the ocean floor. Use of force on the top of the guidepost or a component thereof is undesirable because of the tendency to buckle the component, especially if it is very long. This effectively limits the guidepost length in order to prevent buckling. Use of frangible release mechanisms can be unreliable. Manipulation of the base of the guidepost or the guidepost-receptacle by a remotely operated vehicle can be impossible because the areas around the base are not always accessible.
SUMMARY OF THE INVENTION
The latch mechanism of this invention makes possible the release and retrieval of a guidepost from its guidepost-receptacle without applying compressive force to the guidepost or one of its components. This makes possible the use of guideposts of greater length than previously feasible. This latch mechanism also avoids the use of frangible devices and external manipulators when released in its normal mode. Use of this mechanism does not require diver assistance; therefore, it is suitable for deep water applications. Further, the latch mechanism of this invention can utilize a full bore receptacle which avoids lodging of small debris that could prevent latching of the guidepost to the receptacle.
Under normal operating conditions the locking and unlocking of the guidepost within the guidepost-receptacle is accomplished by the action of an inner mandrel within the guidepost as it is brought into or out of bearing with a collet operated snap ring carried by the guidepost.
As long as tension is maintained on the guideline, the mandrel forces the expandable collet outward, which keeps the lower snap ring pushed outward into the receptacle groove, holding the guidepost securely in the receptacle.
Release under normal circumstances is effected by slacking off on the guideline, which drops the inner mandrel in the guidepost, allowing the collet at the lower end of the mandrel to contract, thereby relieving pressure on the lower snap ring. Simultaneously, a shoulder on the upper end of the mandrel drops, allowing a retrieval ring carried by the guidepost to be pushed inward above the shoulder by a drop collar. After slackening of the guideline releases the lower snap ring, and after dropping a drop collar from the surface engages the retrieval ring, resumption of tension on the guideline pulls the mandrel shoulder up against the retrieval ring for pulling the guidepost to the surface. This makes possible the pulling of the guidepost from the receptacle, popping the lower snap ring out of the groove in the receptacle.
Additionally, in the event that the normal mode of release fails, the mandrel has a designed break point which allows the guidepost to be released by pulling on the guideline until the mandrel separates, releasing the collet and lower snap ring. Finally, if the mandrel becomes stuck in the latched position, release pins are provided which can be manipulated by a remotely operated vehicle to forcibly drive the mandrel down, releasing the collet and lower snap ring.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional view of the latch mechanism of the present invention shown in the latched position.
FIG. 2 is a sectional view of the latch mechanism of FIG. 1 shown in the unlatched position.
FIG. 3 is a sectional view of the latch mechanism of FIG. 1 showing the emergency breakpoint of the mandrel.
FIG. 4 is a sectional view of the latch mechanism of FIG. 1 showing operation of the release pins.
DETAILED DESCRIPTION OF THE INVENTION
As shown in FIG. 1, guidepost A comprises a hollow cylindrical guidepost housing 100 which contains an inner mandrel 200 the upper portion of which is joined to a guideline 300. The mandrel 200 can extend out of housing 100 through opening 105 to its point of connection with guideline 300. Alternatively, guideline 300 can be joined to mandrel 200 within housing 100.
The exterior surface of guidepost housing 100 mates with the interior surface of a guidepost-receptacle 400 which is mounted on a base (not shown) on the ocean floor.
The latching and unlatching of guidepost A to guidepost-receptacle 400 is accomplished by the actions of a lower snap ring 120 carried on housing 100 which registers with a locking groove 420 provided on the interior surface of guidepost-receptacle 400. The action of the lower snap ring 120 is controlled through snap ring drive buttons 122 which are operated by an expandable collet 130 which is positioned within housing 100. The operation of the collet 130 is in turn controlled by and dependent upon the positioning of an inner mandrel 200 carried within housing 100 with respect to various bearing surfaces and shoulders provided on the mandrel 200 with respect to and for cooperation with various bearing surfaces and shoulders provided as part of the interior surface structure of housing 100.
Guidepost A thus generally comprises a cylindrical housing 100, an inner mandrel 200, located within housing 100 and joined at its upper end to a guideline 300, and a collet 130 which operates through drive buttons 122 to control a snap ring 120 which is carried in an annular groove 124 provided in the exterior surface of housing 100 at its lower end. The outer perimeter of snap ring 120 has beveled upper and lower edges, giving it a rounded cross-section. Similarly, locking groove 420 has a rounded contour, so snap ring 120 can be pulled free of groove 420 by pulling upward on guidepost A.
Inner mandrel 200 comprises an upper portion 210 and a lower portion 220. The upper portion of mandrel 200 has a shoulder 212 used in retrieval. Guideline 300 is joined to upper portion 210 of mandrel 200 at this point or mandrel upper portion 210 can extend out of housing 100. The lower portion of mandrel 200 is provided with bent post release surface 240, and spring retaining flange 230. Lower portion 220 of mandrel 200 terminates as a frusto-conical surface 222 designed to register with and bear upon a matching frusto-conical surface 132 of collet 130.
As pointed out before, guidepost housing 100 comprises a hollow cylindrical body. The exterior surface of housing 100 is provided with holes for retrieval snap ring drive buttons 162, holes for ROV bent post release drive buttons 182, and annular ridge 140 of larger diameter than the interior diameter of guidepost-receptacle 400 to stop movement of housing 100 into guidepost-receptacle 400 in the event that the locking position is passed during insertion. The interior surface of housing 100 is provided with, at its upper end, emergency removal shoulder 170 upon which the upper end of mandrel 200 will bear for emergency release operation, upper snap ring groove 164, middle snap ring groove 184, guidepost flange 150, and holes for lower snap ring drive buttons 122. Guidepost A, comprising housing 100 and mandrel 200 further comprises a spring retained between guidepost flange 150 and mandrel flange 230. Spring 500 is a coil spring having a total capacity less than the submerged weight of the guidepost housing 100.
Guidepost-receptacle 400 comprises a hollow cylindrical housing the upper end of which flares open to act as funnel 410 to receive and guide the lower end of guidepost housing 100 into the cavity of guidepost-receptacle 400. Annular locking groove 420 on the interior surface of guidepost-receptacle 400 provides a recess into which lower snap ring 120 on the guidepost A can snap, locking guidepost A into guidepost-receptacle 400. The lower snap ring 120 is generally cylindrical with a gap between the ends which provides for the ring to be compressed to an outer diameter which is less than or equal to the interior diameter of the guidepost-receptacle 400.
The snap ring is made of spring steel and in an expanded state is designed to have an outer diameter greater than the interior diameter of guidepost-receptacle 400. The thickness of the snap ring is chosen such that in its expanded state the interior diameter of the snap ring is less than the exterior diameter of the guidepost housing 100. Snap ring 120 is positioned within a lower annular groove 124 provided in the exterior surface of the guidepost housing 100 at its lower end at a position on housing 100 which registers with an annular groove 420 provided in the interior surface of guidepost-receptacle 400 for lock down. Snap ring 120 is thereby carried within the lower groove 124 of housing 100 and securely affixed with housing 100.
Located within the lower housing groove 124 and behind snap ring 120 are a plurality of lower snap ring drive buttons 122 which have extensions 123 which extend into the interior of housing 100 through an opening provided in lower groove 124. A collet 130 is located within housing 100 the drive shoulder 131 of which bears against the extensions 123 of the drive buttons 122.
Guidepost A is held in place in guidepost-receptacle 400 by lower snap ring 120 which is outward biased and sized to fit snugly in a locking groove 420 provided on the interior surface of the guidepost-receptacle 400. Snap ring drive button 122 rests behind snap ring 120 in lower groove 124 and protrudes through to the inside of guidepost 100 where it contacts collet 130. Collet 130 is forced outward by contact at surface 132 with frusto-conical surface 222 on the mandrel lower end 220.
Guidepost A also has retrieval ring 160 and retrieval ring drive button 162 in upper groove 164. Retrieval ring 160 is normally fully seated in upper groove 164 immediately outboard of retrieval shoulder 212 on mandrel upper end 210. Guidepost A also has emergency removal shoulder 170 on its inner surface spaced vertically above retrieval shoulder 212.
The operation of the device of the present invention will now be described. Guidepost A is supported by guideline 300 by means of its attachment at the upper end 210 of mandrel 200, as guidepost A is lowered toward guidepost-receptacle 400 guided by the use of a television camera and maneuvering water jets (not shown). During this lowering step, guidepost A is supported on mandrel 200 by two means. Primarily, the weight of guidepost A is supported by the contact between surface 132 of collet 130 and frusto-conical surface 222 of mandrel lower end 220. Secondarily, a smaller portion of the weight of guidepost A is supported by coil spring 500 between guidepost flange 150 and mandrel flange 230. The total capacity of coil spring 500 is less than the submerged weight of guidepost A, so some portion of the weight is always supported by frusto-conical surface 222, ensuring the outward biasing of lower snap ring 120.
Upon arrival at guidepost-receptacle 400, guidepost lower end 112 is guided into guidepost-receptacle 400 by the help of receptacle funnel 410. Continued lowering of guidepost A into guidepost-receptacle 400 is maintained until lower snap ring 120 rests on receptacle funnel 410. Movement of guidepost A ceases at this point because lower snap ring 120 can not recede into groove 124 until pressure on snap ring driven button 122 is relieved. This is achieved by slackening of guideline 300, which, because of the weight of mandrel 200 and downward force by coil spring 500, allows mandrel 200 to drop in relation to guidepost A.
This relative dropping of mandrel 200 relieves outward pressure on collet 130, allowing it to pivot inward about its lower end 134. This inward flexing of collet 130 relieves outward pressure on snap ring drive button 122 and snap ring 120, allowing them to recede into groove 124 as guidepost A drops into its final position. The lower beveled edge of snap ring 120 causes snap ring 120 to recede into groove 124 as it bears upon funnel 410 under the weight of guidepost A. As snap ring 120 aligns with groove 420 on the inner surface of guidepost-receptacle 400, it snaps outward into groove 420. Any tension on guideline 300 pushes upward and outward on surface 132 of collet 130, increasing the outward force on snap ring 120, holding snap ring 120 securely in groove 420.
During insertion of guidepost A into guidepost-receptacle 400, it is possible that snap ring 120 can pass groove 420 because of lack of contact between collet 130 and snap ring drive button 122. In that event, guidepost A will continue into guidepost-receptacle 400 until annular ridge 140 rests upon funnel 410. Upward tension on guideline 300 will then apply upward and outward force on collet 130 and lift guidepost 100 until snap ring 120 snaps into groove 420.
In order to normally retrieve guidepost A, referring to FIG. 2, drop collar 600 is dropped from the ocean surface along guideline 300 until it rests on the top of guidepost A, and guideline 300 is slackened. Drop collar 600 is of sufficient length and weight to slide over and depress retrieval ring drive button 162 which in turn drives retrieval ring 160 partially out of upper groove 164. Since guideline 300 has been slackened, mandrel 200 has dropped, and retrieval ring 160 protrudes over the perimeter of retrieval shoulder 212.
The aforementioned dropping of mandrel 200 relieves the outward force on collet 130 and snap ring 120, allowing snap ring 120 to be pulled free of guidepost-receptacle groove 420. As tension is applied to guideline 300 to retrieve guidepost A, retrieval shoulder 212 rises into contact with retrieval ring 160 and pushes upward on guidepost A. This causes snap ring 120, because of its rounded cross-section and the rounded contour of groove 420, to pull out of groove 420, freeing guidepost A for retrieval. This upward tension on mandrel 200 causes no outward force on snap ring 120 because the contact between retrieval shoulder 212 and retrieval ring 160 prevents surface 222 of mandrel lower end 220 from contacting surface 132 of collet 130 to force collet 130 outward. Guidepost A rides to the surface on retrieval ring 160 and retrieval shoulder 212.
Rather than using the normal retrieval method described above, emergency retrieval is effected by simply increasing the tension on the guideline. Referring now to FIG. 3, mandrel 200 has a machined surface 242 designed to break at a tensile stress lower than the yield strength of the guideline 300. As tension on guideline 300 is increased to this yield point, mandrel 200 parts at surface 242 and mandrel lower end 220 drops with the assistance of force of spring 500, releasing the outward force on collet 130 and snap ring 120. Simultaneously, mandrel upper end 210 rises until retrieval shoulder 212 contacts emergency removal shoulder 170 on the interior of guidepost housing 100. This applies upward force on guidepost A, pulling snap ring 120 free of guidepost-receptacle groove 420. Guidepost A then rides to the surface on emergency removal shoulder 170.
Finally, if sideways forces are applied to guidepost A sufficient to cause it to bend, mandrel 200 can become stuck and fail to drop when guideline 300 is slackened in preparation for retrieval. Guidepost housing 100 is designed with increased wall thickness below point 190 to insure that any bending will take place high enough not to affect the operation of the lower half of mandrel 200. Bent post release wedges 180 and their associated drive buttons 182 are arranged in middle groove 184 so that the tapered surfaces on the inner ends of wedges 180 align with frusto-conical bent post release surface 240 on mandrel 200. As seen in FIG. 1, in normal latched position, wedges 180 contact surface 240 at its lower, outer edge.
When retrieval of a bent post is required, guideline 300 is slackened. A remotely operated vehicle well known in the trade is positioned near the bent guidepost, and hydraulic tool 700 on the remotely operated vehicle is used to depress wedge drive buttons 182. This drives wedges 180 inward, forcing mandrel 200 downward as wedges 180 slide along surface 240 of mandrel 200. This downward motion of mandrel 200 releases snap ring 120 in the normal fashion. Guidepost A can then be retrieved by use of a drop collar 600 or a drillpipe-mounted overshot (not shown).
The drawings and description given here address a preferred embodiment of this invention. Variations will become obvious to those skilled in the art. To the extent that such variations are equivalent, it is intended that they be encompassed by the following claims. | A subsea guidepost latch mechanism which latches a guidepost to a guidepost-receptacle by means of an external snap ring on the guidepost and an internal groove in the guidepost-receptacle. The snap ring is held in the groove by a collet inside the snap ring which is forced outward by an inner mandrel in the guidepost when upward tension is placed on the mandrel by a guideline. The guidepost is released from the guidepost-receptacle by releasing tension on the guideline which allows the mandrel to drop, releasing outward force on the collet and the snap ring. This allows the snap ring to be pulled out of the guidepost-receptacle groove. | 4 |
BACKGROUND OF THE INVENTION
This invention is directed to the production of six types of inorganic crystalline fibers:
(1) fibers wherein a fluormica constitutes the predominant crystal phase;
(2) fibers wherein a fluoramphibole constitutes the predominant crystal phase;
(3) fibers wherein canasite constitutes the predominant crystal phase;
(4) fibers wherein potassium and/or sodium fluorrichterite constitutes the predominant crystal phase;
(5) fibers wherein fluorapatite constitutes the predominant crystal phase; and
(6) fibers wherein a fluoride-containing, spodumene-type crystal constitutes the predominant crystal phase.
The production of inorganic crystalline articles containing a fluormica as the predominant crystal phase has been the subject of numerous disclosures. To illustrate:
U.S. Pat. No. 3,689,293 describes the preparation of such articles from precursor glass compositions in the R 2 O-MgO-(Al 2 O 3 ,B 2 O 3 )-SiO 2 -F system, wherein R 2 O is an alkali metal oxide. X-ray diffraction analyses identified the basic mica as corresponding to a fluorophlogopite solid solution; that solid solution commonly comprising three components: normal fluorophlogopite, KMg 3 AlSi 3 O 10 F 2 , boron fluorophlogopite, KMg 3 BSi 3 O 10 F 2 , and a subpotassic aluminous phlogopite whose extract composition was unknown but which was thought to approach close to K 0 .8 Mg 2 .9 Al 0 .9 Si 3 .1 O 10 F 2 .
U.S. Pat. No. 3,732,087 is drawn to articles wherein tetrasilicic fluormica crystals constitute the predominant crystal phase. Such articles are prepared by heat treating precursor glass articles having compositions within the (K,Rb,Cs) 2 O-(Sr,Ba,Cd)O-MgO-SiO 2 -F system.
U.S. Pat. No. 3,756,838 is directed to articles wherein an alkali metal-free, alkaline earth metal fluormica constitutes the predominant crystal phase. Such articles are produced by heat treating parent glass articles having compositions in the (Ba,Sr)O-MgO-Al 2 O 3 -SiO 2 -F field.
The formation of inorganic crystalline articles wherein fluoramphibole crystals comprise the predominant crystal phase is disclosed in U.S. Pat. No. 3,839,056. Such articles are prepared by heat treating precursor glass articles having compositions within the (Li,Na) 2 O-(Ca,Mg)O-(Ca,Mg)O-(B,Al) 2 O 3 -SiO 2 -F system. The backbone of the amphibole structure is formed by double silicate chains which are crosslinked alternately by oxygen and fluorine. Each double chain is made up of single chains arranged side-by-side in a herringbone pattern. Fluoramphibole crystals can have a fibrous or needle-like habit. The growth of such crystals in situ in glass articles can yield a fiber-containing matrix wherein the fibers are undamaged and, therefore, extremely strong. X-ray diffraction studies evidenced three different types of fluoramphibole crystal structures; viz., fluorrichterite, Na 2 CaMg 5 Si 8 O 22 F 2 , fluormagnesiorichterite, Na 2 Mg 6 Si 8 O 22 F 2 , and lithium-containing proto-amphibole, LiMg 6 .5 Si 8 O 22 F 2 .
The production of inorganic crystalline articles containing canasite as the predominant crystal phase is described in U.S. Pat. No. 4,386,162. The crystals grown in situ through the heat treatment of parent glass bodies are conjectured as having the formula Ca 5 Na 4 K 2 [Si 12 O 30 ]F 4 with probable solid solution to Ca 5 Na 3 K 3 [Si 12 O 30 ]F 4 . As is explained there, canasite consists of a multiple chain silicate demonstrating an anisotropic blade-like crystal habit. Electron microscopy and x-ray diffraction studies have indicated that, structurally, canasite crystals are composed of parallel silicate chains crosslinked to make a long, box-like backbone in which the potassium ions rest. Those complex chain units are crosslinked into groups of four and are separated by networks composed primarily of Na(O,F) 6 and Ca(O,F) 6 octahedra. That characteristic interlocking chain silicate structure has yielded articles exhibiting moduli of rupture in excess of 50,000 psi and exceptional toughness, i.e., resistance to impact.
Inorganic crystalline articles containing potassium fluorrichterite as the predominant crystal phase are disclosed in U.S. Pat. No. 4,467,039. Potassium ions are substituted in part for sodium ions in the fluorrichterite structure, resulting in crystals having the formula KNaCaMg 5 Si 8 O 22 F 2 . The habit of those crystals is strongly anisotropic and predominantly unidimensional. Fundamentally, the crystals consist of polymer chain silicates in which double or higher order multiple chains form the backbone.
Because the substance of animal and human bones consists essentially of hydroxyapatite, Ca 5 OH(PO 4 ) 3 , which is permeated in an intimate mixture of albuminoids (collagen), considerable research has been undertaken to synthesize the mineral hydroxyapatite and its fluoride-containing analog, Ca 5 F(PO 4 ) 3 , for use as bone implant and bone replacement materials. U.S. Pat. Nos. 3,922,155, 4,120,730, and 4,131,597 are illustrative of the research which has been directed to the production of glass-ceramic materials containing fluorapatite at the predominant crystal phase.
Inorganic crystalline articles containing spodumene (classic formula Li 2 O:Al 2 O 3 :4SiO 2 ) as the predominant crystal phase have been extensively marketed, principally because of their low coefficient of thermal expansion and their relatively high refractoriness. Such articles were first described in U.S. Pat. No. 2,920,971, and have been the subject of numerous subsequent patents.
SUMMARY OF THE INVENTION
The primary objective of the instant invention is to prepare inorganic crystalline fibers having compositions hitherto unknown in the field of such fibers, and to provide a novel method for synthesizing such fibers. Thus, six distinctive types of inorganic crystalline fibers have been produced wherein the predominant crystal phase developed is one of the following: (1) a fluormica selected from the group of normal fluorophlogopite, boron fluorophlogopite, subpotassic aluminous phlogopite, tetrasilicic fluormica, and an alkali metal-free, alkaline earth metal fluormica; (2) a fluoramphibole selected from the group of fluorrichterite, fluor-magnesio-richterite, and lithium-containing proto-amphibole; (3) canasite; (4) potassium and/or sodium fluorrichterite; (5) fluorapatite; and (6) a spodumene solid solution-type crystal containing fluoride. Each of those fibers is prepared from base compositions having the stoichiometry of or in the near vicinity of the stoichiometry of the particular crystal phase desired into which MoO 3 and/or WO 3 and/or As 2 O 3 are incorporated within about 0.5-5% by weight total, and wherein the original batch contains fluoride within about 15-60 mole percent excess of that required stoichiometrically to form the desired crystal. A minor amount of MoO 3 and/or WO 3 and/or As 2 O 3 is present in the fibers. It must be noted that the action of As 2 O 3 in developing fiber growth is much less dramatic than that of MoO 3 or WO 3 . Higher concentrations of As 2 O 3 (˜ 3-5%) are generally required to grow crystalline fibers. Therefore, MoO 3 and WO 3 are the preferred agents to obtain the desired crystalline fibers.
Three general processes have been devised to prepare the desired fibers:
(A) batches are melted, the melt cooled to a temperature below the transformation range thereof and simultaneously shaped into a body of a desired geometry, and the body heated in a closed container at a temperature within the range of about 800°-1000° C. for a period of time sufficient to grow fibers projecting from the surface of the body;
(B) batches free from MoO 3 and/or WO 3 and/or As 2 O 3 are melted, the melt cooled to a temperature below the transformation range thereof and simultaneously shaped into a body of a desired geometry, the body comminuted to finely-divided particles, the particles mixed with finely-divided particles of MoO 3 and/or WO 3 and/or As 2 O 3 , and that mixture heated in a closed container at a temperature within the range of about 800°-1000° C. for a period of time sufficient to grow fibers projecting from the surface of the particles; and
(C) batch materials in finely-divided particulate form corresponding to or closely approximating the stoichiometry of the desired crystalline fibers and including appropriate amounts of MoO 3 and/or WO 3 and/or As 2 O 3 and fluoride are mixed together, that mixture is formed into a body of a desired configuration, and that body is fired in a closed container at about 800°-1000° C. for a period of time sufficient to grow fibers projecting from the surface of the body.
Inasmuch as the growth of the fibers takes place on the surface of the precursor bodies, it will be appreciated that increasing the surface area available for fiber growth leads to increased fiber production. Consequently, the precursor body will customarily be fired in the form of finely-divided particles to effect the greatest yield of fibers. One efficient method for producing such particles without extensive crushing, pulverizing, etc., involves the well-known practice of "drigaging"; i.e., the melt is run as a stream into cold water. Of course, the resulting particles can be comminuted still further, if desired. Another method for increasing the fiber production involves the heat treatment of the precursor body in the form of plates of large area, but of relatively thin thickness dimension (˜0.25"-0.5").
Although the mechanism of fiber growth has not been fully elucidated, because the fibers grow well in covered containers, but not in open containers, and because the addition of MoO 3 and fluoride to MoO 3 -free compositions, while heat treating such compositions, gives rise to fiber production, it has been theorized that the fibers are produced through a combination bulk diffusion and vapor deposition process wherein MoO 2 F 2 acts as a growth promoter. That theory is further supported by the high temperature mass spectrometric identification of the moiety Mo 2 F 2 in the vapor species evolved from the compositions being heat treated to yield fluormica and fluorapatite fibers. Further, a comparison of chemical analyses of those fibers with the parent body has shown a content of MoO 3 in the crystalline fibers; that factor also strongly suggesting that molybdenum promotes and participates in the structural growth of fibers and that it is delivered via the gaseous phase.
Whereas the function of WO 3 has not been studied as extensively as that of MoO 3 , because the growth of fibers requires the presence of WO 3 and fluoride, coupled with heat treatment in a closed container and the identification of a WO 2 F 2 moiety in the vapor species, it is postulated that a like mechanism is involved in its action in producing the desired crystalline fibers.
Again, the operation of As 2 O 3 in sponsoring the growth of fibers has not been analyzed in substantial detail. Nevertheless, because the growth of fibers requires the presence of As 2 O 3 and fluoride, coupled with heat treatment in a closed container, plus the fact that AsF 3 and AsF 5 have been identified in the vapor phase, it has been hypothesized that a similar solid state diffusion/vapor deposition mechanism is also operative here.
The fiber growth commonly takes on the appearance of a dense mat of fibers projecting from the surface of a body; the diameters of the fibers ranging within about 0.5-10 microns, the lengths thereof ranging up to about one inch (2.54 cm), and the aspect ratios thereof ranging up to and in excess of 1000 to 1.
PRIOR ART
U.S. Pat. No. 3,464,836 discloses the production of fibers containing at least 15% by weight BaO and at least 50% by weight of a crystal phase selected from the group of spodumene, jadeite (Na 2 O:Al 2 O 3 :4SiO 2 ), and benitoite (BaO:TiO 2 :3SiO 2 ). MoO 3 , WO 3 , As 2 O 3 , and fluoride are nowhere referred to in the patent. Because of the absence of any reference to fluoride, a fluoride-containing spodumene could not have been prepared.
U.S. Pat. No. 4,484,950 describes the formation of fibers selected from the group of calcium metaphosphate, calcium sodium phosphate, and calcium lithium phosphate, MoO 3 , WO 3 , As 2 O 3 , fluoride, and apatite crystals are nowhere mentioned in the patent.
U.S. Pat. No. 4,503,157 is directed to the preparation of sintered composite bodies consisting of mineral fibers entrained within an apatite matrix. The apatite body is produced by hot pressing powders of apatite (fluorapatite is mentioned as a starting material) to sinter the apatite material into a unitary body. No reference is made to MoO 3 , WO 3 or As 2 O 3 . Where a fiber reinforced article is desired, the fibers are mixed into the apatite powder and that mixture sintered together through hot pressing.
British Patent No. 972,541 is drawn to the hydrothermal production of fibers having the general formula Na x H y M z (Si 4 O 11 ) 2 (OH) m F n , wherein M is at least one metal selected from the group of Co, Mg, and Ni, x is 1.5-3, y is 0.2-2, z is 5-6, m is 0-2, n is 0-2, n+m=2, and x+y=14. MoO 3 , WO 3 , and As 2 O 3 are nowhere mentioned and the products of the patent have compositions outside of those of the present invention.
British Patent No. 1,415,628 specifically discusses the formation of fibers wherein the crystal phase is β-eucryptite or β-spodumene. The patent also alludes to the preparation of fibers containing crystals of cordierite, mullite, spinel, corundum, nepheline, anorthite, forsterite, or albite, but no working examples in support thereof are provided. NaF and CaF 2 are referred to as possible nucleating agents, but there is no suggestion that the crystals contained fluoride. Moreover, neither MoO 3 , WO 3 , nor As 2 O 3 is mentioned and there is no requirement of firing the precursor body in a closed container.
DESCRIPTION OF PREFERRED EMBODIMENTS
Whereas the following discussion involved laboratory work, it will be appreciated that the inventive method can be scaled up to commercial practice.
Fluormica Fibers
Table I records a number of compositions illustrating the capability of the present invention for producing inorganic crystalline fibers containing fluormica as the predominant crystal phase. The compositions are tabulated in terms of mole percent on the oxide basis except for the concentrations of MoO 3 , WO 3 , As 2 O 3 , V 2 O 5 , Cr 2 O 3 , MnO 2 , ZnO, NiO, and Co 2 O 3 , which are reported in terms of weight percent in addition to the base composition. Because it is not known with which cation(s) the fluoride is combined, it is merely listed in terms of F and the oxygen=fluorine correction factor entered in accordance with conventional analysis practice. The actual batch ingredients may comprise any materials, either oxides or other compounds, which, when melted together, will be converted into the desired oxide in the proper proportion. In the compositions of Table I, an alkaline earth metal fluoride and/or an alkali metal silicofluoride customarily provided the source of fluoride.
The batch constituents were compounded, mixed together in a tumble mill, and the mixtures charged into platinum or silica crucibles. (Fiber yield did not appear to be influenced by the type of crucible.) Lids were placed onto the crucibles and the crucibles then introduced into an electrically-fired furnace operating at about 1400°-1500° C. After about 3-4 hours the melts were either drigaged by running into a bath of cold tap water or cast into steel molds to produce glass slabs of various sizes up to 14" squares with a thickness of 1". To reduce the extent of fluoride volatilization, the slabs were not annealed. Before heat treating those slabs, a 0.25" surface layer was removed therefrom in order to expose the fluoride-rich interior of the slabs.
TABLE I 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 SiO.sub.2 42.0 42.0 42.0 42.0 42.0 42.0 42.0 42.0 42.9 42.9 42.9 42.9 42.9 42.9 42.9 42.9 42.9 42.0 42.0 42.0 42.0 42.0 MgO 29.4 29.4 29.4 29.4 29.4 29.4 29.4 29.4 31.3 31.3 31.3 31.3 31.3 31.3 31.3 31.3 31.3 29.4 29.4 29.4 29.4 29.4 Na.sub.2 O 4.0 4.0 4.0 4.0 4.0 4.0 4.0 4.0 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.0 4.0 4.0 4.0 4.0 K.sub.2 O 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 CaO 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 -- -- -- -- -- MnO.sub.2 ZnO NiO Co.sub.2 O.sub.3 SrO BaO Al.sub.2 O.sub.3 B.sub.2 O.sub.3 Li.sub.2 O F 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 103.4 103.4 103.4 103.4 103.4 103.4 103.4 103.4 107.21 107.21 107.21 107.21 107.21 107.21 107.21 107.21 107.21 103.4 103.4 103.4 103.4 103.4 O = F -3.4 -3.4 -3.4 -3.4 -3.4 -3.4 -3.4 -3.4 -7.21 -7.21 -7.21 -7.21 -7.21 -7.21 -7.21 -7.21 -7.21 -3.4 -3.4 -3.4 -3.4 -3.4 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 MoO.sub.3 -- 0.5 1.0 1.5 2.0 2.5 3.0 4.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 -- -- -- -- -- WO.sub.3 -- 1.0 2.0 3.0 -- -- V.sub.2 O.sub.5 -- -- -- -- 1.0 2.0 Cr.sub.2 O.sub.3 -- -- -- -- -- -- As.sub.2 O.sub.3 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 SiO.sub.2 42.0 42.0 42.0 42.0 42.9 42.9 42.9 42.9 42.9 42.9 42.9 42.9 42.9 42.9 42.9 42.9 4.29 42.9 42.9 42.9 42.9 42.9 MgO 29.4 29.4 29.4 29.4 31.3 31.3 31.3 31.3 31.3 31.3 31.3 31.3 31.3 29.0 29.0 29.0 29.0 29.0 29.0 29.0 29.0 26.3 Na.sub.2 O 4.0 4.0 4.0 4.0 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 4.3 K.sub.2 O 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.01.0 1.01.0 1.01.0 1.0 1.0 1.0 1.0 CaO -- -- -- -- 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 0.71 MnO.sub.2 -- -- -- 2.27 2.27 -- -- -- ZnO -- -- -- -- -- 2.27 2.27 -- NiO -- -- -- -- -- -- -- 2.27 2.27 -- -- -- Co.sub.2 O.sub.3 -- 2.27 2.27 -- SrO -- -- -- 5.0 BaO -- -- -- -- Al.sub.2 O.sub.3 B.sub.2 O.sub.3 Li.sub.2 O F 27.0 27.0 27.0 27.0 27.0 27.0 27.027.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 28.0 103.4 103.4 103.4 103.4 107.21 107.21 107.21 107.21 107.21 107.21 107.21 107.21 107.21 107.18 107.18 107.18 107.18 107.18 107.18 107.18 107.18 108.21 O = F -3.4 -3.4 -3.4 -3.4 -7.21 -7.21 -7.21 -7.21 -7.21 - 7.21 -7.21 -7.21 -7.21 -7.18 -7.18 -7.18 -7.18 -7.18 -7.18 -7.18 -7.18 -8.21 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 MoO.sub.3 -- -- -- -- -- 2.0 -- 2.0 -- 2.0 -- 2.0 -- 2.5 WO.sub.3 -- -- -- -- 1.5 3.0 4.0 -- -- -- V.sub.2 O.sub.5 3.0 -- -- -- -- -- -- 1.5 3.0 4.0 Cr.sub.2 O.sub.3 -- 1.0 2.0 3.0 -- -- -- -- -- -- As.sub.2 O.sub.3 45 46 47 48 49 50 51 52 53 5 4 55 56 57 58 59 60 61 62 SiO.sub.2 42.9 42.9 42.9 42.9 42.9 42.9 41.0 40.0 42.0 42.0 42.0 41.5 40.0 42.9 42.9 42.9 42.9 42.9 MgO 21.3 26.3 21.3 -- -- 21.3 29.4 29.4 29.4 29.4 29.4 29.4 29.4 31.3 31.3 31.3 31.3 31.3 Na.sub.2 O 4.3 4.3 4.3 4.3 4.3 4.3 4.0 4.0 -- 2.0 4.0 4.0 4.0 4.3 4.3 4.3 4.3 4.3 K.sub.2 O 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 -- 1.0 1.0 1.0 1.0 1.0 1.0 1.0 CaO 0.71 0.71 0.71 0.71 0.71 0.71 -- -- -- -- -- 0.5 0 0.71 0.71 0.71 0.71 0.71 MnO.sub.2 ZnO NiO -- -- -- -- Co.sub.2 O.sub.3-- -- -- -- SrO 10.0 -- -- 31.3 -- 5.0 -- -- -- -- -- -- BaO -- 5.0 10.0 -- 31.3 5.0 -- -- -- -- -- -- Al.sub.2 O.sub.3 -- -- 1.0 -- -- -- -- -- 2.0 -- -- -- -- -- B.sub.2 O.sub.3 -- -- -- 2.0 -- -- -- -- 1.0 -- -- -- -- -- Li.sub.2 O -- -- -- -- 4.0 2.0 1.0 -- F 28.0 28.0 28.0 28.0 28.0 28.0 27.0 27.0 27.0 27.0 27.0 27.0 27.0 30.0 30.0 30.0 30.0 30.0 108.21 108.21 108.21 108.21 108.21 108.21 103.4 103.4 103.4 103.4 103.4 103.4 103.4 110.21 110.21 110.21 110.21 110.21 O = F -8.21 -8.21 -8.21 -8.21 -8.21 -8.21 -3.4 -3.4 -3.4 -3.4 -3.4 -3.4 -3.4 -10.21 -10.21 -10.21 -10.21 -10.21 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 MoO.sub.3 2.5 2.5 2.5 2.5 2.5 2.5 2.0 2.0 2.0 2.0 2.0 2.0 2.0 -- -- -- -- -- WO.sub.3 V.sub.2 O.sub.5 Cr.sub.2 O.sub.3 As.sub.2 O.sub.3 -- 0.5 1.0 3.0 4.0 5.0
The glass samples were charged into glazed porcelain crucibles, covers placed thereupon, and the crucibles then introduced into an electrically-heated furnace. The temperature within the furnace was raised at a rate of about ˜250° C./hour to a temperature suitable for inducing the desired growth of fibers, generally about 900°-990° C., and the temperature was maintained within that range for a sufficient length of time to achieve a substantial growth of fibers. Thereafter, the electric current to the furnace was cut off and the furnace allowed to cool with the crucibles retained therewithin. This latter procedure, termed "cooling at furnace rate", is simply a convenient practice which has no substantive effect upon the crystalline products. Likewise, the heating rate is not critical; much faster or slower rates would be equally useful. Finally, whereas specific dwell periods at individual temperatures were employed, that practice is, again, merely a matter of convenience. The temperature may be permitted to vary within the effective range for growing fibers.
Table II reports the heat treatment applied to each of the glass compositions contained within covered glazed porcelain crucibles, along with a visual appraisal of fiber growth. X-ray diffraction analyses of the fibers indicated a micaceous structure.
TABLE II______________________________________Example No. Heat Treatment Visual Description______________________________________ 1 968° C.-8 hours None 2 " Microscopic-sized 3 " Very slight 4 " Slight 5 " Good* 6 " Good* 7 " Moderate 8 " None 9 " Slight10 " Better than 911 " Good*12 " Good*13 " Good*14 " Good*15 " Good*16 " Excellent**17 " Excellent**18 " None19 " None20 " None21 " None22 " None23 " None24 " None25 " None26 " None27 " Slight28 " Better than 2729 " Good*30 " Microscopic-sized31 " "32 " "33 " "34 " "35 " "36 980° C.-10 hours None37 " None38 " None39 " None40 " None41 " None42 " None43 " None44 " None45 " None46 " None47 " None48 " None49 " None50 " None51 " None52 " None53 " None54 " None55 " None56 " None57 " None58 950° C.-2 hours None59 " None60 " Slight61 " Good*62 " Good*______________________________________ *Good indicates dense surface mat with fibers of 0.125"-0.25" length **Excellent indicates dense surface mat with fibers of >0.25" length
Table III records wet chemical analyses (weight percent) of the batch for Example 5, of the glass produced from melting the batch, and of the crystallized fibers derived by firing drigaged particles of the glass at 968° C. for 8 hours. The CaO is an impurity in the MgCO 3 batch material.
TABLE III______________________________________ Batch Glass Fibers______________________________________SiO.sub.2 55.2 57.3 56.3MgO 25.9 27.2 27.5Na.sub.2 O 5.7 6.11 5.82K.sub.2 O 2.1 2.46 1.96CaO 0.25 0.30 0.87F 11.2 10.7 7.96MoO.sub.3 2.0 1.92 1.73______________________________________
It is believed significant that the content of MgO in the glass and in the fibers is virtually the same, thereby indicating easy diffusion of Mg +2 ions from the glass to the fiber. No magnesium-containing species was detected in the vapor phase at the growth temperature. This phenomenon is deemed surprising in view of the decreased contents of Na + and K + in the fibers when compared to the glass, since each of those ionic species would be expected to have a greater ion diffusion content than that of Mg +2 . The Ca +2 ions also appear to diffuse preferentially to the fiber; the CaO content of the fiber is almost three times that of the glass on a weight basis (2.5 times on a molar basis). No species containing Ca +2 ions has been detected in the vapor phase. The fluoride content of the glass indicates remarkably little loss thereof during melting; the fluoride content of the fibers is about 75% of that in the glass.
The Examples recited in Table I, coupled with the fiber growth descriptions in Table II, indicate that, whereas the base glass composition approximates the stoichiometry of a fluormica, a higher MgO content appears to induce a greater fiber yield. This circumstance is of special interest with regard to WO 3 . Hence, Examples 18-20 evidenced no fiber formation; Examples 27-29 (higher MgO contents) exhibited fiber growth.
V 2 O 5 and Cr 2 O 3 were not effective in inducing substantial yields of fiber. Substitutions of MnO 2 , ZnO, NiO, and Co 2 O 3 for MgO in the higher MgO base compositions, as summarized in Examples 36-43, eliminated the growth of fibers with or without the inclusion of MoO 3 . Likewise, the substitution of SrO and BaO for MgO prevented the growth of fibers even in the presence of MoO 3 (Examples 44-50). The various substitutions of Al 2 O 3 , B 2 O 3 , Li 2 O, and CaO for SiO 2 , as exemplified in Examples 51-57, resulted in no substantial growth of fibers. Such findings indicate the need to maintain the base composition close to the stoichiometry of fluormica to insure good fiber yield.
As can be observed in Examples 58-62, As 2 O 3 promotes the growth of fibers when in concentrations of at least about 3% by weight.
Fluoramphibole Fibers
Table IV reports a number of compositions which, upon heat treatment, will yield fibers containing a fluoramphibole as the predominant crystal phase. The compositions are recorded in terms of weight percent on the oxide basis. Because it is not known with which cation(s) the fluoride is combined, it is simply tabulated as F and the oxygen=fluorine correction factor recited in accordance with conventional analysis practice. The actual batch ingredients may constitute any materials, either oxides or other compounds, which, when melted together, will be converted into the desired oxide in the proper proportions. In the compositions of Table IV, an alkaline earth metal fluoride and/or an alkali metal silicofluoride customarily comprised the source of fluoride.
The batch components were compounded, mixed together in a tumble mill, and those mixtures run into platinum or silica crucibles. Lids were placed onto the crucibles and the crucibles moved into an electrically-heated furnace operating at about 1400° C.-1500° C. After about 3-4 hours the melts were either drigaged or cast into steel molds similarly to the laboratory examples reported in Table I.
TABLE IV______________________________________63 64 65 66 67 68 69______________________________________SiO.sub.2 55.9 51.3 48.7 53.8 53.2 53.2 54.8MgO 26.2 25.8 25.5 24.5 24.2 24.1 26.8K.sub.2 O 2.0 4.0 3.9 -- -- -- 2.0Li.sub.2 O 3.6 -- -- -- -- -- --CaO 0.86 0.3 0.3 -- -- -- 0.75Na.sub.2 O -- 5.3 5.2 9.3 9.2 9.1 5.7Al.sub.2 O.sub.3 -- 1.1 4.3 1.1 2.2 3.2 --F 11.5 12.2 12.0 11.4 11.2 11.2 10.8MoO.sub.3 3.0 2.0 2.0 2.5 2.5 2.5 3.0 103.06 102.0 101.9 102.6 102.5 103.3 103.85O = F -3.06 -2.0 -1.9 -2.6 -2.5 -3.3 -3.85 100.0 100.0 100.0 100.0 100.0 100.0 100.0______________________________________
In like manner to the glasses of Examples 1-62, except that covered platinum crucibles were used instead of glazed procelain crucibles, the samples were heat treated in an electrically-fired furnace. In general, the heat treatment will be carried out at temperatures ranging from about 950°-1000° C., preferably at least 970° C. Hence, it has been observed that some glass compositions will yield fibers of fluormica at temperatures in the range of about 950°-970° C., but fibers of fluoramphibole at temperatures higher than 970° C. Again, the furnace was heated at a rate of about ˜250° C./hour and permitted to cool to room temperature at furnace rate with the samples retained therewithin.
Table V records the heat treatment to which each sample was exposed and a visual description of the fibrous growth, along with an identification of the crystal phases present as determined through X-ray diffraction analysis. Fluormica was observed to be present as a secondary phase in several of the specimens. "Good" fiber growth indicates a dense surface mat of fibers having lengths of about 0.125-0.25". "Fair" fiber growth signifies sparse surface coverage of fibers of about the same length.
TABLE V______________________________________Example Heat Visual CrystalNo. Treatment Description Phases______________________________________63 970° C. for Fair Fluoramphibole 18 hours64 970° C. for Good Fluoramphibole + 18 hours Fluormica65 970° C. for Good Fluoramphibole + 18 hours Fluormica66 970° C. for Good Fluoramphibole + 18 hours Fluormica67 970° C. for Good Fluoramphibole + 18 hours Fluormica68 970° C. for Good Fluoramphibole + 18 hours Fluormica69 970° C. for Good Fluoramphibole 18 hours______________________________________
Example 63 illustrates that Li 2 O may be substituted for Na 2 O, but fiber production is reduced thereby. However, that substitution eliminates the growth of fluormica crystals. Examples 66-69 point out that the presence of K 2 O is not necessary for fiber generation. Finally, Example 69 indicates that higher firing temperatures promote the growth of fluoramphibole crystals at the expense of fluormica.
Canasite Fibers
Table VI lists a number of compositions in terms of mole percent on the oxide basis, except for the concentrations of MoO 3 which are reported in terms of weight percent in addition to the base composition, which, upon heat treatment, will yield fibers containing canasite as the predominant crystal phase. Because it is not known with which cation(s) the fluoride is combined, it is merely reported as F and the oxygen=fluorine correction factor tabulated in accordance with conventional analysis practice. The actual batch ingredients may be any materials, either oxides or other components, which, when melted together, will be converted into the desired oxide in the proper proportions. In the compositions of Table VI, an alkaline earth metal fluoride and/or an alkali metal silicofluoride customarily provided the source of fluoride.
The batch constituents were compounded, mixed together in a tumble mill, and those mixtures charged into platinum or silica crucibles. After placing lids thereon, the crucibles were introduced into an electrically-fired furnace operating at about 1400°-1500° C. and maintained therewithin for about 3-4 hours. Thereafter, the resulting melts were either drigaged or cast into steel molds in like manner to Examples 1-62 described above.
TABLE VI__________________________________________________________________________70 71 72 73 74 75 76 77 78 79 80 81 82 83 84__________________________________________________________________________SiO.sub.2 55.7 55.7 55.7 55.7 53.7 55.7 55.7 53.7 55.7 55.7 53.7 51.7 55.7 55.7 55.7CaO 21.6 21.6 21.6 21.6 23.6 21.6 21.6 21.6 21.6 21.6 21.6 21.0 21.6 21.6 21.6Na.sub.2 O 9.6 9.6 11.6 7.6 9.6 8.6 9.6 10.6 8.5 12.9 9.6 10.6 8.5 5.6 12.9K.sub.2 O 7.3 7.3 5.3 9.3 7.3 6.3 7.3 8.3 8.5 4.0 9.3 10.3 8.5 11.3 4.0F 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 35.0 129.2 129.2 129.2 129.2 129.2 129.2 129.2 129.2 129.3 129.2 129.2 129.6 129.3 129.2 129.20=F 29.2 29.2 29.2 29.2 29.2 29.2 29.2 29.2 -29.3 -29.2 -29.2 -29.6 -29.3 -29.2 -29.2 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0MoO.sub.3 -- 2.0 2.0 2.0 2.0 2.0 4.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0__________________________________________________________________________
Table VII records another group of glass compositions which, when heat treated, will produce fibers containing canasite as the predominant crystal phase. The compositions are tabulated in terms of weight percent on the oxide basis. The batch ingredients were compounded, mixed together, and melted in like manner to Examples 70-84 above.
TABLE VII______________________________________85 86 87 88 89 90 91______________________________________SiO.sub.2 46.5 46.2 46.5 46.1 45.9 45.7 45.9CaO 18.1 18.0 18.1 18.0 17.9 17.8 17.4Na.sub.2 O 9.8 9.8 9.8 9.7 9.7 9.7 9.7K.sub.2 O 14.5 14.5 14.5 14.4 14.4 14.4 14.4F 11.1 11.6 11.1 11.8 12.1 12.6 12.2MoO.sub.3 2.5 2.5 3.5 2.5 3.5 2.5 2.5 102.5 102.6 103.5 102.5 103.5 102.7 102.1O = F 2.5 -2.6 -3.5 -2.5 -3.5 -2.7 -2.1 100.0 100.0 100.0 100.0 100.0 100.0 100.0______________________________________
The glass samples were loaded into platinum crucibles, lids placed thereon, and the crucibles moved into an electrically-heated furnace. In like manner to Examples 1-84 above, the temperature of the furnace was raised at about ˜250° C./hour to the value reported in Table VIII. After being held at that temperature for the period of time also recorded in Table VIII, the crucibles were cooled to room temperature at furnace rate. In general, the temperature to produce the desired fibers will range between 800°-950° C., temperatures above 825° C. being preferred.
It was observed that fiber growth is independent not only upon composition, but also upon the temperature and time period of heat treatment; i.e., high temperatures and/or longer periods of heat treatment yield fibers of greater length.
Table VIII lists the heat treatment applied to each sample and a visual description of the product resulting therefrom. "Superior" indicates a dense surface covering of fibers having lengths of about 0.5-0.75" with diameters between about 5-15 microns; "Excellent" signifies a dense surface covering of fibers exhibiting lengths of about 0.5"; "Good" designates a dense surface covering of fibers exhibiting lengths up to about 0.25"; "Fair" defines a rather sparse surface covering of fibers with lengths up to 0.5"; "Poor" refers to a sparse surface covering of fibers having lengths up to 0.25". X-ray diffraction analyses identified the canasite structure.
TABLE VIII______________________________________Example No. Heat Treatment Visual Description______________________________________70 910° C. for 12 hours None71 " Good72 " "73 " "74 " "75 " "76 " "77 " "78 " "79 " Poor, glass softened80 " None, glass melted81 875° C. for 48 hours Fair82 860° C. for 45 hours Good83 " "84 " "85 840° C. for 48 hours Excellent86 " "87 " "88 " Superior89 " Fair90 " "91 " Poor______________________________________
As was observed above with respect to fluormica and fluoramphibole glass compositions, no fiber growth was experienced when the glass samples were heat treated in open crucibles. That circumstance confirms the importance of maintaining an appropriate gaseous fluoride atmosphere and supports the proposed mechanism of fiber growth being based partially upon gaseous diffusion.
Potassium and/or Sodium Fluorrichterite Fibers
Table IX recites a group of compositions, tabulated in terms of mole percent on the oxide basis, which, when heat treated in a particular manner, will produce fibers containing potassium and/or sodium fluorrichterite as the predominant crystal phase. The MoO 3 , WO 3 , and As 2 O 3 contents are expressed in terms of weight percent in excess of the phase composition. Inasmuch as it is not known with which cation(s) the fluoride is combined, it is simply recorded in terms of F and the oxygen=fluorine correction factor entered in accordance with conventional analysis practice. The actual batch ingredients may be any materials, either oxides or other compounds, which, when melted together, will be converted into the desired oxide in the proper proportions. In the glasses of Table VIII, an alkaline earth metal fluoride and/or an alkali metal silicofluoride customarily furnished the source of the oxide.
The batch ingredients were compounded, mixed together in a tumble mill, and those mixtures run into platinum or silica crucibles. Covers were placed onto the crucibles and the crucibles were moved into an electrically-fired furnace operating at about 1400°-1500° C. After a residence time of about 3-4 hours, the resulting melts were either drigaged or poured into steel molds, as described above with respect to Examples 1-91.
TABLE IX__________________________________________________________________________92 93 94 95 96 97 98 99 100 101 102 103 104__________________________________________________________________________SiO.sub.253.33 53.33 53.33 53.33 53.33 53.33 53.33 53.33 53.33 53.33 53.33 53.33 53.33Na.sub.2 O6.67 6.67 6.67 6.67 6.67 6.67 6.67 -- 2.00 -- -- -- --K.sub.2 O 6.67 4.67 6.67 6.67 6.67 6.67CaO 6.67 6.67 6.67 6.67 6.67 -- -- 6.67 6.67 6.67 6.67 -- --MgO 33.33 33.33 33.33 33.33 33.33 33.33 33.33 33.33 33.33 33.33 33.33 33.33 26.63SrO -- -- -- -- -- 6.67 --BaO -- -- -- -- -- -- 6.67ZnO -- -- -- -- 6.67 13.33F 30.0 30.0 30.0 30.0 30.0 30.0 30.0 30.0 30.0 30.0 30.0 30.0 30.0130.0 130.0 130.0 130.0 130.0 130.0 130.0 130.0 130.0 130.0 130.0 130.0 130.0O = F-30.0 -30.0 -30.0 -30.0 -30.0 -30.0 -30.0 -30.0 -30.0 -30.0 -30.0 -30.0 -30.0100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0MoO.sub.3-- 3.2 1.98 5.05 1.0 1.99 2.1 2.0 2.1 -- -- 2.6 2.6WO.sub.3 -- -- 3.2 -- -- --As.sub.2 O.sub.3 -- -- -- 4.1 -- --__________________________________________________________________________
Following the practice described above with respect to Examples 1-91, the glasses of Table IX were placed in covered silica crucibles and heat treated in an electrically-fired furnace. In general, heat treating temperatures of about 825°-900° C. will be required to generate the desired fluorrichterite-containing fibers, with temperatures between about 840°-875° C. being preferred. Once again, the furnace was heated at a rate of about ˜250° C./hour and permitted to cool to room temperature at furnace rate.
Table X lists the heat treatment to which each sample was subjected and a visual description of the fibrous growth; X-ray diffraction analyses identified potassium or sodium fluorrichterite as the predominant crystal phase in each.
TABLE X______________________________________Example Heat Treatment Visual Description______________________________________92 850° C. for 24 hours None93 " Dense growth*93 " Medium growth, some glass fusion94 900° C. for 24 hours Medium growth95 850° C. for 24 hours Dense growth96 " Microscopic growth97 " Medium-fair growth98 " Medium-fair growth99 " Dense growth99 900° C. for 24 hours Dense growth, some glass fusion99 820° C. for 24 hours Microscopic growth99 800° C. for 12 hours None100 850° C. for 12 hours Dense growth101 850° C. for 24 hours Dense growth101 850° C. for 12 hours Microscopic growth102 850° C. for 24 hours Fair growth103 850° C. for 24 hours Good growth**104 850° C. for 24 hours Good growth**______________________________________ *Dense growth indicates a dense surface mat with fibers averaging about 0.25" in length. **Good growth indicates a dense surface mat with fibers averaging about 0.125" in length.
Fluorapatite Crystalline Fibers
Table XI reports compositions, expressed in terms of mole percent on the oxide basis, which, upon exposure to a defined heat treatment, will produce fibers containing fluorapatite as the predominant crystal phase. Since it is not known with which cation(s) the fluoride is combined, it is merely recited in terms of F and the oxygen=fluorine correction factor listed in accordance with conventional analysis practice. The actual batch constituents may be any materials, either the oxides or other compounds, which, when melted together, will be converted into the desired oxide in the proper proportions. Table XII records another group of compositions, expressed in terms of weight percent on the oxide basis, illustrating the effect of MoO 3 content on the growth of fluorapatite fibers. In the compositions reported in Tables XI and XII, an alkaline earth metal fluoride and/or an alkali metal silicofluoride provided the source of fluoride.
The batch ingredients were compounded, mixed together in a tumble mill, and charged into platinum or silica crucibles. After placing lids thereon, the crucibles were moved into an electrically-fired furnace operating at about 1400°-1500° C. and held therewithin for 3-4 hours. The resulting melts were either drigaged or cast into steel molds in accordance with the practice outlined above.
TABLE XI__________________________________________________________________________105 106 107 108 109 110 111 112 113 114 115__________________________________________________________________________SiO.sub.2 46.25 46.25 46.25 43.0 43.0 43.0 43.0 43.0 43.0 43.0 43.0Na.sub.2 O 4.0 4.0 4.0 4.0 4.0 4.0 4.0 4.0 4.0 6.0 6.0K.sub.2 O 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 2.0 2.0P.sub.2 O.sub.5 4.0 4.0 4.0 4.0 4.0 4.0 4.0 4.0 4.0 3.6 3.6CaO 20.0 -- -- 14.7 -- -- 14.7 14.7 -- 26.4 --SrO -- -- 20.0 -- -- 14.7 -- 14.7 -- -- --BaO -- 20.0 -- -- 14.7 -- 14.7 -- -- -- 26.4MgO -- -- -- 14.7 14.7 14.7 -- -- 29.0 -- --F 30.0 30.0 30.0 30.0 30.0 30.0 30.0 30.0 30.0 30.0 30.0MoO.sub.3 0.75 0.75 0.75 0.75 0.75 0.75 0.75 0.75 0.75 1.5 1.5 106.0 106.0 106.0 112.15 112.15 112.15 112.15 112.15 111.75 112.5 112.5O = F -6.0 -6.0 -6.0 -12.15 -12.15 -12.15 -12.15 -12.15 -11.75 -12.5 -12.5 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0__________________________________________________________________________
TABLE XII______________________________________ 116 117 118 119 120______________________________________SiO.sub.2 52.0 52.0 52.0 52.0 38.1Na.sub.2 O 4.64 4.64 4.64 4.64 3.4K.sub.2 O 1.75 1.75 1.75 1.75 1.3P.sub.2 O.sub.5 10.7 10.7 10.7 10.7 7.8CaO 21.0 21.0 21.0 21.0 --BaO -- -- -- -- 42.1F 12.0 12.0 12.0 12.0 12.0MoO.sub.3 2.8 1.0 2.0 4.0 1.1 104.89 103.09 104.09 106.09 105.8O = F -4.89 -3.09 -4.09 -6.09 -5.8 100.0 100.0 100.0 100.0 100.0______________________________________ 121 122 123 124______________________________________SiO.sub.2 38.1 38.1 38.1 38.1Na.sub.2 O 3.4 3.4 3.4 3.4K.sub.2 O 1.3 1.3 1.3 1.3P.sub.2 O.sub.5 7.8 7.8 7.8 7.8BaO 42.1 42.1 42.1 42.1F 12.0 12.0 12.0 12.0MoO.sub.3 2.3 3.0 4.0 4.5 107.0 107.7 108.7 109.2O = F -7.0 -7.7 -8.7 -9.2 100.0 100.0 100.0 100.0______________________________________
Following the procedure outlined above with respect to Examples 1-104, the glasses of Tables XI and XII were placed in glazed porcelain crucibles, the crucibles covered, and the crucibles moved to an electrically-fired furnace. The temperature within the furnace was raised at a rate of about ˜500° C./hour to 900° C. and held at that temperature for 16 hours. Thereafter, yet again, the furnace was allowed to cool to room temperature at furnace rate. In general, exposure temperatures between about 850°-1000° C. will yield fluorapatite fibers, with temperatures between 900°-925° C. being preferred.
Table XIII presents a visual description of the fibrous growth developed in each heat treated sample. As defined in that Table, "Good" indicates a dense mat of fibers having lengths of at least 0.25" with diameters of about 5-15 microns. "Slight" and "Fair" represent smaller amounts of fiber growth which are visible only upon microscopic examination. X-ray diffraction analyses identified the hexagonal structure of apatite.
TABLE XIII______________________________________Example No. Visual Description______________________________________105 Good106 "107 "108 Slight109 Fair110 Good111 "112 Fair-to-Good113 Very slight114 Good115 Good (0.375" long)116 Good117 Slight118 Good119 "120 Slight121 Good122 "123 "124 Fair______________________________________
The maximum level of P 2 O 5 which can be incorporated in the glass which permits melting of the glass at temperatures below 1600° C. is about 4.5 mole percent. About 4% by weight MoO 3 represents the maximum solubility thereof in the glass; higher concentrations lead to increased volatilization of MoO 3 since that compound sublimes at about 800° C. It is of interest to note that even combinations of MgO (not normally compatible with the apatite structure) with CaO, SrO, or BaO in the base glass can produce good yields of fiber on heat treatment of the glass, generally up to 1:1 molar ratios of Mg:M, where M=Ca, Sr, or Ba. It has also been discovered that the addition of excess fluoride in the form of NH 4 HF 2 to the samples in the covered crucibles leads to the formation of long fibers, i.e., about 0.5-1" in length (0.5-2 microns in diameter), upon heat treatment of the glass.
Table XIV records the results of chemical analyses performed on the fibers grown through the heat treatment of Examples 105, 106, and 107. The glass of Example 105 was heated at 920° C. for 16 hours; the glasses of Examples 106 and 107 were heated at 900° C. for 16 hours. An empirical formula for each fiber was calculated from the analyses and those formulae are also listed in Table XIV. Each formula was calculated on the basis of (PO 4 ) -3 being 3.0, since (PO 4 ) -3 is the most accurate analysis.
TABLE XIV______________________________________ 105 106 107______________________________________Ca 41.44 -- --F 3.78 1.77 1.91(PO.sub.4).sup.-3 49.68 24.05 33.14MoO.sub.3 4.72 4.52 4.35Sr -- -- 60.72Ba -- 67.97 --Na.sub.2 O <0.2 0.27 0.21K.sub.2 O <0.2 <0.1 <0.1SiO.sub.2 <0.1 0.2 <0.1______________________________________Empirical Formulae______________________________________Example No. 105 Ca.sub.4.93 F.sub.0.95 (PO.sub.4).sub.3Example No. 106 Ba.sub.4.88 F.sub.0.88 (PO.sub.4).sub.3Example No. 107 Sr.sub.4.96 F.sub.0.91 (PO.sub.4).sub.3______________________________________
The empirical formula calculated for each type of apatite fiber corresponds well with respect to the anticipated M 5 F(PO 4 ) 3 stoichiometry with trace amounts of Na 2 O, K 2 O, and SiO 2 incorporated into the structure. The increased concentration of MoO 3 found in the fibers, as compared to that in the precursor glass, is consistent with the phenomenon observed above in the fluormica fibers. Such circumstance again supports the proposed mechanism for fiber growth; viz., that molybdenum promotes and participates in the structural growth of the apatite fibers and is delivered by means of the gaseous phase.
Fluoride-Containing, Spodumene-Type Fibers
Table XV recites compositions having the stoichiometry of classic spodumene (Li 2 O:Al 2 O 3 :4SiO 2 ), expressed in terms of mole percent on the oxide basis, to which excess fluoride and MoO 3 were added, also reported in terms of mole percent. Because it is not known with which cation(s) the fluoride is combined, it is simply recorded in terms of F and the oxygen=fluorine correction factor tabulated in accordance with conventional analysis procedure. The actual batch components may comprise any materials, either oxides or other compounds, which, when melted together will be converted into the desired oxide in the proper proportions.
The batch ingredients were compounded, mixed together in a tumble mill, and charged into platinum crucibles. After placing lids thereon, the crucibles were moved into an electrically-fired furnace operating at 1450° C., maintained therewithin for three hours, and the melts then either drigaged or poured into steel molds in accordance with the practice described above.
TABLE XV__________________________________________________________________________125 126 127 128 129 130 131 132__________________________________________________________________________SiO.sub.2 66.6 66.6 66.6 66.6 65.5 66.6 66.6 66.6Al.sub.2 O.sub.3 16.7 16.7 16.7 16.7 16.4 16.7 16.7 16.7Li.sub.2 O 16.7 16.7 16.7 16.7 16.4 16.7 16.7 16.7MoO.sub.3 -- 1.0 1.7 2.55 1.7 1.5 1.5 --F 30.0 30.0 30.0 -- 15.0 5.0 30.0 100.0 131.0 131.7 132.55 100.0 116.5 106.5 130.00=F -- -31.0 -31.7 -32.55 -- -16.5 -6.5 -30.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0__________________________________________________________________________
Two sets of samples were prepared from the glasses of Table XV and charged into porcelain crucibles. To one set of samples powdered NH 4 HF 2 was added in an amount to yield a 1:3 volume ratio of NH 4 HF 2 to glass. No addition was made to the second set of samples. Lids were placed upon the crucibles and the crucibles then moved into an electrically-fired furnace. Following the practice generally outlined above, the temperature within the furnace was raised at about ˜250° C./hour to 900° C., held at 900° C. for 12 hours, and, once again, the furnace was permitted to cool to room temperature at furnace rate. In general, heat treating temperatures within the range of 850°-1000° C. will produce the desired fibers, with temperatures between about 850°-900° C. being preferred.
Table XVI provides a visual description of fiber growth. As employed therein, "Good" indicates fibers having lengths averaging about 0.5" and diameters between about 1-5 microns, with growth concentrated at sharp edges and ridges of the glass; "fair" signifies a sparser yield of fibers; "poor" denotes a very sparse yield, the fibers being mainly microscopic-sized. Only those glass samples containing the added NH 4 HF 2 generated colorless, transparent, needle-like fibers. In like manner of the examples described above, fibers only occurred with a combination of MoO 3 and excess fluoride; neither MoO 3 nor excess fluoride alone produced fibers.
TABLE XVI______________________________________Example No. Visual Description______________________________________125 None126 Fair127 Good128 Somewhat less than 127129 None130 Poor131 None132 None______________________________________
An examination of Table XVI with Table XV indicates the need for careful control of the MoO 3 and F concentrations. Hence, MoO 3 levels between about 1-3 mole percent and excess F in amounts greater than about 15% yield the desired fibers. Examples 129 and 131 with added NH 4 HF 2 were also treated at 950° C. for 24 hours, but no substantial formation of fibers was observed in either.
X-ray diffraction analysis of the fibers grown in Example 127 after heat treatment for 12 hours at 900° C. indicated the fibers were crystalline and spodumene-like in character. Thus, X-ray diffraction patterns derived therefrom exhibit some major peaks similar to those of spodumene, but also some other unidentifiable peaks. The spectrum corresponds to no currently-known crystal species. That the fibers do not possess a true monoclinic spodumene structure is not unexpected, however, since fluoride is not a normal component of the spodumene moiety.
X-ray diffraction and optical microscope studies of fibers grown in Example 127 after a heat treatment for 24 hours at 900° C. showed them to be amorphous, but of similar shape. It is hypothesized that excessive heat treatment results in depletion of fluoride in the spodumene crystal with resulting conversion to the glassy phase.
X-ray energy of dispersion analyses of both the crystalline and amorphous fibers indicated the presence of Al, Si, and Li with traces of Mo in each.
Table XVII records chemical analyses in weight percent of the glass prepared from Example 127, crystalline fibers grown by heat treating the glass of Example 127 for 12 hours at 900° C., and amorphous fibers resulting from heat treating the glass of Example 127 for 24 hours at 900° C. Table XVII also recites an empirical formula for each fiber as calculated from those analyses. Each formula was calculated on the basis of Al 2 O 3 =1 mole.
TABLE XVII______________________________________ Crystalline AmorphousGlass Fibers Fibers______________________________________SiO.sub.2 59.95 58.15 61.53Al.sub.2 O.sub.3 25.76 23.58 26.98Li.sub.2 O 7.12 6.92 6.75F 6.55 8.7 3.75MoO.sub.3 2.47 3.34 3.15______________________________________ Crystalline Fibers Li.sub.2 O:Al.sub.2 O.sub.3 :4.19 SiO.sub.2 :1.98 F:0. MoO.sub.3 Amorphous Fibers 0.85 Li.sub.2 O:2Al.sub.2 O.sub.3 :3.87 SiO.sub.2 :0.75 F:0.083 MoO.sub.3
As is apparent from Table XVII, the levels of F and MoO 3 in the crystalline fibers have increased significantly over those present in the precursor glass. That condition parallels the phenomenon observed above with respect to the fluormica and fluorapatite fibers, again suggesting a solid state-vapor phase mechanism for fiber growth. In contrast, the fluoride content of the amorphous fibers is less than one-half that present in the crystalline fibers, thereby indicating a loss of fluoride upon prolonged heat treatment. It is believed most significant that the empirical formula calculated from the chemical analysis of the crystalline fibers very closely approximates that of true spodumene with a slight increase in SiO 2 content (assuming Al 2 O 3 =1.00), and with about 2 gram atoms of fluoride per spodumene unit. In the amorphous fibers, however, the concentration of Al 2 O 3 has effectively increased at the expense of Li 2 O and SiO 2 ; which circumstance can be expected from the loss of fluoride through the volatilization of LiF and SiF 4 from the fibers. | This invention is directed to the production of inorganic crystalline fibers containing a minor amount of Mo0 3 and/or W0 3 and/or As 2 0 3 and wherein the predominant crystal phase is selected from the group of a fluormica, a fluoramphibole, canasite, potassium and/or sodium fluorrichterite, fluorapatite, and a lithium-containing, beta-spodumene-type crystal. | 3 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is the U.S. national stage of International Application No. PCT/EP2010/064483, filed Sep. 29, 2010 and claims the benefit thereof. The International Application claims the benefit of German Application No. 10 2009 043 537.9 filed on Sep. 30, 2009; both applications are incorporated by reference herein in their entirety.
BACKGROUND
[0002] Described below is a method and an assembly for determining cell vitalities. The method includes binding living cells to magnetic particles, application onto a sensor array, uniform distribution over the sensor array, magnetic immobilization of the magnetic particles with the bound cells over the sensor array, and application of substances for maintaining and/or improving the cell vitality onto the sensor array, and/or application of substances for worsening the cell vitality onto the sensor array. The assembly includes a sensor array composed of sensors which are configured to be in direct fluidic contact with a fluid, and a device for generating a magnetic field over the sensor array.
[0003] In microbiology, a large number of methods are known for the study of pathogenic microorganisms on the basis of cell culture and antibiotic resistance tests. The “phenotypic” approach, in which the action such as for example the growth or the inhibition of cell growth is studied, is advantageous. Via the action on cell cultures, a direct reference to the action on man or animals can be obtained. In this, cell cultures are placed in a nutrient solution for days on end, e.g. in Petri dishes, and observed. The growth or the damage to the cell cultures is measured and assessed over long periods. The long periods which are necessary for the observation make the method very costly and time-consuming.
[0004] For measuring the growth or the damage to the cell cultures, sensor systems can be used. Living cells are for example grown on sensors in order then to monitor the vitality of the cells for example by measurement of impedance, oxygen or pH. As sensors, interdigital electrode arrays, oxygen sensors or pH sensors can be used. Measures of the vitality of the cells are inter alia their adhesion to surfaces, their respiration or their metabolism. However, growing the cells on the sensors is time-consuming and leads to limited storability of the sensor systems. Cells that have grown on the sensors can migrate on the surface and/or die off.
[0005] For measurement of the vitality of cells via an oxygen or pH value, a defined liquid film between a cell wall and a sensor surface is necessary. With direct growth of the cell wall on the sensor surface, the defined liquid film can be lost. This can lead to impairment of the measurement, right down to the case wherein a measurement becomes impossible.
[0006] For a reliable measurement, it is also necessary that the sensor surface be free from dead cells. For this reason, before each treatment or measurement interval, dead cells must be removed from the sensor surface. This is as a rule effected by reagents, which is associated with expenditure and can lead to damage to the sensor surfaces. This prevents comparable and reproducible measurements.
[0007] Hence, described below are a method and an assembly for determining cell vitalities, which allow rapid and simple as well as reliable measurement of parameters which are typical of cell vitality. At the same time, error factors, such as for example the migration of cells on the surface or measurement errors due to direct surface growth with no liquid film between cell and sensor surface, should be excluded.
SUMMARY
[0008] The method for determining cell vitalities includes binding living cells to magnetic particles, and application of the magnetic particles with bound cells onto a sensor array, and uniform distribution of the magnetic particles with the bound cells over the sensor array, and magnetic immobilization of the magnetic particles with the bound cells over the sensor array, and application of substances for maintaining and/or improving the cell vitality onto the sensor array. Further, substances for worsening the cell vitality onto the sensor array can also be applied.
[0009] Through the binding of the living cells to magnetic particles, the movement of the cells becomes controllable by an external magnetic field. They can for example be bound to the magnetic particles by antibodies, in particular when the particles have a diameter in the nano- to micrometer range. With larger particles in the range of a few hundred micrometers diameter, the cells can also grow on the surface of the particles. After the binding, the cells can be temporarily stored in a holding vessel. For the measurement of the cell vitality of the living cells, the cells are then moved over to a sensor array and there immobilized magnetically. The movement can for example be effected by a flowing liquid or by magnetic interaction. Cells magnetically immobilized over the sensor array can then be assayed, for which substances for maintaining and/or improving and/or worsening the cell vitality are used. The chemical products which are formed during the metabolism of the cells or the consumption of chemical substances during the metabolism of the cells are measured by the sensors of the sensor array, for example qualitatively or quantitatively. On account of the assembly of the sensors in the form of an array, these measurements can be made with spatial resolution.
[0010] The use of magnetic particles for the handling of the cells allows the use of cells as required and the rapid, reliable supply of living cells to the sensor array. Thus for example previously prepared living cells stored in the holding vessel can be supplied to the sensor array at the relevant time for the measurement for example of environmental pollutants to be made. Alternatively for example, certain cells from blood can be “filtered out” by binding to the magnetic particles and be specifically supplied to the sensor array by the magnetic particles. This can be effected more simply and more cheaply than for example by manipulation by pipettes or by proliferation of cell cultures over days and on specific nutrient solutions.
[0011] The substances for maintaining and/or improving the cell vitality can include oxygen and/or nutrient solution. The substances for worsening the cell vitality can include antibiotics. During a measurement, the substances can be specifically added onto the sensor array once or alternately at intervals, and changes in the metabolic products of the cells can be measured during this. This enables reliable and prompt statements about the cell vitality and is cheaper and more time-saving than the observation of cell growth of individual cell cultures in nutrient solutions in Petri dishes, for example optically.
[0012] In the method, an optimal temperature for cell vitality can be set, in particular 37° C. At this temperature, the measurement signal of converted metabolic products or the decrease in starting substances for the metabolic reactions of the cells is particularly large and thus easy to measure.
[0013] The sensors of the sensor array can include electrochemical and/or chemical sensors. These can in particular be configured to measure values which serve as a measure of cell vitality. In contrast to optical measurements, with electrochemical measurements the non-transparent magnetic particles do not interfere with the measurement. Electrochemical sensors can be made very small and cheaply in array form and yield reliable measurement results. The purely electrical evaluation of current-voltage signals by electrochemical sensors is simpler and cheaper to perform than for example with optical measurements.
[0014] As quantities measured by the sensors, substances consumed by cells and/or metabolic products of cells can be measured, in particular acids as pH and/or oxygen as pO 2 and/or proteins. These quantities are clear measures of the vitality of a cell. Thus for example due to the metabolism of a cell, oxygen is consumed in its vicinity. The decrease in the oxygen in its immediate vicinity is thus a clear measure of the vitality of the cell.
[0015] The cells bound to the magnetic particles over the sensor array can be removed when necessary, in particular by manipulation of the magnetic field over the array. Thereby, a sensor can again be regenerated and prepared for the next measurement. Measurement at intervals over more prolonged periods is thereby enabled. Dead cells, if they were not removed, would block the sensors and falsify measurement results or make measurement quite impossible. Through the measurement by the sensor array, dead cells can be identified and specifically transported away via the magnetic field. The transport of dead cells away and the possibility of renewing the sensor resulting from this is useful precisely with regard to the measurement of environmental pollutants and the functioning of a sensor over a longer period.
[0016] Here the removal of dead cells can repeatedly be followed by binding living cells to magnetic particles, application of the magnetic particles with bound cells onto the sensor array, and uniform distribution of the magnetic particles with the bound cells over the sensor array for a reliable, specific measurement of individual cells, and magnetic immobilization of the magnetic particles with the bound cells over the sensor array, and application of substances for maintaining and/or improving the cell vitality onto the sensor array, and/or application of substances for worsening the cell vitality onto the sensor array. Measurement over long periods or a repeated use of a sensor array for different measurements thereby becomes possible.
[0017] The assembly for determining cell vitalities includes a sensor array composed of sensors which are configured to be in direct fluid contact with a fluid, and a device for creating a magnetic field over the sensor array. A layer which simultaneously includes magnetic particles and living cells is formed on the sensor array. The assembly can be used for the method described above.
[0018] Here the living cells can be embedded in a matrix of magnetic particles in the layer on the sensor array. This ensures that at least some or all cells do not grow directly on the sensors and a liquid film is located between the cells and the sensors. This makes reliable measurement of the vitality of the cells possible for the first time. Without a liquid film between the cells and the sensor surface, reliable recording of the reaction products or starting material concentration or the change therein by the sensors is not possible. The magnetic particles so to speak serve as spacers for the cells, in order to prevent direct growth of any cells on the sensor surfaces.
[0019] The layer on the sensor array including magnetic particles and living cells can have an essentially equal thickness over the region of the sensor array. In particular, the thickness of the layer can lie in the micrometer range. The thickness of the layer can lie in the range from 10 to 1000 micrometers. Through a uniform layer thickness, accumulation of cells over individual sensors can be prevented and with a thickness in the micrometer range cells in the particle matrix are close enough to a nearest sensor, with a correspondingly small distance of the sensors from each other, for products or the decrease in starting substances for it to be possible for the sensors to record the cell metabolism. By essentially uniform thickness, it is meant that certain fluctuations because of the irregularities of round particles and undulations in the layer surface due to slight fluctuations in the particle numbers at a point are possible in the range of less than one power of ten.
[0020] Between the living cells and the sensors of the sensor array, at least one closed layer of magnetic particles can be located, which ensures that no cells grow directly on a sensor surface. In particular, cavities between the magnetic particles can be fillable with liquid in order to enable electrochemical measurements. The sensor array can be coated with a closed layer of magnetic particles before the layer with living cells is formed on the sensor array. A separation of the layer formation into two steps increases the reliability of the vitality measurement of the cells, since it is ensured that no cells deposit into the closed layer and grow directly on a sensor surface.
[0021] The assembly can include a flow cell with a support, wherein the sensor array is arranged on one surface of the support in fluid connection with the flow cell of the sensor array.
[0022] The sensors of the sensor array can be electrochemical sensors, in particular microsensors with a total space usage of one sensor on the surface of the sensor array in the micrometer range. Thus the size of one sensor is of the order of that of one cell and assignment of the measurement signal of one sensor to one cell becomes possible. The conversion of substances by one cell lies in a range which can be measured by a sensor with a size in the micrometer range. Sensors which are much larger, for example of the order of millimeter size, cannot reliably measure concentration changes on a scale as small as are triggered by the cell metabolism in the direct vicinity of a cell. The use of electrochemical sensors for the first time makes it possible to form the sensors in the micro meter range and yields reliable measurement signals even with nontransparent particles.
[0023] The assembly can include at least one device for changing the magnetic field. This can be a coil device and/or a device for moving permanent magnets. Thereby the magnetic field can be formed such that a uniform layer of magnetic particles is formed over the sensor array. When the magnetic field is removed for example by rotation of a permanent magnet or interruption of a flow of current through the coil, the immobilization of the magnetic particles and hence the cells over the sensors can be reversed and dead or damaged cells can be removed or transported away from the sensor array. New, fresh cells can be immobilized anew over the sensor array, for example by again turning on the current in the coil or again bringing the permanent magnet into a position in which a magnetic field for immobilizing the magnetic particles or magnetic beads is produced. Thus the sensor array with living cells is available for a fresh measurement.
[0024] The advantages connected with the assembly for determining cell vitalities are analogous to the advantages which were described previously with reference to the method for determining cell vitalities.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] 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:
[0026] FIG. 1 is a cross-sectional representation through a flow cell with a device for creating a magnetic field for immobilizing magnetic particles according to the related art,
[0027] FIGS. 2A-2C are cross-sectional representations through a flow cell with a device for creating and changing a magnetic field for immobilizing magnetic particles with cells over a sensor array,
[0028] FIG. 3 is an enlarged representation of the flow channel shown in FIGS. 2A-2C with a uniform layer of cells in a magnetic particle matrix with the device for creating and changing the magnetic field, and
[0029] FIG. 4 is an enlarged representation of the uniform layer of cells in a magnetic particle matrix on the sensor array shown in FIG. 3 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0030] 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.
[0031] FIG. 1 is a section through a flow cell 1 according to the related art. The flow cell 1 includes a flow channel 2 which is flowed through by a liquid in the flow direction 3 . The liquid contains individual magnetic particles or magnetic beads to which for example DNA fragments can be bound. The flow channel 2 is surrounded by a device for creating a magnetic field 5 , 5 ′, i.e. permanent magnets are mounted above and below the flow channel 2 . Via a mu metal body 6 , 6 ′ directly above and below the flow channel 2 , the magnetic field of the permanent magnets 5 , 5 ′, represented in FIG. 1 by the magnetic lines of force 7 , is concentrated to a small region within the flow channel 2 .
[0032] A place with the highest magnetic field density 8 , at which the magnetic beads 4 in the fluid are collected and immobilized, is formed in the flow channel 2 . Using cooling bodies 9 , 9 ′, which are located above and below the flow channel 2 , and Peltier elements 10 , 10 ′ in thermal connection with heat coupling plates 11 , 11 ′, also each located above and below the flow channel 2 , the temperature can be controlled or adjusted in the flow channel 2 at the place with the highest magnetic field density 8 . Thus for example DNA fragments, bound onto the magnetic beads 4 , can be amplified by a PCR (polymerase chain reaction) by changing the temperature in the form of time gradients between two temperatures.
[0033] FIG. 2 shows a cross-sectional representation through an assembly for measuring cell vitality according to one practical example. A flow channel 2 is located between two permanent magnets 5 , 5 ′. A device, not shown, for changing the magnetic field 16 , which can for example be a rotatable stepping motor, is connected to one of the permanent magnets 5 ′. In FIG. 2A , the permanent magnet 5 ′ is in a position wherein a magnetic field is present in the inside of the flow channel 2 . Magnetic particles 4 in the flow channel are immobilized and collected by the magnetic field in the region between the permanent magnet 5 and the permanent magnet 5 ′. In this region, a chip module 12 with chip 13 is located, on which there is a sensor array 14 in fluid contact with the flow channel 2 . Thus with liquid flowing the magnetic particles 4 and cells 15 which are bound to the magnetic particles 4 are magnetically immobilized over the sensor array 14 by the magnetic field.
[0034] In FIG. 2B , the liquid is in a motionless state and the permanent magnet 5 ′ rotated by 90° compared to the position of FIG. 2A , as a result of which no magnetic field caused by the permanent magnet 5 ′ is present in the flow channel 2 . The lines of force 7 take a course which do not point from the permanent magnet 5 to the permanent magnet 5 ′ and do not pass through the flow channel 2 . The magnetic particles 4 and cells 15 can move and redistribute themselves freely over the sensor array 14 , for example by circular liquid flows over the sensor array 14 or by diffusion or convection.
[0035] In FIG. 2C , the liquid is in a motionless state and the permanent magnet 5 ′ again rotated into the original position, as shown in FIG. 2A . In the region over the sensor array 14 in the flow channel 2 , a magnetic field operates whose lines of force 7 are at an essentially uniform distance from one another. The uniform field distribution over the sensor array 14 leads to a formation of an essentially uniformly thick layer of magnetic particles 4 , in which cells 15 are embedded. The magnetic particles 4 form a kind of matrix, in which the cells 15 are immobilized over the sensor array 14 .
[0036] FIG. 3 shows an alternative practical example for the formation of a variable magnetic field in the flow channel 2 over the sensor array 14 . A permanent magnet 5 is located under a magnetic field-shaping element 16 . The magnetic field-shaping element 16 can for example be magnetizable iron and has an external shape which leads to the formation of a particularly uniform magnetic field in the flow channel 2 over the sensor array 14 . In the example shown in FIG. 3 , the magnetic field-shaping element 16 is made rounded on the side which faces in the direction of the sensor array 14 . The uniformly created magnetic field over the sensor array 14 leads to the formation of an essentially equally thick layer of magnetic particles 4 with embedded cells 15 over the sensor array 14 . The permanent magnet 5 can be mounted movably and on removal of the permanent magnet 5 from the magnetic field-shaping element 16 the magnetic field in the flow channel can be “switched off”. On again bringing the permanent magnet 5 close to the magnetic field-shaping element 16 the magnetic field in the flow channel can be “switched on” again. Alternatively to the permanent magnet 5 and/or the magnetic field-shaping element 16 , electrical coils can be mounted close to the sensor array 14 , which on current flowing through the coils create a controllable or adjustable magnetic field.
[0037] FIG. 4 shows an enlarged representation of the essentially uniformly thick layer of magnetic particles 4 with embedded cells 15 over the sensor array 14 shown in FIGS. 2 C) and 3 . In the matrix of magnetic particles 14 , cells are always present which are located with a spatial distance from the sensor 17 lying closest. This ensures that these cells 15 do not grow directly on the sensor 17 and that a liquid film exists or is located between these cells 15 and the sensors 17 . As a result, reliable electrochemical measurements of the cell vitality with the sensors 17 for the first time become possible. The cells 15 cannot migrate since they are embedded and immobilized in the matrix of magnetic particles. With formation of the layer of magnetic particles 4 with cells 15 with a thickness in the micrometer range and location of the sensors 17 in an array shape with a distance between the sensors 17 in the range of micrometers to each nearest neighbor, it is ensured that the region of the change in a measured quantity 18 due to the cells 15 in the vicinity of the cells 15 is in contact with at least one sensor 17 . The region of the change in a measured quantity 18 in the vicinity of the cells 15 can for example be the diffusion length of oxygen. In their metabolism, living cells 15 consume oxygen and the change in the oxygen concentration can be measured in the region 18 by the sensors 17 .
[0038] If the cells are damaged due to the measurement or have died, then these can be simply transported away by switching off the magnetic field and switching on a fresh liquid flow. A new layer of magnetic particles 4 with fresh living cells 15 can be formed over the sensor array 14 and the assembly can be available for a fresh measurement. Thereby a regenerable sensor assembly which can perform measurements at intervals over prolonged periods such as for example days, weeks or months is provided.
[0039] A description has been provided with particular reference to preferred embodiments thereof and examples, but it will be understood that variations and modifications can be effected within the spirit and scope 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). | The method includes binding living cells to magnetic particles, adding them to a sensor array, uniformly distributing over the sensor array, magnetically fixing the magnetic particles having the bound cells over the sensor array, and adding substances to maintain and/or improve the cell vitality to the sensory array, and/or adding substances to worsen the cell vitality to the sensor array. The assembly includes a sensor array composed of sensors, which are designed to be in direct fluidic contact with a fluid, and a device for generating a magnetic field over the sensor array. A layer that comprises magnetic particles and living cells is formed on the sensor array. | 6 |
CROSS-REFERENCE TO RELATED APPLICATION(S)
This application incorporates by reference and claims priority from application Ser. No. 10/628,220, filed Jul. 28, 2003, entitled “Line Splice Using Barb and Receiver,” by Russell E. Blette, John E. Stark and Jeffrey L. Wieringa.
BACKGROUND OF THE INVENTION
This invention relates in general to a device and method for linearly connecting strand materials and more particularly to a device which facilitates the connection of fishing lines.
In many types of fishing, and particularly in fly fishing, it is necessary or desirable to linearly connect sections of fishing line, either because of different properties of the sections or to repair a break. A fly fisherman must be equipped with a fishing rod, a fishing line called a fly line, a device such as a reel to hold the fly line, a leader line commonly called a leader, and flies. A leader is a relatively short, fine, tapered segment of monofilament line, with its larger or butt end attached to the fly line and its smaller or terminal end to the fly.
Fly fishing involves casting a line a substantial distance over a body of water wherein only the weight of the line is used to effect the cast. A skilled fly caster typically uses a tapered line and a tapered leader at the end of this line. One of the more difficult aspects of fly fishing involves connecting the end of the leader to the end of the fishing line by tying a knot. The knot must be specially selected to avoid kinks and/or slip-separation of the leader from the line.
Typically, a leader will range from as short as 5 or 6 feet to as long as 12 to 15 feet. Some leaders possess a true taper, that is, they undergo a gradual change in diameter from the butt end to the terminal end without any interruptions in the leader material. Other leaders consist of lengths of varying diameter leader material tied together. Many fishermen favor the latter, that is the knotted leader, in that it enables them to tailor the leader to their own needs. But irrespective of whether the fisherman uses a truly tapered leader or a knotted leader, the fisherman will usually find it necessary to replace the end section or segment of the leader, often called the tippet, for this is where the leader is thinnest and weakest, and where it will break if its capacity is exceeded. Tippet replacement and repair usually require a fisherman to form a knot. Moreover, when a fisherman changes to a smaller fly, a thinner tippet is often required. Hence, the typical fisherman must tie knots from time to time in leader material, which is usually monofilament line.
The knots which join the lengths of leader material either to the fly line or to other leader sections must accommodate the varying diameters of material and must be strong. Nail knots and Albright knots meet these requirement, but are time consuming to tie and require skill, good eyesight and considerable manual dexterity. Moreover, the knot is usually the weakest part of the fish line and may cause the breaking of the fish line at the knot.
Thus, there remains a need for a quick and easy device and method for strong linear connection of fishing lines.
BRIEF SUMMARY OF THE INVENTION
A splice system for linear connection of fishing lines includes a female connector and a male connector. Each connector has first and second opposite ends, a longitudinal axis, and a shaped exterior surface. The first end of the female connector is connected to a first fishing line section; the second end has a first opening; and the connector has a raised interior feature. The second end of the male connector is connected to a second fishing line section; the first end is configured for coaxial insertion into the first opening of the female connector, and the first end has a raised exterior feature. The connectors have a first relative position representing a disengaged state and a second relative position representing an engaged state. The first relative position and the second relative position are rotationally displaced about the axis.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is perspective view of one embodiment of the splice system of the present invention.
FIG. 2 is perspective view the embodiment of FIG. 1 , shown from a different angle.
FIG. 3 is a cross-sectional view along line 3 - 3 of FIG. 2 , showing the two connectors of the splice system in a disconnected configuration.
FIG. 4 is a cross-sectional view along line 4 - 4 of FIG. 2 , showing the two connectors rotated for insertion of the male connector into the female connector.
FIG. 5 is a cross-sectional view of the two connectors of FIG. 4 , rotated for connection of the male connector and the female connector.
FIG. 6 is perspective view of one embodiment of a tool of the present invention for use in facilitating the rotation and connection of the male and female connectors in a first embodiment of a connection method.
FIG. 7 is a perspective view of a card holding multiple female connectors.
FIG. 8 is a partial perspective view illustrating use of a connector holding tool disposed on the card of FIG. 7 in a second embodiment of a connection method.
FIG. 9 is a partial perspective view illustrating use of a connector holding tool disposed on the card of FIG. 7 in a third embodiment of a connection method.
While the above-identified drawing figures set forth several embodiments of the invention, other embodiments are also contemplated, as noted in the discussion. In all cases, this disclosure presents the invention by way of representation and not limitation. It should be understood that numerous other modifications and embodiments can be devised by those skilled in the art which fall within the scope and spirit of the principals of this invention. The figures may not be drawn to scale. Like reference numbers have been used throughout the figures to denote like parts. Where modifiers such as first, second, top, bottom, etc. are used, they are for purposes of description only and not limitation.
DETAILED DESCRIPTION
FIG. 1 is perspective view of one embodiment of the splice system of the present invention. Splice system 10 connects fly or fishing line 12 and leader 14 or other fishing line segments along longitudinal axis 15 . Splice system 10 includes two main components: male connector or barb 16 and female connector or receiver 18 .
Leader 14 is either permanently or removably secured to barb 16 . Fly line 12 is either permanently or removably secured to receiver 18 . FIG. 1 illustrates barb 16 partially inserted into, but not yet fully mated with, receiver 18 . When barb 16 is fully inserted into receiver 18 , a raised exterior feature on a first end of barb 16 engages with a raised interior feature on receiver 18 to facilitate a strong, yet reversible locking connection between barb 16 and receiver 18 . In the illustrated embodiment, the raised exterior features of barb 16 include flanges 20 with radially extending shoulders 22 .
In an exemplary embodiment, barb 16 has a shaped exterior surface having one or more exterior ribs 28 ; similarly; receiver 18 has a shaped exterior surface having one or more exterior ribs 29 . When barb 16 and receiver 18 are fully connected (e.g. FIG. 5 ), radially extending stop surface 24 of barb 16 is disposed adjacent radially extending end surface 26 of receiver 18 and exterior ribs 28 of barb 16 align with exterior ribs 29 of receiver 18 . In one embodiment, barb 16 and receiver 18 include tapered surfaces 30 and 32 , respectively, to enhance the movement of splice system 10 through air and water.
When barb 16 and receiver 18 are fully connected, thereby connecting leader 14 to fly line 12 , a fisherman can cast fly line 12 and leader 14 over the water to place fly 34 into the body of water. In an exemplary embodiment, barb 16 and receiver 18 are each molded from a lightweight, resilient and durable material such as plastic or nylon. Nylon 66, available from E.I. DuPont de Nemours and Co., Inc., Wilmington, Del., is used in one suitable embodiment. Polypropylene, which floats in water, is used in another suitable embodiment.
In an exemplary embodiment, a connected system 10 of barb 16 and receiver 18 is less than about 0.75 inch (19.05 mm) long and less than about 0.125 inch (3.2 mm) in diameter. In some embodiments, fly line 12 is about 0.932 inch (0.81 mm) to about 0.042 inch (1.07 mm) in diameter. In some embodiments, leader 14 is about 0.020 inch (0.51 mm) to about 0.026 inch (0.66 mm) in diameter. Splice system 10 , with its low profile, small size, light weight, elongated shape and circular cross section is advantageous over other connection methods in that it is easy to use, very small, lightweight, and aero- and hydrodynamic. The shape and size allow a fly line 12 and leader 14 connected by splice system 10 to glide easily through air and water without disrupting the flow of the fishing line in casting. In particular, tapered surface 32 of receiver 18 improves the “pick up” of splice system 10 off the water and allows for more accurate casting due to the reduction of frictional resistance with respect to the water and air, compared to other splice systems.
In one embodiment, buoyancy is incorporated into barb 16 and/or receiver 18 by using buoyant materials or adding buoyant features such as dispersed hollow glass beads in the bulk material. System 10 , when brightly colored, is functional as a strike indicator because it visibly signals movement of the leader and fly during a fish strike.
In some applications, a sinking line is preferred. In that case, sinking ingredients such as tungsten powder can be incorporated into barb 16 and/or receiver 18 , or a sinking member (not shown) may be added. Moreover, the sinking member may be colored to render it highly visible by day or night or camouflaged, as desired. Other treatments for the components of splice system 10 include protection against ultraviolet light.
FIG. 2 is perspective view the embodiment of FIG. 1 , shown from a different angle. In the illustrated example, barb 16 has two flanges 20 with associated radial shoulders 22 . Receiver 18 has a raised interior feature, which in the illustrated example includes a ridge 36 having first and second ends and a stop rib 38 connected to one end of ridge 36 . The embodiment preferably has another ridge 36 and stop rib 38 feature on an opposite interior surface of receiver 18 (not visible).
To connect barb 16 and receiver 18 , a user inserts first end 40 of barb 16 past end surface 26 of receiver 18 . The user rotates barb 16 and/or receiver 18 about axis 15 until flanges 20 align with interior areas of receiver 18 which are not blocked by ridges 36 . The user then advances barb 16 into the opening on the receiver 18 to advance radial shoulders 22 past ridges 36 . Such advance is ultimately limited by contact of extending stop surface 24 on barb 16 with end surface 26 on receiver 18 . The user then rotates barb 16 relative to receiver 18 about axis 15 to position each radial shoulder 22 behind a respective ridge 36 . Due to the presence of stop rib 38 , this rotation step can be performed in only one direction. When a flange 20 contacts stop rib 38 , further rotation is not possible; at this point, the user is assured that barb 16 and receiver 18 are adequately connected to prevent axial separation. In an exemplary embodiment, the degree of rotation required to connect system 10 can be a quarter turn or half turn, for example.
In an exemplary embodiment, barb 16 has one or more exterior ribs 28 and receiver 18 has one or more exterior ribs 29 . In such an embodiment, when system 10 is fully connected, ribs 28 align with ribs 29 , offering visual assurance that the locking rotation is complete. Moreover, ribs 28 and 29 provide gripping surfaces to facilitate the rotation of barb 16 and receiver 18 with respect to each other.
In the illustrated embodiment, two flanges 20 are shown, which cooperate with two ridges 36 . However, it is contemplated that more or fewer such features can be used. Similarly, the exemplary embodiment has four exterior ribs 28 , which align with four exterior ribs 29 . However, any number of such features can be used.
FIG. 3 is a cross-sectional view along line 3 - 3 of FIG. 2 , showing the two connectors of the splice system in a disconnected configuration. In the illustrated embodiment, each flange 20 has a narrow width adjacent first end 40 of barb 16 and gradually widens to terminate at radial shoulder 22 . However, it is contemplated that such a tapered shape may be replaced by a simple partial annulus or other shape. A narrow neck 42 is disposed on barb 16 between radial shoulder 22 and stop surface 24 . One embodiment also includes annular step 43 to provide increased lateral stability when barb 16 and receiver 18 are connected. In one embodiment, barb 16 includes axial bore 44 and cavity 46 which intersect at interior radially extending shoulder 48 . In an exemplary embodiment, axial bore 44 is large enough to allow the passage of leader 14 but not wide enough to allow the passage of knot 50 in leader 14 . In an exemplary embodiment, cavity 46 is wide and deep enough to accommodate knot 50 .
In the illustrated embodiment, leader 14 is removably connected to barb 16 . To connect leader 14 to barb 16 , a user threads leader 14 through axial bore 44 from second end 52 of barb 16 to first end 40 of barb 16 . After pulling leader 14 through first end 40 , the user ties the end of leader 14 into knot 50 . If leader 14 is especially thin, a double knot may be used. If leader 14 extends beyond knot 50 , the user can trim off the extra length if desired. Then, the user pulls back on leader 14 to seat knot 50 against shoulder 48 .
In an alternative embodiment, leader 14 is attached to barb 16 during manufacturing with knot 50 or another mechanism. A filler or plug (not shown) may be inserted to close end 40 of cavity 46 during manufacture to permanently secure leader 14 in barb 16 . In another embodiment, leader 14 is integrally formed with barb 16 so that axial bore 44 , cavity 46 and knot 50 are eliminated. This can be accomplished, for example, by molding barb 16 over leader 14 so that they form an inseparable unit.
In the illustrated embodiment, receiver 18 includes axial bore 54 and cavity 56 , which intersect at shoulder 58 . Axial bore 54 is large enough to allow the passage of fly line 12 but not wide enough to allow the passage of knot 60 formed at the end of fly line 12 . In one embodiment, axial bore 52 has a diameter of between about 0.030 inch (0.76 mm) and about 0.050 inch (1.27 mm). Additionally, cavity 56 is wide enough to accommodate knot 60 and deep enough to accommodate knot 60 and the portion of barb 16 from first end 40 to stop surface 24 . To attach fly line 12 to receiver 18 , a user threads fly line 12 from first end 62 of receiver 18 through second end 26 . The user then ties knot 60 in fly line 12 . If fly line 12 is especially thin, a double knot maybe used. If excess fly line 12 extends beyond knot 60 , the user can trim off the extra length if desired. The user then pulls fly line 12 back in the direction of first end 62 to seat knot 60 against shoulder 58 .
In the illustrated embodiment, ridge 36 has a tapered configuration. However, it is contemplated that such a tapered shape may be replaced by a simple partial annulus or other shape.
With fly line 12 thereby connected to receiver 18 and leader 14 connected to barb 16 , fly line 12 and leader 14 can be connected to each other by connecting barb 16 and receiver 18 , as described with reference to FIG. 2 . Fly line 12 and leader 14 are beneficially aligned along axis 15 to facilitate smooth and predictable movement through air and water.
In one embodiment, barb 16 and receiver 18 include tapered surfaces 30 and 32 , respectively, to enhance the movement of splice system 10 through air and water. Tapered surface 30 extends from a narrow diameter near second end 52 of barb 16 to a greater diameter toward stop surface 24 . Tapered surface 32 extends from a narrow diameter near first end 62 of receiver 18 to a greater diameter toward second end surface 26 .
FIG. 4 is a cross-sectional view along line 4 - 4 of FIG. 2 , showing the two connectors rotated for insertion of the male connector into the female connector. To connect barb 16 and receiver 18 , a user inserts first end 40 of barb 16 past end surface 26 of receiver 18 . To insert barb 16 completely into receiver 18 , the connectors are rotated with respect to each other about axis 15 so that flanges 20 align with interior areas of receiver 18 which are not blocked by ridges 36 . The user then advances radial shoulders 22 past ridges 36 (as shown in FIG. 4 ). This is a first relative position of barb 16 and receiver 18 , wherein flanges 20 are not engaged with ridges 36 .
FIG. 5 is a cross-sectional view of the two connectors of FIG. 4 , rotated for connection of the male connector and the female connector. Once barb 16 is fully inserted into receiver 18 , as shown in FIG. 4 , receiver 18 is rotated relative to barb 16 about axis 15 in the direction shown by arrow 61 to achieve the configuration shown in FIG. 5 . This is a second relative position of barb 16 and receiver 18 , wherein flanges 20 are engaged with ridges 36 . In an alternative embodiment, barb 16 can be rotated with respect to receiver 18 in the opposite direction. The relative rotation direction between barb 16 and receiver 18 is set by the location of stop rib 38 , which may be positioned on the opposite side of ridge 36 in an alternative embodiment, thereby requiring a reverse rotation direction for engagement.
Once the rotation step is complete, a flange 20 contacts stop rib 38 , and further rotation is prevented. At this point, each radial shoulder 22 is locked above a respective ridge 36 . An advantage of this invention is that the locking step is reversible. By reversing the rotation step and insertion steps, barb 16 and receiver 18 can be separated. This is particularly desirable because a user can then connect a different barb 16 to the receiver 18 or a different receiver 18 to the barb 16 without having to discard either section and without having to tie complicated connection knots. Thus, fly lines 12 and leaders 14 may be interchanged and preserved for later use. Morever, system 10 is not limited to the connection of fly line 12 to leader 14 , but can be used to connect pairs of any types of lines.
In one exemplary embodiment, an interference fit exits between barb 16 at radial shoulder 22 and interior surface of receiver 18 to provided added strength to the connection of system 10 . In an exemplary embodiment, barb 16 at first end 40 has an outside diameter of about 0.090 inch (2.29 mm); barb 16 , measured across opposed radial shoulders 22 has an outside diameter of about 0.120 inch (3.05 mm); and bore 56 has a largest unexpanded inner diameter of about 0.106 inch (2.69 mm). This interference fit prevents unintended rotation of barb 16 and receiver 18 relative to one another, thus ensuring that they stay coupled together in use.
In an exemplary embodiment, the materials and dimensions of barb 16 and receiver 18 are chosen so that barb 16 and receiver 18 cannot be separated with manual tensile or separation force along axis 15 of at least about 8 pounds (3.6 kg), absent a reverse rotation of the connectors, as discussed above. In an especially suitable embodiment, barb 16 and receiver 18 cannot be separated with tensile or separation force along axis 15 of at least about 10 pounds (4.5 kg). Nylon is an especially suitable material for barb 16 and receiver 18 because it swells slightly in water, leading to an even stronger interference connection between barb 16 and receiver 18 .
FIG. 6 is perspective view of one embodiment of a tool of the present invention for use in facilitating the rotation and connection of the male and female connectors in a first embodiment of a connection method. Because barb 16 and receiver 18 are each very small, the present invention provides for exemplary tools to aid in their connection and disconnection. Tool 63 includes barb holder 64 and receiver holder 65 . Each holder 64 , 65 includes shaped orifice 66 to hold either barb 16 or receiver 18 . In an exemplary embodiment, orifice 66 includes one or more rib-shaped perimeter cut-outs 67 to mate with any exterior ribs 28 , 29 , thereby providing for a secure, non-rotating hold between the holder 64 , 65 and the respective connector 16 , 18 . An exemplary embodiment includes hollow areas 68 between walls 70 for savings in materials, cost, and weight. The illustrated embodiment includes slot 69 , through which fly line 12 or leader 14 is inserted.
Tool 63 is used as follows in an exemplary connection method. Barb 16 is inserted into orifice 66 so that exterior ribs 28 nestle into corresponding orifices 66 ; leader 14 is strung through slot 69 so that it hangs from a bottom of barb tool 64 . The structure of receiver tool 65 is very similar to that of barb tool 64 . Receiver 18 is inserted into orifice 66 (not visible) of receiver tool 65 so that exterior ribs 29 nestle into corresponding orifices 66 ; fly line 12 is strung through slot 69 so that it hangs from a top of receiver tool 65 .
The user can then grasp the relatively large tools 64 , 65 to achieve the rotation motions required for the connection and disconnection of system 10 about axis 15 , as described with respect to FIGS. 2-5 . In an exemplary embodiment, barb tool 64 is about 1.0 inch (25.4 mm) wide, about 0.375 inch (9.5 mm) thick, and about 1.0 inch (25.4 mm) long, with a wall thickness of about 0.08 inch (2.0 mm). In an exemplary embodiment, receiver tool 65 is about 1.0 inch (25.4 mm) wide, about 0.375 inch (9.5 mm) thick, and about 1.5 inch (38.1 mm) long, with a wall thickness of about 0.08 inch (2.0 mm). In an alternative embodiment, tool 63 may take the form of any device having shaped orifice 66 .
FIG. 7 is a perspective view of a card holding a multiple female connectors 18 . Card 72 provides for convenient storage of, and easy accessibility to, receivers 18 . Card 72 is easily stored in a user's vest pocket, providing a convenient storage unit for receivers 18 , which might otherwise be easily lost because of their small size. An added convenience is that a user can thread fly line 12 through receiver 18 and tie knot 60 while the receiver 18 is held on card 72 , thus reducing the risk of dropping and losing the receiver 18 while tying on fly line 12 . In one embodiment, receivers 18 are integrally molded with card 72 , leaving connecting members 74 and 76 at end 62 and end 26 of each receiver 18 , respectively. In one embodiment, each connecting member 74 and 76 secures the respective receiver 18 to card 72 during routine handling, but is easily broken with manual force for the removal of a receiver 18 from card 72 .
In one embodiment, card 72 includes tool 78 to facilitate the connection of barb 16 and receiver 18 . Tool 78 includes slot 80 and a slot terminus. In the illustrated embodiment, the slot terminus is a shaped orifice 82 , similar to shaped orifice 66 of FIG. 6 . In one embodiment, card 72 includes orifice 84 as an attachment means to allow a user to secure card 72 to the user's clothing, for example. In an exemplary embodiment, card 72 is about 3-⅜ inches (85.7 mm) long, about 2-½ inches (63.5 mm) wide and has a thickness of about ⅛ inch (3.2 mm). While five receivers 18 are illustrated, it is contemplated that more or fewer may be provided on a single card 72 .
FIG. 8 is a partial perspective view illustrating use of connector holding tool disposed 78 on card 72 in a second embodiment of a connection method. In one method of use, a user slides leader 14 through slot 80 to orifice 82 so that barb 16 rests in orifice 82 . The shape of orifice 82 closely mates with the exterior shape of barb 16 to prevent rotation of barb 16 within orifice 82 . With barb 16 thus held, the user can then attach receiver 18 . The use of receiver holder 65 ( FIG. 6 ) is especially helpful because of the difficulty of handling the very small receiver 18 . In an exemplary embodiment, orifice 82 has a diameter of about 0.116 inch (2.95 mm) and slot 80 has a width of about 0.053 inch (1.35 mm).
FIG. 9 is a partial perspective view illustrating use of a connector holding tool disposed on the card of FIG. 7 in a third embodiment of a connection method. In the method illustrated in FIG. 9 , receiver 18 is inserted into orifice 82 of tool 78 . In this embodiment, tool 78 of card 72 holds receiver 18 to facilitate the insertion of barb 16 into receiver 18 . The shape of orifice 82 closely mates with the exterior shape of receiver 18 to prevent rotation of receiver 18 within orifice 82 . With receiver 18 thus held, the user can then attach barb 16 . The use of barb holder 64 ( FIG. 6 ) is especially helpful because of the difficulty of handling the very small barb 16 .
Although the present invention has been described with reference to preferred embodiments, workers skilled in the art will recognize that changes may be made in form and detail without departing from the spirit and scope of the invention. For example, while a flange and ridge connection is illustrated, it is also contemplated that the invention can use other types of releasable connections. For example, a threaded or other type of connection using a rotary motion to connect the barb and receiver may be used. | A splice system for linear connection of fishing lines includes a female connector and a male connector. Each connector has first and second opposite ends, a longitudinal axis, and a shaped exterior surface. The first end of the female connector is connected to a first fishing line section; the second end has a first opening; and the connector has a raised interior feature. The second end of the male connector is connected to a second fishing line section; the first end is configured for coaxial insertion into the first opening of the female connector, and the first end has a raised exterior feature. The connectors have a first relative position representing a disengaged state and a second relative position representing an engaged state. The first relative position and the second relative position are rotationally displaced about the axis. | 8 |
FIELD OF THE INVENTION
The present invention relates to remediation of waste water collection systems such as sewage systems and grease traps. This invention more particularly pertains to a bioremediation device and a process for initially reducing the grease and other organic materials in the collection system and then maintaining the remediation effect in the collection system.
BACKGROUND OF THE INVENTION
Description of Related Art
Modern progress has necessitated the development and use of waste collection systems as an alternative to unabated sewage disposal. Such collection systems are necessitated by the inherent limitations of residential and commercial sewage systems. Most of today's sewage systems are not able to accept either the quantities or the varying types of raw sewage produced from residential and commercial facilities. Simply, the output of residential and commercial sewage has outpaced the acceptable capacity for these sewage systems. Moreover, the contents of the sewage itself often makes unrestricted disposal and collection impractical or outright hazardous.
As a result of the increasing and undue strain placed on community sewage systems, limitations have been placed on both the quantities and types of waste which may be properly disposed in these systems. For example, state and local municipalities have placed limitations on the quantities of oil and grease which may be introduced into municipal sewage collection systems. Most commercial businesses are required to maintain a grease trap to collect the grease, thereby preventing most of the grease from entering the sewage system. The grease or other organic waste is collected in the trap where the organic material will naturally decompose or eventually be removed and reclaimed along with the non-organic waste. However, in an effort to minimize both the accumulation as well as efforts to remove the collected waste in these traps, the use of remediation devices has been implemented that introduce bacterial supplements into the collection system. The bacterial supplements reduce the amount of grease and maximize organic decomposition.
Presently, commercially available bioremediation devices are commonly used to remediate waste collections systems such as sewage systems and grease traps. The term "bioremediation" refers to a biological process wherein grease and other organic matter are converted to carbon dioxide and water. However, these known remediation devices inadequately address today's needs. Such remediation devices are unsuited for reducing the accumulated waste materials to a level where the collection system can then be adequately maintained. Moreover, as a result of the increasing use of waste collection system, the demand for removal of accumulated waste has equally increased. Therefore, extended periods of time between reduction and/or removal of the accumulated waste often exacerbates waste handling problems.
It is known to place a bacterial incubator in a collection system to facilitate organic reduction of waste materials. For example, U.S. Pat. Nos. 4,670,149 and 4,925,564 to Frances disclose bacterial incubator devices providing a large surface area intended to facilitate bacterial growth within the sewage collection system. The bacteria enter the system by passing through the enclosure and are intended to indiscriminately attack the contents of the collection system without regard to distinguishing particular contents or providing relatively rapid short-term bioremediation followed by maintenance of remediating bacteria and enzymes in the system.
In response to the realized inadequacies of these earlier remediation devices, it became clear there is a need for a bioremediation device which will individually address the waste material as well as the waste water throughout the collection system. This device must have a variable capacity to provide relatively rapid introduction of bacteria and enzymes, or both, into the waste water to initiate remediation of organics such as grease or the like. Once the organic waste materials have been substantially reduced, the remediation device should maintain remediating bacteria or enzymes in the waste water in the collection system by replenishing the remediating agents that are diminished or flow out the system.
BRIEF SUMMARY OF THE INVENTION
The present invention alleviates or solves the above-described problems in the prior art by providing an improved bioremediation device and process. The present device satisfies the need for a more effective remediation device having a variable capacity to initiate relatively rapid remediation of organic waste materials such as grease and accumulated surface scum, and to maintain remediation in the waste water in a system.
In accordance with the invention, this object is accomplished by providing a remediation device of the above kind in that a bioactive element is deposited within the collection system. The bioactive element has active ingredients of variable strength and concentration. The bioactive element is strongest when initially placed within the waste collection system, in order to provide a relatively powerful remediation device to reduce organic waste materials, such as grease or scum, throughout the system. The effect of the bioactive element diminishes as a result of the waste material being reduced. However, the bioactive element then yields bacteria or enzymes in sufficient concentration to maintain bioremediation in the collection system. Expended bioactive elements are periodically replaced so that the system is continuously maintained.
Preferably, the bioactive element of the present invention comprises a dissolvable outer portion of active ingredients and a dissolvable inner portion of active ingredients. In comparison to the ingredients of the inner portion, the ingredients of the outer portion are stronger or more concentrated, and thus are more effective removing waste materials such as scum near the surface of the collection system. The inner portion is positioned within the outer portion such that once the majority of the surrounding outer portion has dissolved into the collection system, the inner portion of reduced concentration relative to the outer portion becomes exposed to the contents of the collection system.
The bioremediation device comprising a bioactive element that is soluble in the waste material and has at least one active ingredient present in a variable concentration, the variable concentration being greatest substantially at the outside of said element and being least within the element, so that the bioremediation effect of the element is greatest when the waste material is first exposed to the outside of the element and lessens while the element dissolves in the waste materials, whereby the outside of the bioactive element has a relatively great bioactive effect for remediating the waste material and the inside of the bioactive element has a relatively lesser bioremediating effect for maintaining the waste material in the collection system.
A remediation device formed in accordance with the present invention has a number of advantages. An important advantage of the novel remediation device is its ability to initially treat the organic contents of the waste container with a relatively high concentration of bioremediating agents.
Accordingly, an object of this invention is to provide an improvement which overcomes the aforementioned inadequacies of the prior art devices and provides an improvement which is a significant contribution to the advancement of the remediation device art.
Still another object of the present invention is to provide a structurally simple and economical device for remediating waste collection systems.
Yet another object of the present invention is to provide a bioremediation device for biological degradation of a predetermined waste material in a collection system.
The foregoing has broadly outlined some of the more pertinent objects and features of the invention. These should be construed to be merely illustrative of some of the more prominent features and applications of the intended invention. Many other beneficial results can be obtained by applying the disclosed invention in a different manner or by modifying the disclosed embodiments. Accordingly, other objects and a more comprehensive understanding of the invention may be obtained by referring to the detailed description of the preferred embodiment taken in conjunction with the accompanying drawings, in addition to the scope of the invention defined by the claims.
It should be appreciated by those skilled in the art that the conception and the disclosed specific embodiments may be readily utilized as a basis for modifying or designing other structures or methods for carrying out the same purposes of the present invention. It should also be realized by those skilled in the art that such equivalent constructions do not depart from the spirit and scope of the invention as set forth in the appended claims.
For a more succinct understanding of the nature and objects of the present invention, reference should be directed to the following detailed description taken in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front perspective view of a preferred embodiment of the present invention suspended in a waste collection system.
FIG. 2 is a front cross-section view of the bioactive element in the embodiment of FIG. 1.
FIG. 3 is a front elevation view of the present invention in an alternative embodiment.
FIG. 4 is a cross section view taken along line 4--4 of FIG. 3.
FIG. 5 is a front perspective view of the present invention in another alternative embodiment.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
As shown in FIG. 1, a bioremediation device shown generally at 10 comprises a dissolvable bioactive element 12 suspended from the top of a waste collection system for collecting waste material 16 such as waste water and accumulated surface scum including oil and grease. The device is immersed in the waste material. The bioactive element 12 is enclosed within a netting 20 which allows the active ingredients 24 of that element to dissolve directly into the waste material. The bioactive element is suspended from the collection system on a flexible line 30 having a first end 31 and a second end 32. The flexible line is preferably of a material that will permanently retain the bioactive element in the collection system until the device 10 is removed therefrom by the user.
The first end 31 of the line includes a clasp 34 for detachably securing to a loop 24 formed from the netting 20. A tie 22 (FIG. 2) gathers a portion of the netting above the bioactive element to form the loop 24. The netting preferably is made of any suitable foraminous material permits substantially unimpeded exposure of the bioactive element to the waste material and waste water within the collection system. Moreover, in the preferred embodiment, the netting should be able to be shaped in order to form the loop. The tie may be of any suitable material such as a plastic tie or ring which will tie off a portion of the netting.
The second end 32 is detachably secured to a cover 26. To position the bioremediation device of the present invention within the collection system, the bioactive element within the netting is lowered into the collection system on the flexible line 30 through an opening 14 in the top of the collection system. The cover 26 closes an existing access opening to a grease trap or similar collection system.
Preferably, the weight of the device is approximately 10 pounds. The weight of the bioremediation device keeps the bioactive element submerged in the waste material as a result of having a specific gravity greater than 1. However, as the bioactive element dissolves, the device will float to the surface as a result of reduced weight and the natural buoyancy of the netting, to indicate the bioactive element has almost substantially been consumed and that the bioactive element has therefore approached the end of its useful life. Thus, the present embodiment provides an easy way of determining the bioactive element change-out time and to calculate the amount of product needed to treat a given collection system.
In order to remove the expended bioremediation device 10 once the bioactive element has substantially dissolved, the flexible line and netting are pulled back through the opening in the collection system. The spent device 10 may be replenished by placing a fresh such device through the opening.
The variable concentration of at least one active bioremediation ingredient differs throughout the bioactive element 12. It is an important aspect of the invention that a portion of the bioactive element be operative at a relatively high concentration to initially reduce the accumulated waste material 16, and at least another portion be operative at a relatively lower concentration to maintain a lower amount of bacteria and enzymes in the collection system once the waste material has been substantially reduced. To initially reduce the waste material 16, the concentration is significantly greater than the concentration required to maintain the system once the waste materials are initially reduced. The bioactive element of the present invention may be implemented by bacteria and/or enzymes having a capacity for organic reduction and organic maintenance.
As illustrated in FIG. 2, the bioactive element 12 comprises an inner portion 40 and an outer portion 50. The outer portion as shown in the embodiment of FIGS. 1 and 2 is a cylindrical element in the shape of an annulus having an axial hole therethough. The inner portion is a solid that fills the axial hole of the outer portion. The outer portion surrounds the inner portion, thereby limiting the ability of the inner portion to dissolve in the waste material until the outer portion is substantially dissolved. The outer portion preferably is formed from a mold of the desired dimensions, and the outer portion then acts as a mold when forming the inner portion.
In an actual embodiment, the outer portion is approximately 6.5 to 7.0 inches in height and has the shape of an annulus having a thickness of approximately 6 inches. The overall radius of the element is approximately 3 inches wide, thereby leaving an inner radius of 1.5 inches for receiving the inner portion. Thus, the inner portion is sized by the inner confines of the outer portion. Preferably, the inner portion is also 6.5 to 7.0 inches in height and 3 inches wide. As can best be seen in FIG. 2, portions of the inner portion are exposed or revealed from within the outer portion prior to use. The ends of the inner portion are exposed prior to being deposited and dissolved in the waste collection system.
In the preferred embodiment, the outer portion and the inner portion each comprise a blend of biodegradable surfactants which are able to easily structurally degrade by a natural degradation process. A portion of the outer portion may be a surfactant commonly known as forty percent solution sodium 2-ethylhexyl sulfate which is an anionic surfactant carrying a negative charge on the hydrophilic portion in the form of sulfate. This surfactant should preferably make up 8% to 15% by weight of the outer portion. The chemical structure of this surfactant is:
R--O--(CH.sub.2 CH.sub.2 O).sub.n SO.sub.3 m
where R=fatty alkyl or alkylaryl group, N=moles of ethylene oxide, and m=counter ion: Na, NH 4 , Mg, triethanolamine, etc. The market name for this surfactant is Rhodapon BOS™, which can be purchased through the Rhone Poulenc Company at 7500 Prospect Plains Road, Cranbury, N.J. 08512 USA.
Also included in the blend making up the outer portion is 1% to 5% by weight of sodium alpha olefin sulfonate having the chemical structure:
CH.sub.3 (CH.sub.2).sub.N --CH═CH--CH.sub.2 --SO.sub.3 Na.
This surfactant may be acquired under the name Bioterge AS-90™, which can be purchased through the Stephan Company at Edens and Winnetka Roads, Northfield, Ill. 60093 USA.
Additionally, the outer portion of the blend contains a blended surfactant of 2% to 4% by weight having the make up of a disodium wheat germamphodiacetate which is known under the name Mackam 2W, produced through the McIntyre Group Ltd. at 1000 Governors Highway, University Park, Ill. 60466 USA.
A 3% to 4% by weight portion of sodium thiosulfate anhydrous powder is also part of the outer portion in a preferred embodiment. Also included in the blend of the outer portion is forty percent solution powdered bacteria with a count of no less than 50 billion colony forming units (CFUs) per gram. The preferred bacteria is facultative in nature, in that it has the ability to grow with or without the presence of oxygen. The preferred genesis of the strand of bacteria used in the present invention is, but is not limited to, Bacillus Licheniformis, Bacillus Subtilis, Bacillus Amyloliquiefaciens, Bacillus Polymyxa, Pseudomonas Aeruginosa, Pseudomononas Statzeri, Pseudomonas Fluoresceni, Escherichia Hermanii, Bacillus Cereus, Bacillus Thuringiensis, and Bacillus Meg'afarium.
The blend of the outer portion may further include a citric acid powder from 1% to 2% by weight and a vitamin package of approximately 1% to 3% by weight. The vitamin package may comprise, but is not limited to, vitamins A, D, E and K. The remaining portion of the blend making up the outer portion should be made up of sodium sulfate anhydrous powder.
The blend of the outer portion is prepared by blending together the ingredients described above using a mixing apparatus (not shown) capable of mixing viscous liquids. The ingredients of the outer portion are mixed for no less than 30 minutes. The blend is then deposited into the mold designed for manufacturing the outer portion with the aforementioned dimensions where it is allowed to set up for no less than 3 hours.
In a preferred embodiment, the inner portion should similarly comprise the same ingredients and in the same proportions with the following exceptions. The inner portion should comprise 8% to 15% by weight of forty percent solution sodium 2-ethylhexyl. Moreover, the inner portion should comprise of twenty percent solution powdered bacteria with a count of no less than 50 billion CFUs per gram. The present invention is formulated to give the maximum strength dosage of bacteria through the outer portion. The blend of the inner portion is also mixed in a mixing apparatus that is capable of mixing viscous liquids. The inner portion blend is also mixed for no less than 30 minutes and then is dispensed into the center of the outer portion that was previously prepared and which now functions as a mold for forming the inner portion. The inner portion should be allowed to set up within the outer portion for no less than 3 hours.
Preferably, the bioactive element is configured to dissolve in approximately 90 days within systems having flow under 50,000 gallons per month. For systems having a flow of up to 100,00 gallons per month, the element should dissolve in approximately 60 days. For systems having a flow of up to 150,000 gallons per month, the element should dissolve in approximately 30 days.
It should be understood that the nature and amounts of the ingredients, as well as the physical dimensions of the device, are exemplary of the preferred embodiment, and are not meant to limit the practice of the present invention.
The bioactive element of the present invention is not limited to any particular shape. As can be seen in FIGS. 3 and 5, the present invention may be spherical or rectangular. FIG. 4 is a cross-sectional view of the spherical bioactive element shown in FIG. 3. FIG. 4 shows, in particular, that the variable concentration varies in a gradual manner, unlike the stepped variation from outer to inner portions shown in FIGS. 1 and 2 with the concentration greatest substantially at the outside of the element and least at or near the innermost part of the solid.
The use of the bioremediation device 10 as described above constitutes an inventive method of the present invention in addition to the bioremediation device 10 itself. In practicing the method of bioremediating a waste collection system with the bioremediation device 10 as described above, the steps include providing a bioactive element of the type described above into the waste material. The method then includes the step of reducing the waste materials in the collection system as described above. The method also includes the step of maintaining the waste material in the collection system as described above. The step of reducing the waste material may comprise dissolving the outer portion of the bioactive element or charge and the step of maintaining the waste material may comprise dissolving the inner portion of the bioactive element or charge. The process of the present invention rejuvenates the waste collection system.
The present invention has been illustrated in great detail by the above specific examples. It is to be understood that these examples are illustrative embodiments and that this invention is not to be limited by any of the examples or details in the description. Those skilled in the art will recognize that the present invention is capable of many modifications and variations without departing from the scope of the invention. Accordingly, the detailed description and examples are meant to be illustrative and are not meant to limit in any manner the scope of the invention as set forth in the following claims. Rather, the claims appended hereto are to be construed broadly within the scope and spirit of the invention. | A bioremediation device and process for remediation of waste collection systems. The present invention preferably comprises an bioactive element having an outer and an inner portion. The concentration of the bioactive element in the outer portion differs from that of the inner portion so that the concentration is greatest when the waste material is first exposed to the outside of the element and diminishes while the solid dissolves in the waste material. The outer portion is disposed about the inner portion such that substantially all of the outer portion is dissolved for delivery of the bioactive element into the waste material before dissolution of the inner portion occurs. The outer portion has a relatively great bioactive effect for remediating the waste material and the inner portion has a relatively lesser bioremediating effect for maintaining the waste material in the collection systems. | 2 |
This application is a division of application Ser. No. 09/078,659, filed May 14, 1998, (now U.S. Pat. No. 5,925,160) which application is, in turn, a divisional of Ser. No. 08/784,924, filed Jan. 16, 1997 (now U.S. Pat. No. 5,783,507.
FIELD OF THE INVENTION
The present invention relates to ceramic enamel compositions for use in automotive windshields, sidelights and backlights.
BACKGROUND OF THE INVENTION
Ceramic enamel compositions can be used for a variety of applications, such as decorative coatings for glassware, chinaware, and the like. They are especially useful in forming colored borders around glass sheets used for automotive windshields, sidelights and backlights. The colored borders enhance appearance as well as prevent degradation of underlying adhesives by UV radiation.
In general, these enamel compositions consist mainly of a glass frit, a colorant and an organic vehicle. They are applied to a desired region of the substrate and subsequently fired to burn off the organic vehicle and fuse the ceramic solids to the surface of the substrate.
Glass sheets for automotive use are generally coated in the desired region with the ceramic enamel composition and then subjected to a pressure forming process at elevated temperatures. During this treatment the enamel melts and fuses to the glass substrate and the glass is formed into a desired final shape. However, many previous coatings exhibit a tendency to adhere to the materials covering the forming die, e.g., a fiberglass or metal fiber covered die, because these conventional enamels have a low viscosity after melting and tend to stick to other materials at high temperature. Accordingly, such previous enamels are not suitable for use in glass forming processes in which the heated glass coated with enamel is pressure formed with a die.
Various approaches have been suggested in order to facilitate the forming of glass sheets with a ceramic enamel coated thereon with-out the enamel adhering to the forming die. For example, U.S. Pat. Nos. 4,596,590 and 4,770,685 (issued to Boaz) propose the addition of a low valent metal oxide powder, e.g., cuprous oxide, to the paint composition to provide a non-stick barrier between the coating and the fiberglass-covered forming die. U.S. Pat. Nos. 4,684,389; 4,857,096; 5,037,783 and EP 490,611 (issued to Boaz), propose adding finely divided zinc metal powder for a similar effect. The use of an iron metal powder is proposed in U.S. Pat. No. 4,983,196 (issued to Stotka).
A purportedly improved anti-stick ceramic enamel composition is proposed by U.S. Pat. Nos. 5,153,150; 5,208,191 and 5,286,270 (issued to Ruderer et al.) wherein a seed powder containing Zn 2 SiO 4 is combined with the glass frit portion of the composition. The glass frit portion comprises at least 35 percent by weight precursors for crystalline Zn 2 SiO 4 , more particularly, at least 30 weight percent ZnO and at least 5 weight percent SiO 2 .
A further shortcoming of a number of previous ceramic enamel systems is that they employ a lead-containing glass frit. For environmental considerations it is desirable to avoid the use of any lead-containing system.
Along these lines, U.S. Pat. No. 4,882,301 (issued to Gettys et al.) proposes use of a crystallizing amount of Cd 2 SiO 4 with a lead borosilicate glass. This reference states that Zn can be substituted directly for Cd in the glass formulation; however, U.S. Pat. No. 5,208,191 indicates that when zinc is substituted for cadmium, the results have been less than desirable.
Also, while several of the above-mentioned enamel systems may perform satisfactorily in conventional glass forming processes, some may not be suitable for use in the newly-developed "deep bend" processes for forming automotive glass. Moreover, the enamel compositions, must resist certain chemical agents which they may contact.
The previous enamel compositions suffer from one or more of the deficiencies noted above. In contrast, the present invention provides a ceramic enamel composition that avoids these shortcomings.
SUMMARY OF THE INVENTION
The present invention is for a lead-free ceramic enamel composition that forms an at least partially crystallizing zinc silicate material on a glass substrate upon fusing at high temperature.
A ceramic enamel composition of the present invention comprises 40-80% by weight of at least one lead-free metal oxide glass frit which contains precursors of Zn 2 SiO 4 , e.g., ZnO and SiO 2 , of 0.05-15% by weight of a zinc silicate seed material, and 20-35% by weight of a black pigment. The sum of the weight percentage amounts of the aforementioned precursors of Zn 2 SiO 4 provided by one or more frits is less than about 35%, and more than about 15% by weight of the frit or frits.
The zinc silicate seed material of an instant composition is preferably provided as seed crystals in the composition, which upon firing provide nuclei for further crystal growth. It is preferred that at least a portion of the zinc silicate seed material is crystalline in nature. Preferably, the crystalline seed material comprises at least about 95% by weight of crystalline Zn 2 SiO 4 , for instance, approximately 100% by weight of crystalline Zn 2 SiO 4 .
Another aspect of the invention involves including an additional crystalline material, such as a bismuth silicate seed material, in an enamel composition of the invention. A bismuth silicate seed material is preferably provided in at least about 1% by weight of the enamel composition. Preferably, the bismuth silicate seed material comprises a crystalline bismuth silicate, such as crystalline Bi 12 SiO 20 , Bi 4 (SiO 4 ) 3 , Bi 2 SiO 5 , and mixtures thereof, in an amount of about 2 to about 7% by weight.
A method of preparing an instant ceramic enamel composition comprises combining in no particular order the aforementioned components in the desired amounts, and optionally combining them with an organic vehicle.
The present invention also contemplates a method of using the aforementioned ceramic enamel with a glass substrate, e.g., to form a colored border and/or UV resistant border around its periphery. Thus, a glass substrate is provided with a ceramic enamel coating by applying an aforementioned ceramic enamel composition to the glass substrate, optionally applying pressure to the coated glass substrate, and firing the substrate to fuse components of the ceramic enamel composition to the substrate. Among the advantages of an instant enamel are its excellent anti-stick properties, good consistency, broad temperature firing range, low stress, and low cost.
The invention will now be described in more detail with reference to examples.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides a ceramic enamel composition that contains the following components: (1) at least one conventional lead-free oxide glass frit containing precursors of Zn 2 SiO 4 ; (2) a zinc silicate seed material; (3) a colorant (pigment); and, optionally, (4) a vehicle for components (1)-(3). The zinc silicate seed material is believed to assist in nucleating and growing microcrystalline structures, e.g., crystalline zinc silicate phases, in the composition upon firing. Although vehicle (4) is preferably provided in the composition, it can be omitted, and applied later, e.g., at the time of silkscreening, without departing from the essence of the present invention.
Typically, an instant ceramic enamel composition comprises 40-80% by weight of one or more of the aforementioned lead-free oxide glass frits, 0.05-15% by weight of a zinc silicate seed material, and 20-35% by weight of a pigment. More preferably, the lead-free oxide frit is provided in the composition in an amount of 60-65% by weight, the zinc silicate seed material is provided in an amount of 1-5% by weight, and the pigment is provided in an amount of 25-33% by weight. The sum of the weight percentage amounts of the precursors of Zn 2 SiO 4 provided by one or more of the aforementioned frits is less than about 35% by weight of the frit or frits, and the total of weight percentages of the above-mentioned lead-free metal oxide frit(s), zinc silicate seed material, and pigment does not exceed 100%.
Preferably, an instant ceramic enamel composition comprises 60-63% by weight of a lead-free metal oxide frit or frits containing precursors of Zn 2 SiO 4 , 1-3% by weight of a zinc silicate seed material, and 27-30% by weight of a black pigment. It is also preferred that the total of the weight percentages for the precursors of Zn 2 SiO 4 provided by one or more frits is less than about 35% by weight, but greater than about 20% by weight.
As for the ratio of Zn 2 SiO 4 precursors in the glass frit or frits, preferably, the amount of zinc oxide and silicon dioxide provided in an aforementioned at least one lead-free frit is 5-20% and 20-30%, respectively, whenever the total amount of Zn 2 SiO 4 precursors is 35% by weight. More preferably, the amount of zinc oxide provided in the frit or frits is in the range of 10% to 15%, and the amount of silicon dioxide provided in the frit or frits is in the range of 20% to 25%, whenever the total amount of Zn 2 SiO 4 precursors is less than about 35% by weight. The zinc precursor can be provided solely by one frit and the silicon precursor can be provided by a different frit, as long as Zn 2 SiO 4 is formed whenever the enamel composition is fused.
By "precursors of Zn 2 SiO 4 " is meant substances that when fired at high temperature react to form Zn 2 SiO 4 . Chief among such precursors are ZnO and SiO 2 . Other precursors can be used equivalently to these substances, and are readily apparent to those skilled in the art. Such other precursors include polymers, e.g., siloxanes, and discrete compounds, e.g., organometallic compounds, which decompose to form ZnO or SiO 2 upon firing at elevated temperature. The ZnO and SiO 2 , or parent compounds, can be provided either in the same lead-free frit, or in different frits, which upon firing fuse to generate Zn 2 SiO 4 .
The zinc silicate seed material can be selected from any known phase of the Zn/Si phase system; however, zinc orthosilicate (Zn 2 SiO 4 ) is preferred. Preferably, the zinc silicate seed material comprises at least about 90% by weight of crystalline Zn 2 SiO 4 . More preferably, the zinc silicate seed material comprises at least about 95% and up to 100% by weight of crystalline Zn 2 SiO 4 .
As referred to herein, the terms crystal, crystalline, microcrystalline, and the like, mean that the subject material is sufficiently crystalline (ordered) to reveal one or more discrete phase by X-ray diffraction techniques.
While not wishing to be bound by theory, it is believed that the presence of the zinc silicate seed material causes nucleation and growth of crystals leading to increased refractoriness and devitrification. The devitrification involves the separation of microcrystalline structures, such as Zn 2 SiO 4 , and the like, in the fused enamel. The presence of these microcrystalline structures in the fused enamel is believed to greatly reduce the tendency of the enamel to stick to surfaces, e.g., pressing pads, during the shaping of the glass substrate at elevated temperature.
In respect to a lead-free oxide frit employed in the invention, a conventional ceramic oxide frit, such as a zinc-bismuth based frit, can be employed. The frit can contain a boron source in addition to a zinc source. For instance, a frit composed of zinc oxide and boron oxide, and optionally additional materials, can be used. Also, a frit composed of zinc borosilicate, or one composed of a noncrystalline zinc silicate material, can be used. Preferably, such a frit is formulated to generate in situ upon heating the requisite zinc silicate microcrystalline structures. In practice it is preferred to include a crystalline zinc silicate seed material directly in the enamel composition. At least some oxide frit is desirable in the composition in order to provide a flux.
A crystalline zinc silicate material suitable for use in the present invention can be prepared according to any of a number of well-known methods. For instance, Zn 2 SiO 4 (CAS Registry No. 13597-65-4) can be prepared by heating zinc oxide (ZnO) and SiO 2 in a molar ratio of 2:1 at 1300° C. for 72 hours. Other methods of preparing these and related materials are readily apparent to the skilled practitioner.
The particle size for an instant zinc silicate seed material is preferably in the range of 1 to 4 microns, more preferably about 1.8 microns.
Typically, it is preferred also to include a bismuth silicate seed material in an instant composition. While not wishing to be bound by theory, it is believed that the presence of the bismuth silicate seed material causes nucleation and growth of crystals leading to increased refractoriness and devitrification. Devitrification involves the separation of microcrystalline structures, such as Bi 12 SiO 20 , Bi 2 (SiO 3 ) 4 , and the like, in the fused enamel. The presence of these microcrystalline structures in the fused enamel is believed to help reduce the tendency of the enamel to stick to surfaces during the shaping of the glass substrate at elevated temperature.
Preferred bismuth silicate seed materials for this type of reactive system can include, but are not limited by, the compounds Bi 12 SiO 20 , Bi 4 (SiO 4 ) 3 , Bi 2 SiO 5 , and mixtures thereof. Any one or all of these compounds are preferably crystalline and may be present as a mixture within the same crystalline material.
A crystalline bismuth silicate material suitable for use in the present invention can be prepared according to any of a number of well-known methods. For instance, Bi 12 SiO 20 (CAS Registry No. 12377-72-9) can be prepared by heating bismuth oxide and silicon dioxide in a 6:1 molar ratio at up to 840° C. for 16 hours [National Bureau of Standards, Monogr., 25:22 (1985)]. Bi 4 (SiO 4 ) 3 (CAS Registry No. 15983-20-7) can be prepared by firing a 2:3 ratio of bismuth oxide and silica at 780° C. for 50 hours, regrinding, and firing at 830° C. for 18 hours [Roob, et al., North Dakota State Univ., JCPDS Grant-in-Aid Report (1980)]. Bi 2 SiO 5 (CAS Registry No. 12027-75-7) can be prepared by melting a 1:1 ratio of bismuth oxide and silicon dioxide at 1000-1040° C., quenching in water, and crystallizing at 400-520° C. for one week [Keller, et al., Mineralogisch-Petro-graphisches Institut, Univ. Heidelberg, Germany, JCPDS Grant-in-Aid Report (1984)]. Other methods of preparing these and related materials are readily apparent to the skilled practitioner.
The particle size for an instant bismuth silicate seed material is preferably in the range of 1 to 4 microns, more preferably about 1.8 microns.
Additional crystalline materials can be incorporated in the formulation as fillers, such as alumina-silicate compounds, calcium silicate compounds, boro-alumina-silicate compounds, soda-calcia-alumina-silicate compounds, feldspar compounds, titania, zinc borate, and mixtures thereof. Still further metallic and/or oxide materials, e.g., iron, silicon, zinc, and the like, can be added to enhance desired properties, such as resistance to silver bleed-through, especially when their presence promotes the nucleation and growth of the requisite zinc silicate and bismuth silicate microcrystalline structures.
As presently preferred, an enamel composition of the invention contains a base glass frit which is at least one conventional lead-free frit, such as those commercially available from Cerdec Corporation (Washington, Pa.). Such frits can be employed alone or can be blended to achieve the desired properties. Other suitable zinc-containing frits are well-known in the art.
A representative formulation for a suitable lead-free frit of the present invention has a composition as shown in Table I:
TABLE I______________________________________Oxide Weight % Range______________________________________ZnO 3-15SiO.sub.2 10-25Bi.sub.2 O.sub.3 20-55B.sub.2 O.sub.3 2-20Na.sub.2 O 1-10K.sub.2 O 0-3Li.sub.2 O 0-3Cao 0-10SrO 0-10TiO.sub.2 0-5Al.sub.2 O.sub.3 0-5ZrO.sub.2 0-5F.sub.2 0-3______________________________________
A method of making a frit of this type is disclosed in U.S. Pat. No. 5,346,651 (issued to Oprosky et al.). Such frits have a sufficiently low firing temperature to ensure adequate adhesion to the substrate and also possess low density characteristics.
Exemplary zinc-containing frits suitable for use with the invention are commercially available from Cerdec Corporation as E-8018, E-8009, and E-8008.
A pigment of a ceramic enamel of the invention can be any of those commercially available. Particularly preferred pigments are commercially available from Cerdec Corporation as *2991 pigment, which is a copper chromite black pigment, *2980 pigment, which is a cobalt chromium iron black pigment, and *2987 pigment, which is a nickel manganese iron chromium black pigment.
A vehicle to be employed for use with an instant composition is selected on the basis of its end use application. The vehicle should adequately suspend the particulates and burn off completely upon firing of the composition on the substrate. Vehicles are typically organic and include compositions based on pine oils, vegetable oils, mineral oils, low molecular weight petroleum fractions, tridecyl alcohol, synthetic and natural resins, and the like.
Correspondingly, UV-base vehicles are equally applicable for use in the invention. Such UV-base vehicles are well-known in the art and are generally composed of polymerizable monomers and/or oligomers containing, for example, acrylate or methacrylate functional groups, together with photoinitiators and polymerization inhibitors. Representative vehicles are disclosed in U.S. Pat. Nos. 4,306,012 and 4,649,062. As is recognized, such vehicles are cured with ultraviolet radiation after application to the substrate.
The specific vehicle and amounts employed are selected based upon the specific components of the composition and the desired viscosity. In general, the amount of the vehicle is about 10 to about 40% by weight based upon the total weight of the solid enamel composition.
In general, the enamel compositions are viscous in nature, with the viscosity depending upon the application method employed and the end use. For purposes of screen-printing, viscosities ranging from 10,000 to 80,000, and preferably 35,000 to 65,000, centipoises at 20° C., as determined on a Brookfield Viscometer, #7 spindle at 20 rpm, are appropriate.
To prepare an enamel composition of the invention, a frit is ground to a fine powder using conventional methods and is combined in any order with an aforementioned zinc silicate seed material, a pigment, any bismuth silicate seed material, and any fillers. When the zinc silicate seed material of the composition is desired to comprise a crystalline zinc silicate, it is also added. Other oxides, as discussed above, can be added, as well as materials which resist silver bleed-through. More than one representative of each of the different types of components mentioned above can be provided in the enamel composition.
Once the enamel composition is prepared it can be applied to a glass substrate in a conventional manner, such as by screen printing, decal application, spraying, brushing, roller coating, and the like. Screen printing is preferred when the composition is applied to glass substrates.
After application of the composition to a substrate in a desired pattern, the applied coating is then fired to bond the enamel to the substrate. The firing temperature is generally determined by the frit maturing temperature, and preferably is in a broad temperature range. Typically, the firing range for an instant composition is in the range of 1100-1350° F., more preferably in the range of 1200-1300° F., and most preferably about 125° F. Whenever pressure is applied to the substrate, the pressure is typically in the range of 1 to 3 psi, preferably about 2 psi.
The following examples represent preferred embodiments of the invention. They are presented to explain the invention in more detail, and do not limit the invention.
EXAMPLES
Several exemplary enamel compositions were prepared by conventional methods using the components listed in Table II. The indicated weight percentages are calculated based on a printing medium being excluded from the composition. Frit E-8018 referred to in Table II is a lead-free bismuth-borosilicate frit commercially available from Cerdec Corporation, which has a ZnO content of 14.4 and an SiO 2 content of 20.1% by weight. Pigment *2991 is a black pigment commercially available from Cerdec Corporation. Zinc silicate seed was prepared by reacting zinc oxide and silicon dioxide as described, with X-ray diffraction analysis indicating the presence of zinc orthosilicate. Bismuth silicate seed was prepared by reacting bismuth trioxide and silicon as described with X-ray diffraction analysis indicating the presence of eulytite. Identical materials were used for each component in the examples.
TABLE II______________________________________Component Ex. 1 Ex. 2 Ex. 3 Ex. 4______________________________________E-8018 63.64 63.64 63.64 62.00*2991 pigment 30.30 30.30 30.30 26.00Bismuth silicate seed 5.00 4.00 3.03 5.00Zinc silicate seed 1.06 2.06 3.03 7.00______________________________________
The present invention has been described above by way of illustration with reference to examples. However, it should be appreciated that the invention is not limited to the particular embodiments set forth above and that certain obvious modifications can be practiced within the scope of the appended claims. | A ceramic enamel composition contains 40-80% by weight of at least one lead-free metal oxide frit containing precursors of Zn 2 SiO 4 , such as ZnO and SiO 2 , wherein the amount of Zn 2 SiO 4 precursors is less than about 35% by weight of the at least one lead-free metal oxide frit, 0.05-15% by weight of a zinc silicate seed material, and 19-37% by weight of a pigment. The zinc silicate seed material preferably contains crystalline Zn 2 SiO 4 . The enamel preferably also contains a bismuth silicate seed material. The ceramic enamel can be employed as a coating around the periphery of automotive glass and is effective in improving appearance and reducing degradation of underlying adhesives by ultraviolet radiation. | 2 |
TECHNICAL FIELD OF THE INVENTION
[0001] This invention relates to lithographic masks, such as that used for fabricating semiconductor devices.
BACKGROUND OF THE INVENTION
[0002] Lithography is utilized in semiconductor device manufacturing to pattern features on semiconductor workpiece layers for integrated circuit fabrication.
[0003] FIG. 1 shows a lithographic fabrication system 100 for defining features in a workpiece 120 , in accordance with prior art. Typically, workpiece 120 comprises a semiconductor substrate, together with one or more layers of substances (not shown) such as silicon dioxide and a resist layer 101 , affixed to a surface of workpiece 120 .
[0004] Typically, radiation of wavelength λ is emitted by an optical source 106 , such as a mercury lamp or a laser. The radiation propagates through an optical collimating lens or lens system 104 , a patterned lithographic mask 103 having a pattern of opaque and transparent features, and an optical projection lens or lens system 102 . The radiation transmitted through mask 103 is imaged by lens 102 onto resist layer 101 , thereby exposing a patterned area corresponding to the mask pattern. If resist layer 101 is positive, exposed areas will be subject to removal after development and if it is negative, exposed areas will remain intact. Thus, the pattern of mask 103 is transferred to (“printed on”) resist layer 101 . “Mask” as used herein means “mask” and/or “reticle”.
[0005] As known in the prior art, the indicated distances L 1 and L 2 satisfy, in cases of a simple lens 102 , 1/L 1 +1/L 2 =1/F, where F is the focal length of lens 102 . A pattern produced by mask 103 on resist layer 101 will be substantially in focus if resist layer 101 is a distance L 2 from projection lens 102 . This conclusion is based on a geometrical optics analysis which assumes light travels in straight lines. However, when the feature size is comparable to λ/NA, where λ is the illumination wavelength, and NA is the numerical aperture of the projection lens, a physical optics analysis should be considered which includes the wave nature of light. Under this analysis diffraction effects are likely to be produced, decreasing the image resolution even at distance L 2 , thereby reducing resolution of component features. For semiconductor devices it is desirable to maximize the number of circuit components per unit area by minimizing component size. As component size decreases, diffraction effects become more significant, thereby limiting reduction in component size. Decreased sharpness of mask images caused by diffraction effects may reduce product yield and increase device failure rate.
[0006] Diffraction effects may be severe for conventional or binary masks. FIG. 2A depicts a cross-sectional view of a prior art binary mask 10 . Binary mask 10 typically comprises a glass or quartz layer 12 with a patterned chromium layer 40 affixed thereto. The patterned chromium layer comprises a plurality of substantially transparent areas 14 , 15 and 16 and a plurality of attenuating areas 18 , 19 , 20 and 21 . Electromagnetic radiation propagating through areas 14 , 15 and 16 have electric fields associated therewith. Amplitudes of the electric fields at the mask level are represented with respect to a cross-section of the mask in FIG. 2B , wherein steps 36 , 37 and 38 correspond to electric fields from radiation propagating through apertures 14 , 15 and 16 , respectively. Because of the wave-nature of the radiation it spreads as it propagates. Therefore, even though the electric fields are separated from one another at mask level they may interfere with one another a distance away from the mask, such as at a workpiece surface. This is shown in FIG. 2C . Due to the diffraction effect, it is clear that the electric field at the workpiece surface spreads wider relative to that at the mask level. The smaller the feature sizes, as represented by transparent areas 14 , 15 , and 16 , the wider the spread.
[0007] Solid lines 22 and 24 in FIG. 2C represent electric fields from apertures 14 and 16 , respectively, and broken line 26 represents an electric field from aperture 15 . The amplitudes of the electric fields from adjacent openings ( 14 and 15 , for example) overlap in cross-hatched regions 30 and 32 . As shown in FIG. 2D , this interference or constructive addition of electric field amplitudes results in an electric field 34 which has a higher intensity at the workpiece surface in regions 30 and 32 , relative to the surrounding areas than at mask level. Therefore, there is less contrast in the light intensity distribution at the workpiece surface than at mask level, thereby reducing the resolution capability of the tool.
[0008] Undesirable diffraction effects become more significant with small dimension pattern features. “Small dimension” as used herein means small size and small spacing between transparent regions relative to λ/NA, where λ is the wavelength of the optical source and NA is the numerical aperture of the projection system.
[0009] It is known in the art to improve the system resolution by employing phase-shifting masks. The mask imparts a phase-shift to the incident radiation, typically by π radians. Phase-shifting masks generally comprise transparent areas having an optical intensity transmission coefficient T, near 1.0 at the incident radiation wavelength λ, attenuating areas or partially transparent areas having T at λ in the range of about 0.05 to about 0.15, and, optionally, opaque areas, having T less than or equal to about 0.01.
[0010] FIG. 3A depicts a cross-sectional view of a prior art π radian-phase-shifting mask 300 . Mask 300 is substantially similar to binary mask 10 but includes a phase-shifter layer 310 over transparent regions 14 and 16 . Phase-shifter layer 310 reverses the direction of the electric field vectors at apertures 14 and 16 relative to aperture 15 as shown in FIG. 3B at 320 , 322 and 330 . The π radian phase-shift is created by employing a phase-shifter layer 310 with a thickness of d=λ/2 (n−1) where λ is the wavelength of the optical source and n is the refractive index of layer 310 at π. The phase-shifter layer modifies the optical distance traveled by incident radiation, thereby producing a phase-shift. As is shown in FIG. 3C , by peaks 340 , 345 and 350 , the overlapping regions of adjacent electric fields have opposite amplitudes, and therefore, a destructive interference occurs. The cancellation of the electric field at those locations improves the contrast of the intensity field as shown in FIG. 3D . FIG. 3E depicts a vector diagram of the electric field at a workpiece level produced by radiation propagating through π radian-phase-shifting mask. Vector 380 represents an electric field from unshifted radiation such as passes through aperture 15 . Vector 390 corresponds to phase-shifted radiation such as that which propagates through aperture 14 and phase-shifter 310 . The amplitude of vector 390 equals the negative of the amplitude of vector 380 , thereby canceling it out upon interference.
[0011] Phase-shifting masks producing n radian shifts are an improvement over binary masks. However, they do not fully resolve all resolution problems, for example a phase conflict may arise for feature configurations in which a phase transmission is generally unavoidable. Whenever a phase transition occurs a dark line will result.
[0012] Electric field interference has been addressed by using a mask having a π/2 radian shift and a 3/2 π radian shift. Liebmann et al, “Alternating Phase Shifted Mask for Logic Gate Levels, Design and Mask Manufacturing”, SPIE vol. 3679 p. 27 (1999). It is also known in the art to use π:2/3 π:1/3 π:0 radian shifting masks.
[0013] It is therefore desirable to reduce phase conflict thereby substantially eliminating undesirable lines, and thus facilitating feature size reduction and improving product yield and reliability.
SUMMARY OF THE INVENTION
[0014] The invention relates to a phase-shifting mask having substantially equally spaced phases thereby substantially eliminating zeroth order and reducing first order diffraction frequencies. One embodiment of the invention relates to a three-phase-shifting mask having a pattern composed of substantially transparent regions and substantially opaque regions wherein the mask pattern phase-shifts incident radiation by 0, 2/3 π and 4/3 π radians. The invention further relates to a semiconductor device fabricated utilizing the phase-shifting mask. In such applications the invention facilitates reduction in component size and improved device reliability.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 depicts a prior art lithographic system useful in the practice of the invention.
[0016] FIGS. 2A-2D depict a prior art binary mask.
[0017] FIGS. 3A-3E depict a prior art π radian phase-shifting mask.
[0018] FIGS. 4A-4E depict a three-phase-shifting mask of the invention.
[0019] FIG. 5 depicts Fourier spectra of a three-phase-shift mask, a π radian phase-shift mask and a binary mask.
[0020] FIG. 6 depicts a mask pattern.
[0021] FIG. 7 depicts a semiconductor device.
DETAILED DESCRIPTION OF THE INVENTION
[0022] It will be appreciated that the following description is intended to refer to specific embodiments of the invention selected for illustration and is not intended to define or limit the invention, other than in the appended claims.
[0023] The invention comprises a phase-shifting mask having substantially equally spaced phases such that the zeroth order diffraction frequency is substantially canceled and the first order diffraction frequency is reduced as compared to nonphase-shifting masks or masks having unequally spaced phases. Any number of equally spaced phases may provide substantially similar pattern transferring results and are within the spirit and scope of the invention. However, the phase-shifting mask preferably has three equally spaced phases to simplify manufacturing. Phase-shifting masks having phase shifts of 1/3π radian multiples can be fabricated by layering readily available 1/3π radian phase-shifting components.
[0024] FIG. 4A depicts a cross-sectional view of a three-phase-shifting mask 400 . Three-phase-shifting mask 400 has a plurality of substantially transparent areas 402 , 404 and 406 and a plurality of substantially opaque areas 410 , 412 , 414 and 416 . Extending across apertures 402 and 404 are phase-shifters, 420 and 422 , respectively. Phase-shifter 420 produces a 2/3 π radian shift and phase-shifter 422 produces a 4/3 π radian shift. FIG. 4B shows the amplitudes of electric fields at mask level wherein the field areas from apertures 402 and 404 are represented by negative steps 430 and 432 , respectively, and the field area from aperture 406 is represented by positive step 434 . Since the electric fields are vectors by nature, FIG. 4B should be understood as a snapshot of the fields at a specific moment that will continually change with time. FIG. 4C represents electric fields 440 , 442 and 444 at a workpiece from apertures 402 , 404 and 406 , respectively. Unlike the binary mask, the electric fields at the overlap region are added destructively. Therefore, where images on the workpiece surface from apertures 402 , 404 and 406 meet, the intensity is substantially zero as shown in FIG. 4D at 450 and 452 .
[0025] This phenomenon is further depicted in FIG. 4E . FIG. 4E depicts electric field vectors corresponding to an electric field at workpiece level for mask 400 . It should be noted that the amplitudes of the electric fields are the projection of the vectors shown in the figure to the vertical axis. Vector 460 corresponds to an electric field produced by aperture 406 through which unshifted radiation is propagated. Vector 462 represents an electric field at workpiece level produced by radiation propagating through aperture 402 which is phase-shifted 2/3 π radians by phase-shifter 420 . Vector 464 defines an electric field at workpiece level of radiation propagating through aperture 404 and 4/3 π radian phase-shifter 422 . The amplitude of vectors 462 and 464 are substantially equal when vector 460 is at its maximum amplitude as shown in FIG. 4E . The vector array rotates clockwise with time at a frequency determined by the frequency of the incident radiation. As vector 460 rotates, its amplitude will decrease. As the amplitude of vector 460 decreases, the amplitude of vector 462 will become more negative and the amplitude of vector 464 will become less negative. However, the sum of the amplitudes of vectors 460 , 462 and 464 will remain generally equal to zero, thereby substantially eliminating light intensity at the location where the electric fields overlap. For masks having any number of substantially equally spaced phases, corresponding electric field vectors will generally sum to zero.
[0026] Advantageously, the frequency component of three-phase-shift mask 400 is lower than binary mask or π radian phase-shifting mask 300 . This makes it possible for radiation to pass through the limited numerical aperture of the projection lens, and therefore achieve higher resolution with a given system. This phenomenon will also be present for masks with other numbers of equally spaced phases.
[0027] FIG. 5 depicts Fourier spectra of a binary mask, a π radian phase-shifting mask and an equally spaced three-phase-shifting mask. The zeroth order diffraction frequency is substantially eliminated and the first order diffraction frequency is reduced with the three-phase-shifting mask as compared to the binary and π radian phase-shifting masks. Binary mask spectrum 510 indicates a first order diffraction frequency centered at C. π radian phase-shifting mask spectrum 520 has a first order diffraction frequency centered at B indicating a lower frequency. Advantageously, three-phase-shifting mask spectrum 530 shows a center of its first order diffraction frequency to be at A indicating an even lower frequency than that of the π radian phase-shifting mask. Lower diffraction frequency corresponds to improved resolution. Therefore, resolution with a three-phase-shifting mask will be better than that with a binary or π radian phase-shifting mask, thereby facilitating formation of smaller features. Other equally spaced phase-shifting masks should produce results similar to those obtained from the three-phase-shifting mask.
[0028] FIG. 6 depicts one example of a mask pattern in which a phase conflict is likely to occur with a π radian shift. FIG. 6 shows three opaque mask features 610 , 620 and 630 surrounded by transparent areas 640 , 650 , 660 , 670 and 680 . If a π phase-shifting mask is employed to shift radiation propagated through transparent areas 640 and 660 by it radians, and radiation propagated through areas 650 and 670 are left unshifted or at zero, the electric field interference produced by diffraction of radiation propagating through transparent areas 640 , 650 and 660 will be minimized. However, transparent area 680 has portions adjacent to transparent areas 640 , 650 and 660 so that a phase transition is unavoidable between either 680 and 650 or between 680 and 640 / 660 . Where the phase transition occurs, an undesirable dark line will usually be produced. This phenomenon is referred to as “phase conflict”.
[0029] Advantageously, substantially equally spaced phase-shifting masks reduce phase conflict. For example, for the mask pattern depicted in FIG. 6 , by introducing a third phase and having the phases equally spaced, features 650 , 660 and 680 can have different phases from one another, thereby substantially eliminating phase conflict. Furthermore, transparent area 640 can have the same phase as transparent area 660 without producing a phase conflict. Because interference of the electric fields from the three features is substantially eliminated, unwanted dark lines will generally be eliminated.
[0030] The preferred mask thickness will depend on its application and on the mask material. For example, in a photolithographic process used in the fabrication of semiconductor devices the mask thickness is preferably in the range of about 0.22 cm to about 0.64 cm. It will be understood by those skilled in the art that any mask thickness will be suitable that allows the transmission of radiation sufficient to transfer the mask pattern to the workpiece and which has the structural integrity necessary to withstand the process in which it is used.
[0031] The preferred mask material will also depend on the application for which the mask is used. For example, masks typically comprise glass or quartz when used in photolithographic processes in the manufacture of semiconductor devices. Any material sufficient to withstand the particular lithographic process for which it is used and through which sufficient radiation may be transmitted to transfer the mask pattern to the workpiece may be utilized. Additional examples of mask materials include, but are not limited to, silicon dioxide fluorides, alkaline metals fluorides and alkaline earth fluorides. Calcium fluorides and magnesium fluorides are particularly well suited as mask materials.
[0032] In a lithographic process radiation is propagated through the mask and focused with a lens onto a workpiece coated with resist. If a negative resist is used, exposed areas will remain intact. If a positive resist is employed, exposed areas will be removed. By this process, the pattern of the mask will be transferred to the workpiece. Areas in which resist has been removed may then undergo additional processes, for example etching and plating, to form features on the workpiece in a desired pattern.
[0033] The invention further includes a semiconductor device which, when formed using a substantially equally spaced phase-shifting mask, should have better feature definition than that which is formed using a prior art mask, primarily due to improved resolution. FIG. 7 depicts a schematic of a semiconductor device 200 that may be formed using a substantially equally spaced phase-shifting mask. Those skilled in the art will understand that it shows a simplified drawing of semiconductor device 200 for illustrative purposes only. An actual device may have layers of varying thicknesses and may contain other components. Semiconductor substrate 202 is covered by a first dielectric layer 204 . Above first dielectric layer 204 is a first metal layer 206 . Vias or interconnects 208 , 210 , 212 and 214 penetrate layer 204 and conductively connect first metal layer 206 to semiconductor substrate 202 . First metal layer 206 is covered by second dielectric layer 216 which contains vias 218 , 220 and 222 to connect first metal layer 206 to a second metal layer 224 . This layering sequence may be repeated as necessary as shown in part by layers 226 and 228 , and interconnects 232 , 234 and 236 . A top passivation layer 230 may be applied to protect device 200 from adverse electrical, chemical or other conditions, and to provide electrical stability.
[0034] Semiconductor substrate 202 may comprise silicon, for example. Common dielectrics include, but are not limited to, silicon oxides, such as boron phosphorous doped silicate glass (BPSG), those originating from tetraethylorthosilicate (TEOS) and silicon dioxide (SiO 2 ). Common metals include, for example, aluminum, copper and tungsten. In addition, to improve adherence between metal and dielectric layers, thin layers may be introduced between them. Titanium is commonly used for this purpose. Electronic circuitry is defined in the layers by a lithographic technique.
[0035] In the lithographic process used to form the circuitry in device 200 a resist is deposited over a dielectric layer. The resist is exposed by transmitting radiation through the substantially equally spaced phase-shifting mask onto the dielectric layer surface, thereby defining desired circuitry and substantially eliminating phase conflict. The form of radiation used is dependent on the type of resist and other fabrication parameters. Any form of radiation that may expose the resist without adverse effects to the workpiece may be used. Common examples include, ultraviolet radiation, electron beam radiation and x-rays. If a positive resist is used, the exposed areas will be removed revealing the dielectric layer below. The dielectric layer may then be removed, for example by etching. Any technique that will remove the exposed dielectric layer while leaving the resist covered portions intact may also be used. Negative resists may be used wherein the exposed resist areas are left intact after exposure and the nonexposed areas are removed. For negative resist processes a mask is used that defines the spaces between circuit components rather than the circuitry itself Lithographic processes using the substantially equally spaced phase shifting mask may also be employed to form other device features, for example interconnects in the dielectric layers.
[0036] The phase-shifting mask described herein is not limited in use to semiconductor device fabrication and may, within the spirit and scope of the invention, be used for any lithographic process in which it would facilitate transfer of a pattern to a workpiece. | Disclosed is a phase-shifting mask having a pattern comprising a plurality of substantially transparent regions and a plurality of substantially opaque regions wherein the mask pattern phase-shifts at least a portion of incident radiation and wherein the phases are substantially equally spaced, thereby increasing resolution of a given lithographic system. Further disclosed is a semiconductor device fabricated utilizing the phase-shifting mask. | 8 |
FIELD OF THE INVENTION
[0001] The present invention generally relates to design verification, and more specifically to the use of model checking to verify that the design of a device holds certain correctness properties. Even more specifically, the preferred embodiment of the invention relates to a model checking technique that is very well suited for use with embedded processing devices.
BACKGROUND OF THE INVENTION
[0002] Embedded devices are becoming pervasive and playing increasing role in our lives. We depend on cell phones and ATMs. Embedded systems are also used in mission critical applications such as aircraft navigation and control systems, heart pacemaker devices, and military systems. Correct functioning of these devices is crucial. To establish correctness, subjecting them to various possible inputs tests these devices. However, exhaustive testing is not only costly and time consuming but also impossible for non-trivial devices. A complementary approach is to apply static model checking techniques to verify that the design of a device holds certain correctness properties.
[0003] Model Checking is used to establish correctness of a given program. Model Checking techniques typically convert program constructs in a program into equivalent mathematical logic or constructs. These mathematical constructs collectively define the underlying mathematical model of the program. In essence, the mathematical model defines the various states a given program can be in, and the conditions (inputs) required for various state transitions.
[0004] The correctness is established by exploring the state space of the mathematical model and verifying that none of the execution paths will lead to a program state that violates one or more constraints from a pre-defined constraint set.
[0005] Evidently, the correctness proof of a program with any Model Checking technique is based on the assumption that the translation of a program to a mathematical model is flawless. If the translation is incorrect, then the correctness proof is unreliable. That is why it is very important that the translation is correct without a doubt.
[0006] Model Checking techniques are very useful in embedded devices that have real-time software. In such devices, all possible inputs cannot be tested, but the correctness of software is vital because these devices have critical applications such as health and military applications. Real time systems are concurrent reactive systems represented by communicating state machines. The communication channels between state machines are defined using Priority Message Queue programming construct.
[0007] The embedded devices fall into the category of concurrent reactive systems and their design can be expressed through Unified Modeling Language (UML) state machines communicating with each other through signal and message passing. For static model checking, the UML state machines have to be converted into modeling languages suitable for model checking. A challenging aspect of the conversion is efficient modeling of communication channels between the state machines. This aspect is difficult because the scalability of model checking techniques is limited due to the problem of state space explosion. A channel is essentially a non-deterministic priority message queue. The model should be expressive enough to capture the behavior of a non-deterministic priority queue, yet the possible permutations should occupy small state space.
[0008] Existing techniques to model priority queues typically have a single queue, and allow each cell to swap its content with the cell before it depending upon the different priorities of the cells. Though this model is concise (i.e. less bits to model), the behavior is complex (i.e. model of each bit is complex). For symbolic model checking, the behavior needs to be encoded into a representation suitable for model checking (such as SAT (Satisfiability problem) or BDD (Binary Decision Diagram)). Complex behavior results in bigger encoding. Therefore, the complexity of the behavior is an important issue for performing model checking.
SUMMARY OF THE INVENTION
[0009] An object of the present invention is to improve model-checking techniques.
[0010] Another object of this invention is to model non-deterministic queues for efficient model checking.
[0011] A further object of the invention is to facilitate expressing complex behavior of priority queues in a simple and intuitive manner.
[0012] These and other objectives are attained with a method and system for modeling non-deterministic queues for efficient model checking. In this method and system, a multitude of messages are held in a plurality of queues. These messages have n priorities, and the method comprises the step of providing (n+1) queues, including a first queue, and n priority queues. The method comprises the further steps of passing said messages from a source to the first queue; passing each of said messages from the first queue to one of said n priority queues based on the priority of the message; and passing each of said messages from the n queues to a destination based on the priority of the message. One or more non-deterministic waits are introduced into one or more of the passing steps to simplify passing the messages into or out of the n priority queues in a preferred or predetermined manner.
[0013] For example, a non-deterministic wait may be introduced between the first queue and said n priority queues to control the timing of the passing of messages into the first queue. In addition, or as an alternative, a non-deterministic wait may be introduced between the n priority queues and the destination to control the timing of the passing of messages from the n priority queues to the destination.
[0014] In the preferred embodiment of the invention, non-deterministic behavior is simulated using a non-deterministic wait at various stages. Since it has a larger number of queues in comparison to the single queue model, this preferred technique takes more space (i.e. more bits to model). But the behavior is very simple (i.e. the model of each bit is simple). This technique facilitates expressing complex behavior of a priority queue in a simple and intuitive manner, which is closer to the system being modeled, and hence leads to a compact representation to allow efficient model checking.
[0015] Existing methods use a single queue, whose logic is very complex, and hence has significant potential for errors, which jeopardizes the correctness of model checking and renders it useless. The method described herein uses (n+1) queues, where n is the number of priorities. For example, if there are three types of priorities—such as low, medium and high—that a message (from a state machine to another state machine) can have, then this method will use four queues instead of one queue, as done by existing methods. This greatly simplifies the translation and eliminates the risk of mistake while translating communication channels to equivalent mathematical models. An important advantage of this invention is in the great amount of simplification (and hence correctness) achieved in the logic and translation by using (n+1) queues. The invention is particularly useful in the critical role of accurate translation of communication channels to respective mathematical models in Model Checking real time software correctly.
[0016] Further benefits and advantages of this invention will become apparent from a consideration of the following detailed description, given with reference to the accompanying drawings, which specify and show preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] The foregoing will be apparent from the following more particular description of example embodiments of the invention, as illustrated in the accompanying drawings in which like reference characters refer to the same parts throughout the different views. The drawings are not necessarily to scale, emphasis instead being placed upon illustrating embodiments of the present invention.
[0018] FIG. 1 is a schematic pictorial illustration showing a system for modeling priority queues in accordance with a preferred embodiment of the present invention.
[0019] FIG. 2 illustrates an example model for priority queues with three priorities.
[0020] FIG. 3 shows a first example of the present invention.
[0021] FIG. 4 shows a second example of the preferred embodiment of this invention.
[0022] FIG. 5 illustrates a third example of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0023] A description of example embodiments of the invention follows.
[0024] FIG. 1 is a schematic pictorial illustration of a system 10 for model checking, in accordance with a preferred embodiment of the present invention. System 10 typically comprises a model processor 12 , typically a general-purpose computer workstation running suitable model checking software. The system is operated by a user 14 , which may be a design or verification engineer. The model checking software may be downloaded to processor 12 in electronic form, over a network, for example, or it may be supplied on tangible media, such as CD-ROM or non-volatile memory. Processor 12 receives a hardware implementation model 16 of a target system or device 20 in development, which may refer to the entire system or device or to a sub-unit, such as a circuit or functional block. User 14 prepares a path specification 22 , comprising properties for use in model checking of model 16 , and selects initial states of the model. System 10 analyzes the model to find full or partial traces between the initial states and target states, which are inferred by processor 12 based on the path specification. The methods described below in detail are used in this model analysis.
[0025] As indicated above, when modeling embedded devices, and other concurrent reactive systems, their designs can be expressed through UML state machines communicating with each other through signal and message passing. For static model checking, the UML state machines have to be converted into modeling languages suitable for model checking. An important aspect of the conversion is efficient modeling of communication channels between the state machines because the scalability of model checking techniques is limited due to the problem of state space explosion. A channel is essentially a non-deterministic priority message queue. The model should be expressive enough to capture the behavior of a non-deterministic priority queue yet the possible permutations should occupy small state space. The present invention provides a technique to model non-deterministic queues for efficient model checking.
[0026] Generally, a communication channel provides the following guarantee: given two messages m 1 and m 2 , m 1 is guaranteed to be processed before m 2 , if m 1 has arrived before m 2 and m 2 's priority is the same as or lower than the priority of m 1 . Otherwise, the processing order is non-deterministic.
[0027] FIG. 2 illustrates an efficient model 30 for this behavior in accordance with one embodiment of this invention. The model uses (n+1) queues for n priorities. The example shown in FIG. 2 includes a first queue 32 and three priority queues 34 , 36 and 40 . Queue 34 is a high priority queue, queue 36 is a medium priority queue, and queue 40 is a low priority queue. FIG. 2 also shows a message source 42 and a message destination 44 .
[0028] The first queue 32 gets messages, which are then passed to the correct priority queue. The first message available in the non-empty priority queue with the highest priority gets processed first. The nondeterministic behavior is achieved by introducing nondeterministic waits between first queue 32 and the queues 34 , 36 , 40 for the different priorities, and between the queues 34 , 36 , 40 for priorities and destination process 44 . The non-deterministic wait between the first queue 32 and the queues 34 , 36 , 40 for the priorities allows the destination process 44 to look at lower priority messages before a high priority message enters the high priority queue 34 . The non-deterministic wait between the queues 34 , 36 , 40 for priorities and the destination process 44 allows the destination process to look at higher priority messages before early low priority message.
[0029] These features of the invention are illustrated in FIGS. 3 and 4 . More specifically, FIG. 3 illustrates the result of the use of the non-deterministic wait between the first queue 32 and the queues 34 , 36 , 40 for the priorities, and FIG. 4 shows the result of the use of the non-deterministic wait between the queues 34 , 36 , 40 for the priorities and the destination process 44 .
[0030] FIG. 3 illustrates seven states, 51 - 57 . At state 51 (State 1 ), messages “m” and “m” are in the medium priority queue 36 , and messages “h”, “l” and “l” are in the first queue 32 . At state 52 (State 2 ), the first “m” message is sent to the destination 44 , and the first “l” message is sent to low priority queue 40 . At state 53 (State 3 ), the second “m” message is sent to the destination 44 , and the second “l” message is sent to the low priority queue 40 .
[0031] At states 54 and 55 (States 4 and 5 ), a non-deterministic wait, represented at 58 , occurs between the first queue 32 and the priority queues 34 , 36 , 40 . This wait allows the two low priority messages to be sent to the destination 44 before the high priority message in queue 32 is passed to the high priority queue 34 . At states 56 and 57 (States 6 and 7 ), this high priority message is sent to queue 34 and then to the destination 44 . Thus, with the procedure of FIG. 3 , as indicated at state 57 , the order in which the messages are processed is “m”, “m”, “l”, “l”, “h”.
[0032] FIG. 4 also shows seven states 61 - 67 . Similar to the process depicted in FIG. 3 , at state 61 , messages “m” and “m” are in the medium priority queue 36 , and messages “h”, “l” and “l” are in the first queue 32 . At state 62 , the first “m” message is sent to the destination 44 , and the first “l” message is sent to low priority queue 40 . At state 63 , the second “m” message is sent to the destination 44 , and the second “l” message is sent to the low priority queue 40 .
[0033] At state 64 , a non-deterministic wait, represented at 68 , is introduced between the priority queues 34 , 36 , 40 and the destination 44 . This wait allows the high priority message h to be passed from queue 32 to high priority queue 34 before the low priority messages are passed from the low priority queue 40 to the destination 44 . Then, at state 65 , the high priority message h is passed from queue 34 to the destination 44 ; and at states 66 and 67 , the low priority messages are passed from the low priority queue 40 to the destination 44 . Thus, with this procedure of FIG. 4 , as indicated in state 67 , the order in which the messages are processed is “m”, “m”, “h”, “l”, “l”.
[0034] The preferred mechanism of the present invention allows also that the high priority message may be handled between two low priority messages that came earlier. For example, if there is no wait, as would be the case in standard priority queue model, the order in which messages are processed is “m”, “m”, “l”, “h”, “l”.
[0035] This operation is illustrated in FIG. 5 . At state 71 , messages “m” and “m” are in medium priority queue 36 , and messages “l”, “l” and h are in first queue 32 . At states 72 and 73 , both “m”s are passed from queue 36 to destination 44 , and both “l”s are passed from queue 32 to low priority queue 40 . At state 74 , the “h” message is passed from the high priority queue 34 to the destination 44 , and at state 75 , the “l” message is passed from queue 40 to destination 44 . Thus, with this procedure, the messages are processed in the order “m”, “m”, “l”, “h”, “l”.
[0036] The preferred embodiment of the invention provides a number of significant advantages. One important advantage is the great amount of simplification (and hence correctness) achieved in the logic and translation by using (n+1) queues. A particular advantage of this invention is in the critical role of accurate translation of communication channels to mathematical model in Model Checking real time software correctly.
[0037] Included herewith is an Appendix that provides an encoding for a message queue with three priorities and where the size of the FIFO channel is four.
[0038] As will be readily apparent to those skilled in the art, the present invention can be realized in hardware, software, or a combination of hardware and software. Any kind of computer/server system(s)—or other apparatus adapted for carrying out the methods described herein—is suited. A typical combination of hardware and software could be a general-purpose computer system with a computer program that, when loaded and executed, carries out the respective methods described herein. Alternatively, a specific use computer, containing specialized hardware for carrying out one or more of the functional tasks of the invention, could be utilized.
[0039] The present invention, or aspects of the invention, can also be embodied in a computer program product, which comprises all the respective features enabling the implementation of the methods described herein, and which—when loaded in a computer system—is able to carry out these methods. Computer program, software program, program, or software, in the present context mean any expression, in any language, code or notation, of a set of instructions intended to cause a system having an information processing capability to perform a particular function either directly or after either or both of the following: (a) conversion to another language, code or notation; and/or (b) reproduction in a different material form.
[0040] While it is apparent that the invention herein disclosed is well calculated to fulfill the objects stated above, it will be appreciated that numerous modifications and embodiments may be devised by those skilled in the art, and it is intended that the appended claims cover all such modifications and embodiments as fall within the true spirit and scope of the present invention.
[0000]
APPENDIX
#define FIFO_SIZE 4
#define message_type {0,1,2,3}
#define EMPTY 0
#define LOW 1
#define MED 2
#define HIGH 3
vmode default {
module queue (push_in, pop_out , data_in) (data_out, top) {
var vector(0..((FIFO_SIZE)−1)): {EMPTY, LOW, MED, HIGH};
--%for i in 1 .. ((FIFO_SIZE)−2) do
%for i in 1 .. 2 do
assign init(vector(i)) := EMPTY;
assign next(vector(i)) := case
pop_out & push_in: if (vector(i) != EMPTY & vector(%{i+1}) = EMPTY) then
data_in
else vector(%{i+1}) endif;
pop_out : vector(%{i+1});
push_in : if (vector(i) = EMPTY & vector(%{i−1}) != EMPTY) then data_in
else
vector(i) endif;
else: vector(i);
esac;
%end
assign init(vector(0)) := EMPTY;
assign next(vector(0)) := case
push_in & pop_out:
if (vector(1) != EMPTY) then vector(1) else data_in endif;
pop_out : vector(1);
push_in : if (vector(0) = EMPTY) then data_in else vector(0) endif;
else:
vector(0);
esac;
assign init(vector((FIFO_SIZE)−1)) := EMPTY;
assign next(vector((FIFO_SIZE)−1)) := case
pop_out & push_in: if (vector((FIFO_SIZE)−1) != EMPTY) then data_in else EMPTY
endif;
pop_out: EMPTY;
push_in: if (vector((FIFO_SIZE)−2) != EMPTY & vector((FIFO_SIZE)−1) = EMPTY)
then data_in else EMPTY endif;
else:
vector((FIFO_SIZE)−1);
esac;
define data_out := if (pop_out) then top else EMPTY endif;
define top := vector(0);
}
module priority_queue (push_in, in_pop_out , data_in) (data_out, top) {
var pop_out:boolean;
assign pop_out := in_pop_out;
instance high_queue: queue(push_in_high, pop_out_high, data_in_high)(data_out_high,
top_high);
instance low_queue: queue(push_in_low, pop_out_low, data_in_low)(data_out_low,
top_low);
instance med_queue: queue(push_in_med, pop_out_med, data_in_med)(data_out_med,
top_med);
instance trans_queue: queue(push_in_trans, pop_out_trans,
data_in_trans)(data_out_trans, top_trans);
var trans_barrier: boolean;
assign trans_barrier:= {true, false};
define push_in_high:= if (trans_barrier) then false else (if (data_out_trans = HIGH)
then true else false endif) endif;
define push_in_med := if (trans_barrier) then false else (if (data_out_trans = MED)
then true else false endif) endif;
define push_in_low:= if (trans_barrier) then false else (if (data_out_trans = LOW)
then true else false endif) endif;
define pop_out_trans := !trans_barrier;
define pop_out_high := if (!pop_out) then false else if (top_high != EMPTY) then true
else false endif endif;
define pop_out_med := if (!pop_out) then false else if (top_high = EMPTY & top_med !=
EMPTY) then true else false endif endif;
define pop_out_low := if (!pop_out) then false else if (top_high = EMPTY & top_med =
EMPTY & top_low != EMPTY) then true else false endif endif;
define data_in_trans := data_in;
define push_in_trans := push_in;
define data_in_high := top_trans;
define data_in_med := top_trans;
define data_in_low := top_trans;
define data_out := if (pop_out) then top else EMPTY endif;
define top := case
top_high != EMPTY: top_high;
top_med != EMPTY : top_med;
top_low != EMPTY : top_low;
else: EMPTY;
esac;
}
instance check_queue: priority_queue(push_in, pop_out, data_in)(data_out, top);
define push_in := {true, false};
define data_in := {EMPTY, LOW, MED, HIGH};
define pop_out := {true, false};
}
--instance simple_queue: queue(push_in_s, pop_out_s, data_in_s)(data_out_s, top_s);
--define push_in_s := {true, false};
--define data_in_s := {EMPTY, LOW, MED, HIGH};
--define pop_out := {true, false};
vunit abc {
define h_in := push_in = HIGH;
define l_in := push_in = LOW;
define h_out := data_out = HIGH;
define l_out := data_out = LOW;
define nothing := !h_out & !l_out;
}
vunit try {
define h_in := data_in = HIGH & push_in;
define l_in := data_in = LOW & push_in;
define m_in := data_in = MEDIUM & push_in;
define no_in := !push_in;
define h_out := data_out = HIGH;
define l_out := data_out = LOW;
define nothing := !h_out & !l_out;
-- assert{{ (!h_in & !l_in)[*]; h_in }}(false);
assert{{ (!h_in & !l_in) [*]; h_in; (!h_in & !l_in) [*]; h_in; (!h_in & !l_in)
[*]; l_in; (!h_in & !l_in) [*]} &&
{ (nothing)[*]; h_out ; (nothing)[*]; l_out}}(false);
} | A method and system are disclosed for modeling non-deterministic queues for efficient model checking. In this method and system, a multitude of messages are held in a plurality of queues, and these messages having n priorities. The method comprises the steps of providing (n+1) queues, including a first queue, and n priority queues; passing said messages from a source to the first queue; passing each of said messages from the first queue to one of said n priority queues based on the priority of the message; and passing each of said messages from the n priority queues to a destination based on the priority of the message. One or more non-deterministic waits are introduced into one or more of the passing steps to simplify passing the messages into or out of the n priority queues. | 7 |
BACKGROUND OF THE INVENTION
[0001] The present invention relates to optical equipment configured to contract in an optical axis direction during a non-photographing state to achieve enhanced portability, and particularly to optical equipment suitably applied for a camera or a lens barrel.
[0002] As one example of a plurality of types of optical equipment, such as an image capturing apparatus (e.g., a digital camera) for capturing a still image or a moving image or a lens barrel used for such an image capturing apparatus, a lens barrel configured to contract in an optical axis direction during a non-photographing state to enhance portability has been proposed. Japanese Patent Provisional Publication No. 2011-154113A (hereafter, referred to as patent document 1) describes a lens barrel configured such that a variator lens holding frame and a compensator lens holding frame are respectively pressed by coil springs in an optical axis direction, and these lens holding frames are caused to contact cam surfaces of a variable power cam frame through use of such pressing forces. During a photographing operation, both of the variator lens and compensator lens holding frames are moved by the variable power cam frame in the optical axis direction to change power. In a non-photographing state, both of the variator lens and compensator lens holding frames are forcibly moved in the optical axis direction toward a relay lanes holding frame against pressing forces of the coil springs acting respectively on the variator lens and compensator lens holding frames so that the lens barrel contracts in the optical axis direction.
SUMMARY OF THE INVENTION
[0003] According to the technique described in the patent document 1, a relay lens is configured as a variable power lens system not moving in the optical axis direction during the photographing operation, and a variator lens is configured as a variable power lens system moving in the optical axis direction without regard to the relay lens when the power is changed. Therefore, if the technique described in the patent document 1 is applied to a variable power lens system in which a relay lens is moved during changing of power, in particular a variable power lens system in which changing of power is performed while maintaining an interval between a variator lens and a relay lens in the optical axis direction, it is difficult to maintain the interval between the variator lens and the relay lens. That is, since the technique described in the patent document 1 does not provide a configuration for maintaining the interval between the variator lens and the relay lens in the optical axis direction, there may be a case where the interval between the variator lens and the relay lens in the optical axis direction varies during changing of power. In such a case, it becomes difficult to maintain high variable power characteristics.
[0004] The present invention is advantageous in that it provides optical equipment capable of enhancing optical performance while keeping an interval in an optical axis direction between optical elements (e.g., a variator lens and a relay lens) arranged along an optical axis constant.
[0005] According to an aspect of the invention, there is provided optical equipment, comprising: a first holding unit that holds a first optical element; and a second holding unit that holds a second optical element. In this configuration, the first holding unit and the second holding unit are provided to be movable in an optical axis direction so as to allow the optical equipment to reduce a length in the optical axis direction. The first holding unit is configured to be driven by a driving unit in the optical axis direction. The second holding unit is coupled to the first holding unit in regard to the optical axis direction such that the second holding unit is allowed to move integrally with the first holding unit and is allowed to move relatively to the first holding unit.
[0006] With this configuration, it becomes possible to enhance optical performance (e.g., variable power characteristics) of the optical equipment while keeping an interval in an optical axis direction between the first optical element and the second optical element (e.g., a compensator lens and a relay lens).
[0007] In at least one aspect, at least one of the first holding unit and the second holding unit may have a position restriction mechanism formed to restrict relative movement of the first holding unit and the second holding unit in a direction of moving away from each other in regard to the optical axis direction.
[0008] In at least one aspect, the first holding unit may have a plurality of guide pieces arranged along a circumferential direction of the first holding unit. Each of the plurality of guide pieces may be formed to project in the optical axis direction. The second holding unit may have a plurality of position restriction pieces arranged along a circumferential direction of the second holding unit, each of the plurality of position restriction pieces being formed to project in the optical axis direction. The second holding unit may be held by the plurality of guide pieces of the first holding unit at the plurality of position restriction pieces.
[0009] In at least one aspect, each of the plurality of guide pieces may have a guide projection formed at a tip of the each of the plurality of guide pieces. Each of the plurality of position restriction pieces may have a position restriction part formed at a tip of the each of the plurality of position restriction pieces to contact the guide projection of a corresponding one of the plurality of guide pieces in the optical axis direction. In this case, the guide projection and the position restriction part constitute the position restriction mechanism.
[0010] In at least one aspect, the second holding unit may be held on the first holding unit in a state where an outer circumferential surface of each of the plurality of position restriction pieces contacts, in a radial direction, an inner diameter end of the guide projection of a corresponding one of the plurality of guide pieces when the guide projection contacts the position restriction part in the optical axis direction.
[0011] In at least one aspect, in a state where the guide projection is separated from the position restriction part in the optical axis direction, an outer circumferential surface of each of the plurality of position restriction pieces may be separated, in a radial direction, from an inner diameter end of the guide projection of a corresponding one of the plurality of guide pieces.
[0012] In at least one aspect, the optical equipment may further comprise a spring member disposed to cause the second holding unit to be separated from the first holding unit in the optical axis direction. In this case, the guide projection and the position restriction part contact with each other in the optical axis direction by a pressing force of the spring member.
[0013] In at least one aspect, the first holding unit may have a pressing member disposed to elastically contact the second holding unit and to press the second holding unit toward a direction perpendicular to the optical axis direction.
[0014] In at least one aspect, in an extended state of the optical equipment, the first holding unit and the second holding unit may be coupled together in regard to the optical axis direction such that the guide projection and the position restriction part contacts with each other. When the optical equipment is contracted, the first optical unit and the second optical unit may be moved relatively to one another such that the guide projection and the position restriction part are separated each other in the optical axis direction.
[0015] In at least one aspect, when the optical equipment is contracted, the first holding unit and the second holding unit may be moved in a direction of reducing the length of the optical equipment, and the second holding unit contacts a fixed part of the optical equipment.
[0016] In at least one aspect, the optical equipment may further comprise a third holding unit that holds a third optical element and is disposed on an image surface side with respect to the second holding unit. In this case, when the optical equipment is contracted, the second holding unit may contact the third holding unit.
[0017] In at least one aspect, the optical equipment may further comprise a position adjustment mechanism configured to adjust a position of at least one of the first optical element and the second optical element in the optical axis direction and in a direction perpendicular to the optical axis direction with respect to a corresponding one of the first holding unit and the second holding unit.
[0018] According to another aspect of the invention, there is provided optical equipment configured as a lens barrel for a camera, comprising: a fixed frame of the lens barrel; a guide frame supported by the fixed frame; a first cam tube supported by the fixed frame to be rotatable about an optical axis; a moving guide frame movable in an optical axis direction along the guide frame in accordance with rotation of the first cam tube; a second cam tube that is moved integrally with the moving guide frame in the optical axis direction and is rotated together with the first cam tube; a first holding frame that is moved in the optical axis direction by the first cam tube; a second holding frame that is coupled to the first holding frame in regard to the optical axis direction such that the second holding frame is able to move relatively to the first holding frame in the optical axis direction. In this configuration, each of the first holding frame and the second holding frame supports at least one lens.
[0019] With this configuration, it becomes possible to enhance optical performance (e.g., variable power characteristics) of the optical equipment while keeping an interval in an optical axis direction between the lenses (e.g., a compensator lens and a relay lens).
[0020] In at least one aspect, the optical equipment may further comprise a position adjustment mechanism configured to adjust a position of the at least one lens of at least one of the first holding frame and the second holding frame in the optical axis direction and in a direction perpendicular to the optical axis direction with respect to a corresponding one of the first holding frame and the second holding frame.
[0021] According to another aspect of the invention, there is provided optical equipment configured as a lens barrel for a camera, comprising: first, second, third and fourth lenses; a lens driving unit configured to move the first, second and third lenses in an optical axis direction; a first holding frame that holds the second lens; and a second holding frame that holds the fourth lens. In this configuration, the first holding frame and the second holding frame are coupled with each other in regard to the optical axis direction such that the first holding frame and the second holding frame are able to move relatively to each other in the optical axis direction. When the first, second and third lenses are moved by the lens driving unit in the optical axis direction, the second holding frame is moved in the optical axis direction via the first holding frame.
[0022] With this configuration, it becomes possible to enhance optical performance (e.g., variable power characteristics) of the optical equipment while keeping an interval in an optical axis direction between the second lens and the fourth lense (e.g., a compensator lens and a relay lens).
[0023] In at least one aspect, the first, second, third and fourth lenses may be a focusing lens, a variator lens, a compensator lens and a relay lens, respectively.
[0024] In at least one aspect, the optical equipment may further comprise a position adjustment mechanism configured to adjust a position of at least one of the second lens and the fourth lens in the optical axis direction and in a direction perpendicular to the optical axis direction with respect to a corresponding one of the first holding frame and the second holding frame.
[0025] In at least one aspect, each of the first to fourth lenses may be formed as a lens group.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS
[0026] FIGS. 1A and 1B are perspective views illustrating an outer appearance of a lens barrel according to an embodiment.
[0027] FIG. 2 is a cross section of the lens barrel along an optical axis in a capturing state (a wide state).
[0028] FIG. 3 is an exploded perspective view of principal components of the lens barrel.
[0029] FIG. 4 is a cross section illustrating frames of the lens barrel excepting lens systems.
[0030] Each of FIGS. 5A and 5B schematically illustrates relationship between lens systems and cam tubes.
[0031] FIG. 6A is a cross section along the optical axis, illustrating a state where a first holding frame and a second holding frame are combined, and FIG. 6B is an enlarged view of a circled portion B in FIG. 6A .
[0032] FIG. 7A is a side view illustrating a state where the first holding frame and the second holding frame are combined, viewed from an image surface side, FIG. 7B is a cross section cut along a line B 1 -B 1 in FIG. 7A , and FIG. 7C is an enlarged view of a portion C in FIG. 7B .
[0033] Each of FIGS. 8A, 8B and 8C is a cross section along the optical axis, illustrating extending and contracting motion of the lens systems of the lens barrel.
[0034] FIG. 9 is a cross section along the optical axis of the lens barrel in the capturing state (a tele-state).
[0035] FIG. 10 is a cross section along the optical axis of the lens barrel in a non-capturing state (a contracted state).
[0036] Each of FIGS. 11A and 11B is a cross section along the optical axis of the lens barrel, illustrating extending and contracting motion of the first holding frame and the second holding frame.
[0037] Each of FIGS. 12A and 12B schematically illustrates relationship between a lens system and a cam tube in a lens barrel according to a variation of the embodiment.
[0038] FIG. 13A is a perspective view of a lens frame having a lens position adjustment mechanism, and FIG. 13B is a rear view of the lens frame in FIG. 13A .
[0039] FIG. 14A is an exploded perspective view of the lens frame having the lens position adjustment mechanism, and FIG. 14B is a perspective view of an adjustment ring in FIG. 14A .
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0040] Hereinafter, embodiments according to the invention are described with reference to the accompanying drawings. FIGS. 1A and 1B illustrate a lens barrel LL to which optical equipment according to the present invention is applied. Specifically, as an embodiment of the invention, each of FIGS. 1A and 1B illustrates a perspective view of an outer appearance of the lens barrel LL used as a zoom lens detachably attachable to a camera body of a digital camera (not shown). The lens barrel LL is configured to include necessary lens systems which are described in detail later. As shown in FIG. 1A , during a photographing operation, a movable frame 2 is extended to project toward a subject side (hereafter, referred to as an object side) in an optical axis direction relative to a fixed frame 1 having a cylindrical shape. As shown in FIG. 1B , in a non-photographing state, the movable frame 2 is retracted to a subject image side (hereafter, referred to as an image surface side) on which an object image is formed by the lens barrel LL so that the movable frame 2 is substantially accommodated in the fixed frame 1 and thereby the lens barrel LL becomes a contacted state. A lock button 1 b being a push-button is provided on a part of an outer circumference of the fixed frame 1 . The lens barrel LL is configured such that, the lens barrel LL maintains the contracted state when the lock button 1 b is not operated, and can be extended from the contracted state when the lock button 1 b is operated.
[0041] The lens barrel LL is provided with a variable power ring (a zoom ring) 3 to be operated to rotate about an optical axis along a circumferential surface of the lens barrel LL. By operating the variable power ring 3 to rotate in a rotational direction, as shown in FIG. 1A , the movable frame 2 is moved to project relative to the fixed frame 1 from the state where the movable frame 2 is accommodated in the fixed frame 1 , and concurrently lens systems provided the lens barrel LL are moved to achieve a focal length corresponding to a rotated position of the variable power ring 3 . By operating the variable power ring 3 to rotate in an opposite direction to an end position, as shown in 1 B, the lens barrel LL is brought to the contracted state where the movable frame 2 is substantially accommodated in the fixed frame 1 .
[0042] FIG. 2 is a vertical cross section of the lens barrel LL cut along the optical axis, and illustrates the photographing state where the lens barrel LL is extended. In FIG. 2 , hatching are added to principal components. The lens barrel LL includes first to fourth lenses L 1 to L 4 . Although each of the first to fourth lenses is formed to be a lens group having a plurality of lenses, each of these lens groups is simply referred to as a lens (i.e., first to forth lenses L 1 to L 4 ) for the sake of simplicity. In these lens systems, the first lens L 1 is formed as a focusing lens, the second lens L 2 is formed as a variator lens, the third lens L 3 is formed as a compensator lens, and the fourth lens L 4 is formed as a relay lens.
[0043] As shown in FIG. 2 , in the photographing operation, the lens barrel LL is brought to an extended state where the first, second, third and fourth lenses L 1 to L 4 are moved to the object side. When the first to fourth lenses L 1 to L 4 are moved in the optical axis direction to change power through an operation to the variable power ring 3 during the photographing operation, the second lens L 2 and the fourth lens IA are integrally moved while keeping an interval in the optical axis direction between the second lens L 2 and the fourth lens L 4 (hereafter, frequently referred to as an “optic axial interval”) constant. With this configuration, it becomes possible to enhance the variable power characteristics (e.g., achieving stable power change operation) by keeping the optic axial interval of the second lens L 2 and the fourth lens IA constant.
[0044] Hereafter, details of the lens barrel LL are explained. FIG. 3 is an exploded perspective view of the lens barrel LL, and FIG. 4 is a cross section illustrating an assembled state of the fixed frame 1 , a guide frame 4 , a second cam tube 5 , a moving guide frame 6 and a first cam tube 7 . Referring to FIGS. 2 to 4 , components of the lens barrel LL excepting the lens systems include the fixed frame 1 , the guide frame 4 fixedly supported by the fixed frame 1 , the second cam tube 5 rotatably provided about an axis with respect to the fixed frame 1 and the guide frame 4 , the moving guide frame 6 movable in the optical axis direction with respect to the guide frame 4 , and the first cam tube 7 rotatably provided about the axis with respect to the moving guide frame 6 . The moving guide frame 6 and the firs cam tube 7 form the second movable frame 2 .
[0045] A bayonet ring 1 a is attached to the image surface side of the fixed frame 1 having a cylindrical shape so as to be attachable to a lens mount of a camera body (not shown). In the inside of the fixed frame 1 , the second cam tube 5 is inserted to be along an inner circumferential surface of the fixed frame 1 , and the guide frame 4 is inserted on the further inner diameter side.
[0046] The second cam tube 5 is supported, to be rotatable about the optical axis, along the inner circumferential surface of the fixed frame 1 . In this embodiment, a part of the second cam tube 5 on the object side in the optical axis direction is exposed, and the exposed part of the second cam tube 5 is formed as the variable power ring 3 . Therefore, through a rotational operation to the variable power ring 3 , the second cam tube 5 is also rotated about the optical axis. Furthermore, on the inner circumferential surface of the second cam tube 5 , a helicoid groove 5 a and a guide groove 5 b extended in the optical axis direction are formed. The helicoid groove 5 a is formed to move the moving guide frame 6 in the optical axis direction through helicoidal motion. The guide groove 5 b will be described later.
[0047] The guide frame 4 has an end part 4 a formed in a ring shape on the image surface side in the optical axis direction. The guide frame 4 is supported by the fixed frame 1 at the end part 4 . At a plurality of positions along the circumference of the end part 4 a , the guide frame 4 is provided with a plurality of guide keys 4 b protruding in the optical axis direction. In this embodiment, three guide keys 4 b are provided. Each guide key 4 b is configured to be coupled to the moving guide frame 6 in a state where each guide key 4 b is integrated with the moving guide frame 6 in regard to the circumferential direction so as to movably support the moving guide frame 6 in the optical axis direction without letting the moving guide frame 6 rotate about the optical axis.
[0048] The moving guide frame 6 is formed to be a cylindrical shape and is provided with three key grooves 6 a at three positions along the circumferential surface thereof. Between intervals of the key grooves 6 a , cam windows 6 b are formed. Each of the key grooves 6 a engages with a corresponding one of the three guide leys 4 b of the guide frame 4 such that, through engagement between the key grooves 6 a and the guide keys 4 b , the moving guide frame 6 is movable in the optical axis direction with respect to the guide frame 4 without rotating about the optical axis. At an end part on the image surface side of the moving guide frame 6 , the moving guide frame 6 is provided with helicoid projections 6 c protruding outward in the radial direction at a plurality of positions along the circumferential direction.
[0049] The helicoids projection 6 c is engaged with the helicoids groove 5 a on the inner surface of the second cam tube 5 , and when the second cam tube 5 is rotated about the optical axis, the moving guide frame 6 is moved in the optical axis direction by helicoidal motion between the helicoid projection 6 c and the helicoid groove 5 a.
[0050] On the outer circumferential surface of the moving guide frame 6 , the first cam tube 7 is disposed. The first cam tube 7 is disposed to be integrated with the moving guide frame 6 in regard to the optical axis direction while being supported to be movable relative to the moving guide frame 6 around the optical axis. At an end part on the image surface side of the first cam tube 7 , the first cam tube 7 is provided with a plurality of guide projections 7 a , and the guide projections 7 a are engaged with the respective guide grooves 5 b of the second cam tube 5 . With this configuration, when the moving guide frame 6 is moved in the optical axis direction by rotating the second am tube 5 , the first cam tube 7 is also moved in the optical axis direction together with the moving guide frame 6 , and concurrently the first guide tube 7 is rotated integrally with rotation of the second am tube 5 about the optical axis relative to the moving guide frame 6 . Further, on an inner circumferential surface of the first cam tube 7 , three cam grooves including a first cam groove 7 b , a second cam groove 7 c and a third cam groove 7 d are formed. The first, second and third cam grooves 7 b , 7 c and 7 d serve to move the first to third lenses L 1 to L 3 in the optical axis direction.
[0051] Hereafter, configurations of the above described lens systems (i.e., the first to fourth lenses L 1 to L 4 ) will be explained. First, general configurations of the lens systems are explained. FIG. 5A is a schematic diagram generally illustrating arrangement of the first cam tube 7 , the second cam tube 5 and the first to fourth lenses L 1 to L 4 . As shown in FIGS. 5A and 5B , cam followers 8 a , 9 a and 10 a of the first lens frame 8 , the second lens frame 9 and the third lens frame 10 are engaged with the can grooves 7 b , 7 c and 7 d of the first cam tube 7 , respectively. With this configuration, when the second cam tube 5 is operated to rotate, the first cam tube 7 is also rotated integrally, and the first to third lens frames 8 , 9 and 10 are moved in the optical axis direction with rotation of the first cam tube 7 about the axis. Since the second lens frame 9 is formed as a first holding frame, the second lens frame 9 is frequently referred to as a first holding frame 9 hereafter.
[0052] A fourth lens frame 11 is formed integrally with a second holding frame 12 , and the second holding frame 12 is movable in the optical axis direction relative to the first holding frame 9 . The second holding frame 12 is coupled to the first holding frame 9 in regard to the optical axis direction so that an interval between the second holding frame 12 and the first holding frame 9 does not become larger than a predetermined size in the optical axis direction. A compressed coil spring 13 is provided to intervene between the second holding frame 12 and the third lens frame 10 , and the second holding frame 12 is pressed by a spring force of the compressed coil spring 13 in the optical axis direction relative to the first holding frame 9 . With this configuration, in a state where no force acts on the compressed coil spring 13 to contract the compressed coil spring 13 , the second holding frame 12 is moved integrally with the first holding frame 9 in the optical axis direction.
[0053] Hereafter, details about the lens systems are explained. The first lens L 1 placed nearest to an object is a focusing lens, and the first lens frame 8 is formed as a first lens unit 8 . The first lens unit 8 is configured such that a lens frame 8 c holding the first lens L 1 is inserted into a unit tube 8 b having a cylindrical shape. At an end part of the unit tube 8 b on the image surface side, three cam followers 8 a are provided to protrude outward in the radial direction at three positions along the circumferential direction. The cam flowers 8 a are engaged respectively with the first cam grooves 7 b of the first cam tube 7 . With this configuration, the first lens unit 8 is moved in the optical axis direction in accordance with rotation of the first cam tube 7 , and the first lens L 1 is moved in the optical axis direction integrally with the first lens unit 8 . Furthermore, when the moving guide frame 6 is moved in the optical axis direction and thereby the first cam tube 7 is moved in the optical axis direction, the first lens unit 8 is also moved in the optical axis direction.
[0054] In the first lens unit 8 , the lens frame 8 c is provided to be movable in the optical axis direction relative to the unit tube 8 b . Specifically, the lens frame 8 c is screwed into the unit tube 8 b , and a focusing motor 8 d is disposed in the unit tube 8 b . Furthermore, a gear 8 e rotated by the focusing motor 8 d is disposed to engage with a ring gear 8 f provided on the lens frame 8 c . With this configuration, when the focusing motor 8 d is driven, the lens frame 8 c is moved in a screwing manner in the optical axis direction so that the position of the first lens L 1 in the optical axis direction can be adjusted relative to the unit tune 8 and thereby the focusing adjustment is achieved.
[0055] The second lens L 2 is a variator lens, and is held on the second lens frame 9 (i.e., the first holding frame 9 ). The first holding frame 9 is formed by cutting out two portions from a circular plate member, and, at three positions along the circumference, the cam followers 9 a are formed to protrude outward in the radial direction. The cam followers 9 a engage with the second cam groove 7 c of the first cam tube 7 . With this configuration, when the first cam tube 7 is rotated about the axis, the first holding frame 9 is moved in the optical axis direction, and the second lens L 2 held on the first holding frame 9 is also moved in the optical axis direction. Furthermore, when the moving guide frame 6 is moved in the optical axis direction and thereby the first cam tube 7 is moved integrally in the optical axis direction, the first holding frame 9 and the second lens L 2 are also moved in the optical axis direction.
[0056] The first holding frame 9 is provided with a plurality of guide pieces 9 b at a plurality of positions along the circumferential direction. The guide pieces 9 b are formed to protrude in the in the optical axis direction such that the inner diameter slightly decreases toward the image surface side. At and end part of each guide piece 9 b on the image surface side, a guide projection 9 c is formed to protrude inward in the radial direction. As described later, the guide projection 9 c serves to restrict the relative position (i.e., the position in the optical axis direction) of the first holding frame 9 with respect to the second holding frame 12 integrally formed with the fourth lens frame 11 . Furthermore, at two positions along the circumferential direction of the first holding frame 9 , pressing members engaging with the second holding frame 12 are provided. The pressing members are explained later.
[0057] The third lens L 3 is a compensator lens, and is held on the third lens frame 10 . The third lens frame 10 is disposed in an inner region of the first holding frame 9 surrounded by the plurality of guide pieces 9 b , and is provided to be movable in the optical axis direction relative to the first holding frame 9 in a state where the peripheral part of the third lens frame 10 is supported by the guide pieces 9 b . At three positions along the circumferential direction of the third lens frame 10 , arm pieces 10 b each of which is formed to protrude toward the object side are provided. At an end of each arm piece 10 b on the object side, a cam follower 10 a is formed to protrude outward in the radial direction. The cam follower 10 a is engaged with the third cam groove 7 d of the firs cam tube 7 . With this configuration, the third lens frame 10 is moved in the optical axis direction in accordance with rotation of the first cam tube 7 , and the third lens L 3 is moved integrally in the optical axis direction. Furthermore, when the moving guide frame 6 is moved in the optical axis direction and the first cam tube 7 is integrally moved in the optical axis direction, the third lens L 3 is also moved in the optical axis direction.
[0058] The fourth lens L 4 is a relay lens, and is held on the fourth lens frame 11 . The fourth lens frame 11 is integrally supported by the second holding frame 12 . The second holding frame 12 has a circular opening 12 a at a central region including the optical axis, and the fourth lens frame 11 is fitted into the opening 12 a so that the fourth lens frame 11 is integrated with the second holding frame 12 . At a plurality of positions along the circumference of the second holding frame 12 , a plurality of position restriction pieces 12 b respectively corresponding to the plurality of guide pieces 9 b of the firs holding frame 9 are provided to protrude toward the object side in the optical axis direction. The position restriction piece 12 b is formed such that the outer diameter becomes larger toward the object side.
[0059] In this configuration, at an end of each position restriction piece 12 b on the object side, a position restriction part 12 c is formed to protrude outward in the radial direction. Two of the plurality of position restriction pieces 12 b disposed on one side with respect to a virtual diameter line passing through the center of the second holding frame 12 are formed as displaced contacting parts which are described later. Further, at a plurality of positions along the outer circumferential surface of the second holding frame 12 , retracted position restriction parts 12 d are formed to protrude outward in the radial direction.
[0060] As shown in FIG. 2 , the first holding frame 9 and the second holding frame 12 are disposed such that, in a state where the third lens frame 10 is inserted in the inner portion of the first holding frame 9 , the optic axial position restriction pieces 12 b of the second holding frame 12 overlap, in the radial direction, with the corresponding guide pieces 9 b of the first holding frame 9 , on the inner side of the guide pieces 9 b . Between the third lens frame 10 and the second holding frame 12 combined with the first holding frame 9 , the compressed coil spring 13 is disposed. The object side end of the compressed coil spring 13 contacts the image surface side of the third lens frame 10 , and the image side end of the compressed coil spring 13 contacts the object side surface of the send holding frame 12 . With this configuration, the third lens frame 10 and the second holding frame 12 are pressed to separate from one another in the optical axis direction by a pressing force in the axial direction of the compressed coil spring 13 .
[0061] A combined structure of the first holding frame 9 and the second holding frame 12 will now be explained in detail. FIG. 6A is a cross sectional view cut along the optical axis, illustrating the combined state of the first holding frame 9 and the second holding frame 12 . FIG. 6B is an enlarged view of a portion B in FIG. 6A . As described above, the position restriction piece 12 b of the second holding frame 12 overlaps, in the radial direction, with the guide piece 9 b of the first holding frame 9 , on the inner side of the guide piece 9 b . With this configuration, the outer circumferential surface of the position restriction piece 12 b of the second holding frame 12 contacts the inner side end of the guide projection 9 c of the guide piece 9 b of the first holding frame 9 . Through this contact, the second holding frame 12 is supported at the outer circumferential surface of the position restriction piece 12 b in a state where the optical axis of the second holding frame 12 coincides with the optical axis of the first holding frame 9 .
[0062] In this situation, the second holding frame 12 is supported such that the second holding frame 12 is able to move in the optical axis direction relative to the first holding frame 9 . Further, in this combined state, the guide projection 9 c formed on the guide piece 9 b of the first holding frame 9 to protrude inward in the radial direction and the position restriction part 12 c formed on the position restriction piece 12 b of the second frame 12 to protrude outward in the radial direction are disposed to face with each other in the optical axis direction. Therefore, when the holding frames 9 and 12 are moved to become away from one another in the optical axis direction, the guide projection 9 c and the position restriction piece 12 b contact with each other, thereby restricting the optic axial interval between the holding frames 9 and 12 to the maximum optic axial interval.
[0063] FIG. 7A is a side view illustrating the combined state of the first holding frame 9 and the second holding frame 12 viewed from the image surface side. FIG. 7B is a cross sectional view along the line B 1 -B 1 in FIG. 7A . FIG. 7C is an enlarged view of a portion C in FIG. 7B . As shown in FIGS. 7B and 7C , two of the plurality of position restriction pieces 12 b provided on the second holding frame 12 (i.e., two position restriction pieces 12 b disposed on one side with respect to a virtual line passing through the optical axis) are formed as displaced contacting parts 12 e . Each displaced contacting part 12 e is formed such that the thickness thereof becomes larger at a point closer to the object side. An outer surface of the displaced contacting part 12 e is formed to be a slope surface 12 f . Furthermore, an outer surface of an end of the displaced contacting part 12 e on the object side of the slope surface 12 f is formed as a reversed tapered surface 12 g having the thickness which becomes smaller at a point closer to the tip side. In this configuration, a pressing member 14 provided on the first holding frame 9 elastically contacts the tapered surface 12 g.
[0064] The pressing members 14 are provided at positions which are along the circumferential direction of the first holding frame 9 and respectively correspond to the two displaced contacting parts 12 e of the second holding frame 12 . Each of the two pressing members 14 is formed of a spring piece 14 a formed by bending a strip-like leaf spring member, and an object side proximal part 14 b thereof is fixed to the image side surface of the first holding frame 9 by a screw 14 d . An image side tip part 14 c of the spring piece 14 a is bent in a shape of a wedge, and the spring piece 14 a is disposed such that an inner surface of the tip part 14 c contacts the tapered surface 12 g of the displaced contacting part 12 e from the outer diameter side toward the inner diameter side. With this configuration, through an elastic force of the spring piece 14 a , the tip part 14 c of the spring piece 14 a elastically contacts the tapered surface 12 g toward the inner diameter side. As a result, the two displaced contacting parts 12 e are pressed toward the inner diameter side by the pressing members 14 , and, through this pressing force of the pressing member 14 , the entire second holding frame 12 is applied a displacing force toward one direction along the radial direction which is perpendicular to the optical axis direction.
[0065] The extending and contracting operation of the lens barrel LL configured as described above will now be explained. As shown in FIG. 2 , in a short focus length state (a wide state) during the photographing operation, the variable power ring 3 is rotated in one rotational direction, and, in this case, the second cam tube 5 is integrally rotated in the same rotational direction. Therefore, through the helicoidal motion between the helicoids groove 5 a of the second cam tube 5 and the helicoid projection 6 c of the moving guide frame 6 engaging with the helicoids groove 5 a , the moving guide frame 6 is moved toward the object side in the optical axis direction. Concurrently, the first cam tube 7 integrally formed with the moving guide frame 6 in regard to the optical axis direction is also moved toward the object side in the optical axis direction. At this time, due to key coupling with the guide frame 4 , the moving guide frame 6 is not rotated about the optical axis; however, the first cam tube 7 is rotated integrally with the second am tube 5 about the optical axis. FIG. 5A schematically shows this state.
[0066] When the first cam tube 7 is rotated about the optical axis, through cam motion by engagement between the first cam groove 7 b of the first cam tube 7 and the cam follower 8 a of the first lens unit 8 , the first lens unit 8 is moved toward the object side in the optical axis direction. Through such movement of the first cam tube 7 in the optical axis direction and movement of the first lens unit 8 in the optical axis direction, the length of the entire lens barrel LL becomes an extended state.
[0067] Concurrently, through cam motion between the second am groove 7 c of the first cam tube 7 and the cam follower 9 a of the first holding frame 9 , the first holding frame 9 is also moved toward the object side in the optical axis direction. FIG. 8A schematically shows this state. When the first holding frame 9 is moved toward the object side in the optical axis direction, the first holding frame 9 is brought to the state of being positioned away from the second holding frame 12 , and when the first holding frame 9 is separated from the second holding frame 12 by a predetermined axial distance, the guide projection 9 c of the first holding frame 9 contacts the outer circumferential surface of the second holding frame 12 . As a result, the second holding frame 12 is position in regard to a direction perpendicular to the optical axis direction by the guide projection 9 c , and thereby the first holding frame 9 and the second holding frame 12 are brought to the state where the optical axes thereof coincide with each other.
[0068] As the first holding frame 9 is further moved toward the object side in the optical axis direction and the interval between the first holding frame 9 and the second holding frame 12 gets larger, the guide projection 9 c of the first holding frame 9 and the position restriction part 12 c of the second holding frame 12 contact with each other in regard to the optical axis direction, as a result, the first holding frame 9 and the second holding frame 12 are coupled in regard to the optical axis direction, and thereby the second holding frame 12 is moved toward the object side integrally in accordance with movement of the first holding frame 9 in the optical axis direction.
[0069] When the variable power ring 3 is rotated within a required rotational angle range in one rotational direction or a reversed rotational direction, the first cam tube 7 is rotated accordingly, and, due to engagement of the third cam groove 7 d of the first cam tube 7 and the cam follower 10 a of the third lens frame 10 , the third lens frame 10 is moved toward the object side or the image side in the optical axis direction. As a result, as shown in FIG. 9 , when the third lens frame 10 bends the compressed coil spring 13 and is moved to the object surface side, the lens barrel LL becomes the long focal length state (a tele-state). FIG. 8B schematically illustrates the second to fourth lenses L 2 to L 4 in this state.
[0070] During the photographing operation in the wide state or the tele-state, in the first lens unit 8 , the focus adjustment is performed by moving the lens frame 8 c in a screwing motion in the optical axis direction while driving the focusing motor 8 d in the unit tube 8 b , and thereby adjusting the position of the first lens L 1 in the optical axis direction with respect to the unit tube 8 b . Since a general focus adjustment manner can be used in this embodiment, detailed explanation about the focus adjustment will be omitted.
[0071] FIG. 10 is a cross sectional view of the lens barrel LL in the contracted state during the non-photographing operation. When the variable power ring 3 is rotated to a rotational position closer to an end edge on an opposite side with respect to the above described one direction, through the helicoidal motion between the helicoid groove 5 a of the second cam tube 5 integrally rotated with the variable power ring 3 and the helicoid projection 6 a of the moving guide frame 6 engaging with the helicoid groove 5 a , the moving guide frame 6 is moved toward the image surface side in the optical axis direction. Concurrently, the first cam tube 7 integrally disposed with the moving guide frame 6 in the optical axis direction is also moved toward the image surface side in the optical axis direction. As a result, the moving guide frame 6 and the first cam tube 7 are accommodated in the inner diameter portion of the fixed frame 1 and the second cam tube 5 .
[0072] Since, at this time, the first cam tube 7 is rotated about the optical axis integrally with the second cam tube 5 as the firs cam tube 7 is moved in the optical axis direction, the first lens unit 8 is moved toward the image surface side by the first cam groove 7 b and is accommodated in the inner diameter portion of the first cam tube 7 . Concurrently, the first holding frame 9 is moved toward the image surface side by the second cam groove 7 c . Further, the third lens frame 10 is moved toward the image surface side by the third cam groove 7 d . By such movement of the third lens frame 10 toward the image surface side, the compressed coil spring 13 is contracted, and thereby the moving force of the third lens frame 10 is transmitted to the second holding frame 12 via the compressed coil spring 13 , and the second holding frame 12 is moved toward the image surface side.
[0073] The second holding frame 12 is moved toward the image surface side to reach the inner diameter position of the guide frame 4 and the fixed frame 1 , and movement of the second holding frame 12 is restricted in a state where the retracted position restriction part 12 d provided on the second holding frame 12 contacts the object side surface of the guide frame 4 . By such restriction, the second holding frame 12 (i.e., the fourth lens L 4 ) is accommodated in the inner diameter portion of the fixed frame 1 . Further, the second holding frame 12 is pressed toward the guide frame 4 by a spring force of the compressed coil spring 13 intervening between the second holding frame 12 and the guide frame 4 , and thus the moving position of the second holding frame 12 is restricted. FIG. 8C schematically illustrates the second to fourth lenses L 2 to L 4 in this state.
[0074] Thus, the first lens unit 8 , the first holding frame 9 , the third lens frame 10 and the second holding frame 12 are respectively moved toward the image surface side, and the lens barrel LL is set to the contracted state as shown in FIG. 10 . With this configuration, the tube length (i.e., the size in the optical axis direction) of the lens barrel LL in the non-photographing state can be reduced, and thereby portability of the lens barrel can be enhanced. FIG. 5B is a schematic view of the lens barrel in this state.
[0075] Regarding mutual motion of the first holding frame 9 and the second holding frame 12 , during the photographing operation of the lens barrel LL, the guide projection 9 c of the first holding frame 9 and the position restriction part 12 c of the second holding frame 12 contact with each other in regard to the optical axis direction as shown in FIG. 11A where only the first holding frame 9 and the second holding frame 12 are illustrated for the sake of simplicity. Thus, the first holding frame 9 and the second holding frame 12 are coupled together at the optic axial interval defined when the guide projection 9 c of the first holding frame 9 and the position restriction part 12 c of the second holding frame 12 contact with each other. In particular, since the second holding frame 12 is pressed toward the image surface side by the compressed coil spring 13 intervening between the second holding frame 12 and the third lens frame 10 , the guide projection 9 c and the position restriction part 12 c elastically contact with each other by the spring force of the compressed coil spring 13 and thereby the contacting state of the first holding frame 9 and the second holding frame 12 (i.e., the optic axial interval between the first holding frame 9 and the second holding frame 12 ) is kept constant. Furthermore, since the tip part 14 c of the pressing member 14 of the first holding frame 9 elastically contacts the tapered surface 12 g of the displaced contacting part 12 e of the second holding frame 12 , a component of force in the axial direction of the elastic contacting force acting on the tapered surface 12 g supports the elastic contact between the guide projection 9 c and the position restriction part 12 c.
[0076] Therefore, in the lens barrel LL, during the photographing operation, the second holding frame 12 is moved in the optical axis direction while keeping the optic axial interval between the second holding frame 12 and the first holding frame 9 constant, and the focal length is adjusted from the tele-state to the wide state through movement of the third lens frame 10 in the optical axis direction. That is, the first holding frame 9 and the second holding frame 12 are moved in the optical axis direction in the state where the first holding frame 9 and the second holding frame 12 are coupled in regard to the optical axis direction, and thereby the variable power characteristics can be enhanced.
[0077] As shown in FIG. 11B , when the lens barrel LL is contracted, the first holding frame 9 is moved toward the image surface side by the second cam groove 7 c , and at this state the optic axial interval between the first holding frame 9 and the second holding frame 12 is maintained through the effect of the guide projection 9 c , the position restriction part 12 , the compressed coil spring 13 and the pressing member 14 . Accordingly, the second holding frame 12 is moved toward the image surface side together with the first holding frame 9 . When the retracted position restriction part 12 d of the second holding frame 12 contacts the guide frame 4 and further movement of the second holding frame 12 toward the image surface side is restricted, the guide projection 9 c of the first holding frame 9 and the position restriction part 12 c of the second holding frame 12 separate with respect to each other. Therefore, the first holding frame 9 is continuously moved toward the image surface side regardless of the fact that the movement of the second holding frame 12 toward the image surface side is restricted. Further, when the tip of the guide projection 9 c contacts the object side surface of the guide frame 4 and the lens barrel LL becomes the contracted state, further movement of the first holding frame 9 is restricted.
[0078] When the lens barrel LL is contracted, the inner edge of the guide projection 9 c gradually and slightly separates in the radial direction from the outer circumferential surface of the position restriction piece 12 c as the optic axial interval between the first holding frame 9 and the second holding frame becomes smaller because each of the guide piece 9 b and the position restriction piece 12 c is formed such that the inner diameter becomes larger at a point closer to the object side. As a result, the position restriction piece 12 c (i.e., the second holding frame 12 ) has a degree of freedom in the radial direction. Accordingly, when the second holding frame 12 and the first holding frame 9 contact the guide frame 4 and thereby movement thereof is restricted, the guide piece 9 c and the position restriction piece 12 c are prevented from interfering with each other, and thereby smooth contracting motion of the lens barrel LL can be achieved.
[0079] Furthermore, since the tip part 14 c of the spring piece 14 a of the pressing member 14 elastically contacts the tapered surface 12 g of the displaced contacting part 12 e , the displaced contacting part 12 e (i.e., the second holding frame 12 ) is pressed in a direction perpendicular to the optical axis by the pressing member 14 . Therefore, even when a gap exists between the second holding frame 12 and the first holding frame 9 in the radial direction, the second holding frame 12 is displaced in the radial direction by the pressing force from the pressing member 14 in the direction perpendicular to the optical axis, and thereby the second holding frame 12 closely contacts the first holding frame 9 on the opposite side of the region where the pressing member 14 is disposed. As a result, such a gap between the first holding frame 9 and the second holding frame 12 can be absorbed. Accordingly, during the photographing operation, it is possible to maintain the positions of the first holding frame 9 and the second holding frame 12 in the optical axis direction (i.e., it is possible to maintain the state where the optical axes of the second lens L 2 and the fourth lens IA coincide with each other).
[0080] In the lens barrel LL according to the embodiment, the slope surface 12 f is formed on the displaced contacting part 12 e . Therefore, when the first holding frame 9 and the second holding frame 12 move relative to each other in the optical axis direction, the tip part 14 c of the spring piece 14 a of the pressing member 14 contacts and slides on the slope surface 12 f . As a result, rapid change of the pressing force (the elastic contacting force) can be prevented when the pressing member 14 contacts or separates from the tapered surface 12 g . Further, occurrence of impact on the lens barrel LL during the contracting motion or extending motion of the lens barrel LL can be prevented.
[0081] Variations
[0082] In the following, variations of the lens barrel LL are described. The following explanation focuses on features of modified configurations of the lens barrel LL.
[0083] In the above described embodiment, the second holding frame 12 is pressed in the direction perpendicular to the optical axis to absorb the gap in the radial direction by causing the pressing member 14 to contact the displaced contacting part 12 e of the second holding frame 12 . However, the displaced contacting part 12 e may be formed to have an elastic property in regard to the radial direction such that the displaced contacting part 12 e contacts the guide piece 9 b of the first holding frame 9 in the radial direction. In this case, the second holding frame 12 is pressed in the direction perpendicular to the optical axis thanks to the elastic property of the displaced contacting part 12 . As a result, the pressing member can be omitted.
[0084] In the lens barrel, position restriction of the second holding frame 12 toward the image surface side may be achieved by a part of a lens system. FIG. 12A schematically illustrates such a configuration. In this example, the lens barrel is provided with a fifth lens L 5 on the image surface side of the fourth lens L 4 . Specifically, a fifth lens frame 15 of the fifth lens L 5 has a cam follower 15 a , and the can follower 15 a engages with a fourth cam groove 7 e formed on the first cam tube 7 . In this example, the fifth lens L 5 moves only by a slight moving amount in the optical axis direction in accordance with rotation of the first cam tube 7 .
[0085] The fifth lens frame 15 is formed as a third holding frame. The third holding frame stays substantially at the same position in the optical axis direction on the image surface side of the fourth lens L 4 . Therefore, when the lens barrel is contracted, as shown in FIG. 12B , the second holding frame 12 (a fourth lens frame in this example) contacts the third holding frame 15 . With this configuration, it becomes possible to restrict the position of the second holding frame 12 and the first holding frame 9 in the optical axis direction during the contracting motion of the lens barrel, and thereby the suitable contracting motion of the lens barrel can be achieved.
[0086] The lens barrel may be provided with a mechanism enabling adjustment of lens positions of the lenses held on the first to third lens frames both in the optical axis direction and the direction perpendicular to the optical axis. In this example, a lens position adjustment mechanism for the fourth lens LA held on the second holding frame 12 is explained. FIG. 13A is a perspective view illustrating the lens position adjustment mechanism, and FIG. 13B illustrates the lens position adjustment mechanism viewed from the image surface side along the optical axis. FIG. 14A is an exploded perspective view of the lens position adjustment mechanism.
[0087] In FIGS. 13A and 13B , the fourth lens L 4 is held on the second holding frame 12 via the fourth lens frame 11 , and the fourth lens frame 11 is configured to be able to move in the optical axis direction and the direction perpendicular to the optical axis relative to the second holding frame 12 . Specifically, as shown in FIG. 14A , at the image surface side edge of the second holding frame 12 , a ring-shaped fixed ring 16 is supported integrally with the second holding frame 12 . On an inner diameter side of the fixed ring 16 , a ring-shaped adjustment ring 17 is inserted and supported to be able to rotate about the optical axis. Further, the fourth lens frame 11 is held by the fixed ring 16 and the second holding frame 12 while sandwiching the adjustment ring 17 between the second holding frame 12 and the fourth lens frame 11 in the state where the fourth lens frame 11 contacts the image side surface of the adjustment ring 17 .
[0088] At three equally divided positions along the circumferential direction of the fourth lens frame 14 , tension coil springs 18 a each having an elastic force in the optical axis direction are disposed. Each of the tension coil springs 18 a is provided such that an end of the coil spring 18 a is hooked to the second holding frame 12 and the other end of the coil spring 18 a is hooked to the fourth lens frame 11 . With this configuration, the fourth lens frame 11 elastically contacts the adjustment ring 17 by a drawing force of the three tension coil springs 18 a , and is held on the second holding frame 12 by this drawing force.
[0089] At two positions along the circumferential direction of the fourth lens frame 11 (namely, at two positions on one side of a virtual diameter line), compressed coil springs 18 b each having an elastic force in the radial direction are disposed to intervene between the fixed ring 16 and the fourth lens frame 11 . Therefore, the fourth lens frame 11 is pressed, by the compressed coil springs 18 b , toward one radial direction in a plane perpendicular to the optical axis with respect to the fixed ring 16 (i.e., the second holding frame 12 ).
[0090] At two positions in the circumferential direction opposite to the above described one side with respect to the virtual diameter line of the fourth lens frame 11 , adjustment cams 19 disposed on and supported by the fixed ring 16 are provided to contact the fourth lens frame 11 . The adjustment cam 19 is formed to be a circular eccentric cam, and is disposed such that a circumferential surface of the adjustment cam 19 (i.e., a can surface) contacts a circumferential edge of the fourth lens frame 11 in the radial direction. Each of the adjustment cams 19 is formed to have a slit on one surface thereof facing in the optical axis direction, and can be rotated through a rotation operation thereto via the slit using a jig. By this rotation operation, the forth lens frame 11 contacting a cam surface of the adjustment cam 19 can be pressed in the radial direction.
[0091] FIG. 14B is a perspective view of the adjustment ring 17 viewed from the object side. As shown in FIG. 14B , the adjustment ring 17 is integrally formed with a contacting projection 17 a on the object side surface in the optical axis direction. The contacting projection 17 a contacts, in the optical axis direction, a tapered end surface 12 h formed on the image side end part of the second holding frame 12 . The tapered end surface 12 h is formed to be inclined along the circumferential direction, and is displaced in the optical axis direction by the positional difference of the tapered end surface 12 h along the circumferential direction. Further, the adjustment ring 17 is provided with an operation projection 17 b at a part of the image side surface thereof, and is exposed to the image surface side through an arc-shaped window part 11 a formed in the fourth lens frame 11 . By operating the operation projection 17 b in the circumferential direction through the window part 11 a , the position of the adjustment ring 17 in the rotational direction about the optical axis can be adjusted.
[0092] According to the above described lens position adjustment mechanism, by operating the adjustment cam 19 to rotate, the adjustment cam 19 presses, in the radial direction, the periphery of the fourth lens frame 11 contacting the cam surface of the adjustment cam 19 . As a result, the fourth lens frame 11 is moved in the radial direction while bending the compressed coil springs 18 b . Therefore, by appropriately rotating the two adjustment cams 19 , the fourth lens frame 11 can be moved in a plane perpendicular to the optical axis. As a result, it becomes possible to cause the center of the fourth lens frame 11 (i.e., the optical axis of the fourth lens L 4 ) to coincide the optical axis of the lens barrel LL.
[0093] When the position of the adjustment ring 17 is adjusted by operating the operation projection 17 b around the optical axis, the contacting projection 17 a of the adjustment ring 17 is moved along the tapered end surface 12 h while contacting the tapered end surface 12 h of the second holding frame 12 . Therefore, the position of the contacting projection 17 b in the optical axis direction is changed by the tapered end surface 12 h . Accordingly, the fourth lens frame 14 which is caused to elastically contact the image side surface of the adjustment ring 17 by the tension coil springs 18 a is also moved in the optical axis direction integrally with the adjustment ring 17 . As a result, the position of the fourth lens frame 11 (i.e., the position of the fourth lens L 4 in the optical axis direction) can be adjusted. Therefore, even when a position shift in the optical axis direction and/or in the direction perpendicular to the optical axis is caused between the first holding frame 9 and the second holding frame 12 , the lens barrel having a high degree of quality can be provided by adjusting the position of the fourth lens L 4 .
[0094] It is understood that the above described lens position adjustment mechanism can be applied not only to the fourth lens IA but also to the other lens systems.
[0095] In the above described embodiment, each of the first to fifth lenses may be configured as a lens group.
[0096] In the above described embodiment, the disclosed feature is applied to the lens barrel; however, in another embodiment, the disclosed feature may be applied to other optical devices. That is, an optical element used in the optical device to which the disclosed feature is applied is not limited to a lens or a lens group, but may be various types optical elements, such as, an aperture stop, a shutter, a filter or an image pickup device (e.g., a CMOS device).
[0097] The disclosed feature may be applied to a monocle, binoculars, a telescope, a camera module or a lens module for various types of mobile devices, in addition to a lens barrel for a lens interchangeable camera, a lens barrel for a compact camera, a lens barrel for a camcorder.
[0098] The foregoing is the explanation about the embodiment of the invention. The invention is not limited to the above described embodiment, but can be varied in various ways within the scope of the invention. For example, the invention includes a combination of embodiments explicitly described in this specification and embodiments easily realized from the above described embodiment.
[0099] This application claims priority of Japanese Patent Application No. 2015-018947, filed on Feb. 3, 2015. The entire subject matter of the application is incorporated herein by reference. | Optical Equipment, comprising: a first holding unit that holds a first optical element; and a second holding unit that holds a second optical element, wherein: the first holding unit and the second holding unit are provided to be movable in an optical axis direction so as to allow the optical equipment to reduce a length in the optical axis direction; the first holding unit is configured to be driven by a driving unit in the optical axis direction; and the second holding unit is coupled to the first holding unit in regard to the optical axis direction such that the second holding unit is allowed to move integrally with the first holding unit and is allowed to move relatively to the first holding unit. | 6 |
FIELD OF THE INVENTION
[0001] The present invention relates to antennas. More specifically, the invention relates to a method and apparatus for providing an antenna exhibiting improved RF signal reception and transmission due to reduced levels of RF signal reflection loss and dielectric loss.
BACKGROUND OF THE INVENTION
[0002] Radio frequency (RF) antennas are widely used to transmit and receive energy in the form of radio waves. RF antennas are available in many different shapes, sizes and configurations. One type of RF antenna is the Cassegrain antenna. Cassegrain antennas have a hyperbolic shaped subreflector. The sub-reflector is coaxially aligned with and aimed at an axial center of a main parabolic reflector. The sub-reflector is suspended above the main reflector by either a solid support tube extending from a point near the center of the main reflector, one or more support rods extending from a point near the center of the reflector, or one or more support rods extending from a periphery of the main reflector. When the antenna is in the receive mode the sub-reflector directs RF energy received and reflected by the main reflector to a waveguide (i.e., feedhorn) located at the axial center of the main reflector. When the antenna is in the transmit mode, RF energy transmitted from the waveguide is reflected by the sub-reflector onto the main reflector where the energy is radiated from the antenna.
[0003] While the above described Cassegrain antenna is able to adequately send and receive radio signals, it would be desirable to improve its operating efficiency. Specifically, Cassegrain antennas and all other types of antennas which employ the use of a device suspended above a main reflector, such as a horn antenna, patch antenna, etc., suffer transmission losses due to the RF signal being blocked and reflected by the device support members. Such support members are usually in the form of solid support tubes or support rods that exhibit large dielectric constants. Consequently, there is a need for an improved antenna exhibiting reduced levels of reflection loss and dielectric loss, resulting in enhanced RF signal transmission and reception.
SUMMARY OF THE INVENTION
[0004] The present invention overcomes prior art deficiencies by providing an antenna exhibiting improved RF transmission and reception capabilities. Unlike previous antennas, the antenna of the present invention does not make use of a solid support tube or solid support rods to support a sub-reflector or other feed device above a main reflector of the antenna. Instead, the present invention provides an antenna having a sub-reflector or other feed device positioned above a main reflector by a perforated support tube (dielectric) having walls with a low dielectric constant. The perforated support tube permits RF signals to pass through the tube, thus decreasing the signal degradation which would be experienced due to reflection of the signal off the walls of a solid support tube or solid support rods. The perforations may be in the form of holes, slots, or numerous other arrangements.
[0005] Further areas of applicability of the present invention will become apparent from the detailed description provided hereinafter. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] The present invention will become more fully understood from the detailed description and the accompanying drawings, wherein:
[0007] [0007]FIG. 1 is a side view of an antenna in accordance with a first preferred embodiment of the present invention;
[0008] [0008]FIG. 2 a is a perspective view of the perforated support tube of the antenna of FIG. 1;
[0009] [0009]FIG. 2 b is a side view of an alternative preferred form of the support tube;
[0010] [0010]FIG. 2 c is a side view of another alternative preferred form of the support tube;
[0011] [0011]FIG. 3 is a perspective view of the attachment ring of the antenna of FIG. 1;
[0012] [0012]FIG. 4 is a perspective view of the support tube cap of the antenna of FIG. 1;
[0013] [0013]FIG. 5 is a perspective view of the sub-reflector of the antenna of FIG. 1;
[0014] [0014]FIG. 6 is a partial side view of an antenna in accordance with a second preferred embodiment of the present invention with a broken away section of the support tube to better show the patch antenna assembly;
[0015] [0015]FIG. 7 is a perspective view of the patch assembly of the antenna of FIG. 6;
[0016] [0016]FIG. 8 is a side view of the patch assembly of the antenna of FIG. 6; and
[0017] [0017]FIG. 9 is a top view of the patch assembly of the antenna of FIG. 6.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0018] The following description of the preferred embodiment(s) is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses.
[0019] As seen in FIG. 1, an antenna 10 in accordance with a first preferred embodiment of the present invention is shown. The antenna 10 contains a hyperbolic sub-reflector 12 and a parabolic main reflector 14 . The main reflector 14 has a first surface 16 and a second surface 18 . The sub-reflector 12 is mounted to the first surface 16 by a perforated plastic support tube 20 . RF signals received by the first surface 16 are reflected by the sub-reflector 12 to a waveguide in the form of a feedhorn 21 . RF signals transmitted through the feedhorn 21 are reflected by the sub-reflector 12 to the first surface 16 and radiate from the first surface 16 into space. RF signals received by the antenna 10 are carried from the antenna 10 through a suitable conducting device, such as a coaxial cable (not shown). The conducting device may also carry RF signals to antenna 10 to be transmitted by antenna 10 . The conducting device is connected to the antenna 10 by way of a TNC connector 22 disposed on the second surface 18 of antenna 10 .
[0020] With reference to FIG. 2, the perforated plastic support tube 20 will now be described in detail. The perforated tube 20 is comprised of a top portion 23 , a bottom portion 24 , and a mid-portion 26 . The bottom portion 24 contains a series of small holes 28 capable of receiving suitable fastening devices, such as threaded fastening devices or rivets. The top portion 23 similarly contains a first series of small holes 30 and a second series of small holes 32 , both capable of receiving suitable fastening devices, such as the fasteners or rivets described above. Mid-portion 26 contains a plurality of apertures 34 , the apertures 34 being of any suitable size or configuration so as to allow the passage of RF signals easily through the tube 20 . The apertures 34 may be in the form of circular holes as illustrated in FIG. 2 a . An alternative form of the support tube 20 ′ is shown in FIG. 2B wherein the circular holes are replaced by radial slot openings 34 ′. Still another preferred form of the support tube 20 ″ is shown in FIG. 2C wherein the circular holes are replaced by longitudinal slot openings 34 ″. In one preferred form the support tube 20 is formed from a suitably strong plastic, although it will be appreciated that other materials such as, but not limited to, steel or aluminum may also be used. A perforated steel or aluminum support tube could function as a frequency selective surface (FSS).
[0021] The perforated tube 20 is affixed to the first surface 16 of the main reflector 14 by way of an attachment ring 36 shown in FIG. 3. The attachment ring 36 is a circular ring comprised of a base portion 38 and an annular rim 40 . Formed within the base portion 38 is a plurality of small holes 42 capable of receiving suitable fastening devices such as threaded screws. Similar small holes 44 capable of receiving fastening devices, such as threaded screws, are formed in the annular rim 40 .
[0022] The small holes 42 of the base portion 38 cooperate with similar holes (not shown) circumscribing the focal point of the first surface 16 of the main reflector 14 . Suitable fastening devices are inserted through small holes 42 and the holes (not shown) of the first surface 16 to secure the base portion 38 to the first surface 16 . The base portion 38 serves as a support to secure the perforated support tube 20 to the main reflector 14 . Specifically, the perforated support tube 20 is secured to the attachment ring 36 through cooperation of small holes 44 of the annular rim 40 and small holes 28 of the support tube 20 . Small holes 28 and small holes 44 are secured to each other by a suitable fastening device such as screws that are inserted through aligned pairs of small holes 28 and 44 .
[0023] The top portion 23 of the perforated support tube 20 is covered by a support tube end cap 46 as shown in FIG. 4. The cap 46 is comprised of a flat surface portion 48 and a rim portion 50 . The rim portion 50 contains a plurality of small holes 52 for receiving suitable fastening devices such as threaded fasteners or rivets. The small holes 52 are aligned with the first series of small holes 30 and end cap 46 is secured to the support tube 20 by fastening devices extending through the aligned pairs of small holes 30 and 52 .
[0024] Referring now to FIG. 5, the sub-reflector 12 is shown in detail. The sub-reflector 12 contains a cone portion 54 and a circular peripheral base portion 56 . The peripheral base portion 56 contains a series of small holes 58 that cooperate with the second series of small holes 32 . Suitable fastening elements are inserted through aligned pairs of small holes 58 and small holes 32 to secure the sub-reflector 12 to the perforated support tube 20 .
[0025] As seen in FIG. 6, an antenna 10 a in accordance with a second preferred embodiment of the present invention is shown. Antenna 10 a , like antenna 10 of the first preferred embodiment, is comprised of a parabolic main reflector 14 a having a first surface 16 a and a second surface 18 a . Mounted to the first surface 16 a , by way of an attachment ring 36 a , is a perforated plastic support tube 20 a having an end cap 46 a . Mounted to the second surface 18 a is a TNC connector 22 a . As these components of antenna 10 a are identical to those of antenna 10 , there is no need to describe them again in detail with reference to antenna 10 a.
[0026] In addition to the antenna elements described above, antenna 10 a has a patch antenna assembly 60 . The patch antenna assembly 60 is illustrated in detail in FIGS. 7, 8, and 9 . The patch antenna assembly 60 is generally comprised of a patch antenna 62 and a patch attachment ring 64 . The patch antenna assembly 60 is mounted to the first surface 16 a by the perforated plastic support tube 20 a.
[0027] The patch antenna 62 is comprised of a dielectric substrate 66 , a patch element 68 and a ground plane 70 . Both the patch element 68 and the ground plane 70 are preferably made of copper. The copper patch element 68 covers a first end 72 of the dielectric substrate 66 , except for an outer periphery of the first end 72 . At the center of the patch element 68 is hole 74 which is used to receive a suitable conducting device such as coaxial cable 76 . A corresponding hole (not shown) is located in dielectric substrate 66 .
[0028] The ground plane 70 completely covers and is bonded to a second end 78 of the dielectric substrate 66 . The ground plane 70 is preferably made of copper and includes a hole (not shown) aligned with hole 74 of the patch element 68 and the hole (not shown) of the dielectric substrate 66 . The surface of the ground plane not bonded to the dielectric substrate 66 is bonded to the patch attachment ring 64 .
[0029] The patch attachment ring 64 is preferably made of metal. The patch attachment ring 64 is comprised of a ring portion 80 and a surface portion 82 . The ring portion 80 contains a plurality of small holes 84 . The plurality of small holes 84 are aligned with the second series of small holes 32 a of the support tube 20 a and both are capable of receiving suitable fastening devices, such as fasteners or rivets, to secure the patch antenna assembly 60 to the support tube 20 a.
[0030] The surface portion 82 of the patch attachment ring 64 contains cross members 86 and 88 . At the intersect point of cross members 86 and 88 is a hole 90 . Hole 90 is sized to receive coax cable 76 and is aligned with hole 74 , the hole of the dielectric substrate 66 , and the hole of ground plane 70 . Either cross member 86 or cross member 88 also has a connector 92 for receiving the coax cable 76 .
[0031] RF signals received by the main reflector 14 a of antenna 10 a are directed from the main reflector 14 a to the patch antenna 62 . From the patch antenna 62 the RF signals are conducted through the coaxial cable 76 to a TNC connector 94 disposed at the axial center of the first surface 16 a of the main reflector 10 a . From connector 94 the signals are conducted from the antenna by way of a suitable conductive device, such as a coaxial cable (not shown), that is attached to connector 22 a . Likewise, RF signals to be transmitted by antenna 10 a are received by the antenna 10 a through connector 22 a and are carried to the patch antenna 62 by way of the coaxial cable 76 . The RF signals to be transmitted radiate from the patch antenna 62 where they are reflected by the first surface 16 a of the main reflector 14 a into space. It must be noted that antenna 10 a does not require the use of a feedhorn as antenna 10 does.
[0032] While FIGS. 1, 2, and 6 illustrate the second series of small holes 32 being used to support the sub-reflector 12 and the patch assembly 60 , it should be understood that small holes 32 may be configured to support a variety of antenna-related elements called for in a variety of different antennas. It will also be appreciated that other forms of fastening systems, including adhesives, could be used in place of the threaded fastening elements and rivets described herein.
[0033] The use of perforated tube 20 to support the sub-reflector 12 , patch assembly 60 , or any other device enhances the signal strength of the signal received or transmitted by the antenna 10 . Traditionally, the sub-reflector 12 , patch assembly 60 , or other device has been suspended above the main reflector 14 by a solid support tube or solid support rods. However, such a configuration is undesirable because the RF energy radiated or transmitted from the antenna reflects off the solid support tube or solid support rods due to the high dielectric constant exhibited by such supports. As a result of this high dielectric constant, the signal strength of the RF signal received by, or transmitted from, the antenna is degraded.
[0034] In contrast to the prior art antennas, perforated support tube 20 exhibits a decreased dielectric constant as the apertures 34 allow RF signals to pass though the support tube 20 with the signals being reflected less frequently. Because the RF signals are reflected less frequently, antenna 10 is more efficient and is able to receive and transmit RF energy with less signal degradation.
[0035] Thus, an improved antenna exhibiting a perforated support tube with a decreased wall dielectric constant and, consequently, decreased levels of signal degradation due to signal reflection is provided. The decrease in signal degradation is due to the presence of the perforated support tube 20 to support the sub-reflector 12 , patch assembly 60 , or any other desired device above the main reflector 14 . The use of perforated support tube 20 provides an antenna 10 which exhibits a dielectric constant that is significantly lower than prior art antennas. Consequently, RF signal reflection loss is reduced by the perforated support tube and the RF signals received or transmitted are of a greater strength and quality than the signals of prior art antennas. The principles of the present invention are applicable to all support tubes (dielectric) with perforated holes or slots in the wall of the tube to lower the effective dielectric constant.
[0036] The description of the invention is merely exemplary in nature and, thus, variations that do not depart from the gist of the invention are intended to be within the scope of the invention. Such variations are not to be regarded as a departure from the spirit and scope of the invention. | An antenna exhibiting improved radio frequency transmission and reception capabilities. The antenna does not make use of a solid support tube or solid support rods used by previous antennas to support a sub-reflector or other device above a main reflector of the antenna. Instead, the antenna employs the use of a low dielectric constant, perforated, support tube to support the sub-reflector, patch antenna, or other form of antenna element above the main reflector. The perforated support tube permits radio frequency signals to pass through the tube, thus decreasing signal degradation experienced due to reflection of the signal off the solid support tube or off the solid support rods. | 7 |
BACKGROUND OF THE INVENTION
This invention relates, in general, to radio navigation receivers, and more specifically, to a rapid acquisition GPS (Global Positioning System) receiver.
Radio navigation systems are used in tracking aircraft, boats, and land vehicles such as trucks and emergency vehicles. To avoid the limitations inherent in navigation systems utilizing terrestrial transmitters, the GPS has been developed and maintained by the U.S. Government. The GPS uses a network of satellites which can be accessed anywhere in the range of the orbiting satellites. An explanation of the operation of the GPS, as well as a history of the receivers designed to operate with the GPS, is found in U.S. Pat. No. 4,785,463 issued Nov. 15, 1988 to Robert V. Janc and Steven C. Jasper, and U.S. Pat. No. 4,701,934 issued Oct. 20, 1987 to Steven C. Jasper. Both patents are assigned to the same assignee as the present invention.
Rapid acquisition of GPS signals is often more important than accuracy of the information received, particularly in an environment where signal dropout due to interference is likely. Current techniques for signal acquisition, such as those described in the above referenced patents, require several seconds for acquisition. A major factor distinguishing GPS receivers, particularly small, low cost receivers requiring less power, is the speed of acquisition of the GPS signals. The faster the acquisition rate with reasonable accuracy, the more competitive the receiver is.
Another feature of a receiver which is necessary to ensure competitiveness in the GPS receiver market is the ability of the receiver to track multiple satellites simultaneously. In an effort to track satellites, GPS receivers to date have incorporated either sequential or parallel layout architectures. Advocates of sequential architecture claim that sequential architecture receivers reduce hardware cost and reduce interchannel biases that exist in the measurement of relative code phase between multiple satellites. Sequential receivers multiplex all the hardware between the various satellites to be tracked, permitting each satellite to be tracked for a fraction of the total time in a multiplexing manner. With the advent of high speed sampling, however, parallel architectures have been developed with significant reductions in cost and improvements in tracking performances. In parallel architectures, IF samples are processed digitally at rates in excess of the received code rates. This permits the processing of multiple channels with additional correlation ASIC processors. The sensitivity to receiver clock errors is greatly reduced. However, even with the increased speed of the digitally processing parallel architecture, all GPS receivers to date require several seconds for signal acquisition.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide a high speed GPS receiver which reduces the code search time, and subsequent code acquisition time, to 30 milliseconds or less.
Another object of the present invention is to provide a high speed GPS receiver which tracks many satellites simultaneously and allows direct pseudorange measurement.
An additional object of the present invention is to provide a high speed GPS receiver which allows synchronous sampling of multiple GPS satellites.
A further object of the present invention is to provide a high speed GPS receiver which performs GPS code tracking.
A method for rapid acquisition of multiple GPS signals builds upon fast Fourier transformation of input GPS signals to simultaneously track multiple satellites and derive psuedorange measurements that are suitable for navigation solution. The method utilizes 2M samples of the reference signal with N samples of the signal set from the satellites (one millisecond of actual data) with a FFT process to directly compute the fractional psuedorange values for four (4) or more satellites. The FFT process is then combined with a process to determine an integer psuedorange. The integer psuedorange is combined with a fractional psuedorange established by the FFT process to define the GPS navigation solution.
The above and other objects, features, and advantages of the present invention will be better understood from the following detailed description taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a block diagram of a frequency transform correlator according to the present invention.
FIG. 2 shows representative test results of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Code acquisition of Global Positioning System (GPS) signals are routinely performed using a time consuming, time domain correlation technique. For example, the C/A code search method utilized in modern GPS receivers typically requires several seconds for code acquisition.
The present invention reduces the code acquisition time to a search time of under 30 milliseconds, and simplifies the general architecture while allowing simultaneous satellite tracking. To accomplish this, the present invention uses the Discrete Fourier Transform (DFT) as a building block in the design of an advanced GPS receiver. Specifically, the present invention incorporates a modification of DFT known as the Fast Fourier Transform (FFT) which incorporates the Cooley-Tukey algorithm developed in the 1960's. With the advent of advanced computer hardware, the FFT has been used in various applications, many of which involve frequency identification. While the FFT is most often viewed as useful in separating complex signal wave forms into the respective frequency components, a most useful property of the FFT has gone unnoticed in the development of GPS receivers. This property, known as the periodic convolution, generates the transform of the cross correlation function for the received signal and a reference code. The periodic convolution process multiplies the transform of the received signal with the transform of the reference code. Having computed the transform of the cross correlation function, the time domain correlation function can be generated in a single step using the inverse FFT. Since the FFT (and implicitly the inverse FFT) has already been reduced to efficient Very Large Scale Integration (VLSI) hardware, the FFT methodology is easily used for GPS C/A code acquisition and tracking.
The use of FFT in GPS systems is documented in U.S. Pat. No. 4,601,005, issued July 15, 1986, to John Kilvington. However, the U.S. Pat. No. 4,601,005 does not address a key issue important in the actual realization of the use of FFT in GPS. The U.S. Pat. No. 4,601,005 does recognize that the number of samples of the signal set, M, must be correlated with 2M samples from the reference, or overlapping segment in the reference data set. Furthermore, the U.S. Pat. No. 4,601,005 can only track one satellite at a time. This slows target tracking and requires additional circuitry. For simplification of a FFT tracking device, simultaneous parallel tracking of multiple satellites is necessary.
FIG. 1 illustrates the architecture for a frequency transform correlator 10 which measures psuedorange for periodic spread spectrum signals. Frequency transform correlator 10 comprises an RF front end 12 for down conversion of RF signals received by antenna 11, A/D 14 for converting the analog signals received from front end 12 into digital, and for slightly spreading the received signal, and programmable filter 16. A/D 14 is further coupled to sampling control 18. Sampling control 18 facilitates sampling of the input signal at intervals of 1 microseconds. This allows A/D 14 output of 50 to 100 Mhz. Programmable filter 16 then compresses the samples to a rate of 1.023 Mhz resulting in data samples of 1023 elements (M) of a 2048 element array (2M).
Frequency transform correlator 10 further comprises signal memory 20 where the M elements from programmable filter 16 are stored, signal FFT (fast Fourier transform) 22 which receives the stored M elements and processes the 2M elements using a discrete Fourier transform (preferably fast Fourier transform), and final memory 24 which stores the FFT 2M elements.
A reference code 26 simultaneously retrieves from an internal memory a reference code for each satellite being tracked at a given time, and combines the reference codes into a single signal. The summed signal comprises a total of 2048 elements, or 2M samples, within a 2048 element array. The 2M output is converted in a reference FFT 28 using a discrete Fourier transform.
The 2M FFT signal from reference FFT 28 is multiplied in multiplier 30 with the 2M FFT signal stored in final memory 24. The product is computed on a point by point basis for the entire 2048 element array. The inverse 2M FFT of the product is generated in FFT -1 32 to output the correlation function between the reference signals and the input RF signal. The correlation function is output to peak detector/Doppler compensator (PD/DC) 34. FIG. 2 shows an example of the correlation function where four (4) peaks have been detected within PD/DC 34 for 4 satellites. As can be seen in FIG. 2, peaks representing a significant M element for each satellite can be obtained in a single signal process using the 2M FFT/FFT -1 procedure. Peak detection is performed within PD/DC 34 on the magnitude of the 2048 array, and a phase angle of the carrier signal for each satellite is calculated from the phase angle of the inverse FFT at the peaks.
The psuedorange which is required to calculate the GPS navigation solution is comprised of a fractional psuedorange and an integer psuedorange. The fractional psuedorange measurement for each satellite is determined with a one (1) millisecond ambiguity by performing a simple search of the cross correlation function for the peak and then reporting the address of this peak with respect to a reference. The fractional psuedorange represents a fractional part of a C/A (clear acquisition) code length (C/A code length for GPS is one millisecond in time or approximately 300 kilometers). The integer portion of the psuedorange represents the whole number of milliseconds corresponding to the reference epoch, defined as the time when the satellite signal was transmitted. The integer portion of the psuedorange must be established by resolving the one millisecond ambiguity of the fractional psuedorange.
The one millisecond ambiguity of the fractional psuedorange is resolved by detecting bit transitions from the phase measurements available from each detected correlation peak. At bit transition, these phase measurements will change by 180 degrees. By combining bits into words, recognizing the beginning of the GPS data frame, and decoding navigation data transmitted from the satellites, the time of a bit transition can be established. These parameters define the integer psuedorange.
The fractional psuedorange measurement and the integer psuedorange measurement of PD/DC 34 are output to a navigation computation circuit 36. In circuit 36 the two psuedorange measurements are added together to generate a total psuedorange measurement. The total psuedorange measurement is then used to calculate the navigational position of the object being tracked.
PD/DC 34 also operates to compensate for the Doppler effect on the signal from the satellite. As shown in FIG. 1, PD/DC 34 is coupled to sampling control 18 to control the sampling rate within A/D 14 based upon the Doppler compensation. PD/DC 34 is further coupled to reference code 26 for timing and control.
The discrete Fourier transform (DFT) is defined by the transform pair: ##EQU1## and the summations are over the ranges from 0 to N-1.
The DFT of the convolution of two sequences may be computed by multiplying the DFT's of each of the sequences. With high speed A/D conversions at a rate exceeding twice the code bandwidth, such as with GPS systems, the DFT of the received signal can be compute using data from one period of the C/A code (1 millisecond). The DFT contains information on all the GPS signals converted to a frequency. The GPS frequency signals are stored in cache memory for further processing with a transform that is constructed from each of the potential synthesized codes.
For initial acquisition, a Doppler corrected reference code for each satellite to be observed is transformed using DFT. In generating the transform of the reference code, 2M samples are used, where M=1024 elements (GPS code length of +1). The transform for each code is then computed either off line and stored in cache memory, or as needed in real time just prior to the final multiplication process. The transform of the cross correlation function is computed simply by multiplying the transforms on a point by point basis. The signal transform for those points of the 2048 array left empty by the 1023 FFT M elements from final memory 24 are given the value zero.
Thus there has been provided, in accordance with the present invention, a frequency transform correlator that fully satisfies the objects, aims, and advantages set forth above. While the invention has been described in conjunction with specific embodiments thereof, it is evident that many alternatives, modifications, and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, it is intended to embrace all such alternatives, modifications, and variations as fall within the spirit and broad scope of the appended claims. | A method for rapid acquisition of multiple GPS signals builds upon fast Fourier transformation of input GPS signals to simultaneously track multiple satellites and derive psuedorange measurements that are suitable for navigation solution. The method utilizes 2M samples of the reference signal with N samples of the signal set from the satellites (one millisecond of actual data) to directly compute the fractional psuedorange values for four (4) or more satellites. The FFT process is incorporated with a process to determine an integer psuedorange. The integer psuedorange is then combined with a fractional psuedorange to define the GPS navigation solution. | 6 |
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